Total phenols, antioxidant activity expressed as DPPH radical scavenging activity of Smilax genus species.
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More than half of the publishers listed alongside IntechOpen (18 out of 30) are Social Science and Humanities publishers. IntechOpen is an exception to this as a leader in not only Open Access content but Open Access content across all scientific disciplines, including Physical Sciences, Engineering and Technology, Health Sciences, Life Science, and Social Sciences and Humanities.
\\n\\nOur breakdown of titles published demonstrates this with 47% PET, 31% HS, 18% LS, and 4% SSH books published.
\\n\\n“Even though ItechOpen has shown the potential of sci-tech books using an OA approach,” other publishers “have shown little interest in OA books.”
\\n\\nAdditionally, each book published by IntechOpen contains original content and research findings.
\\n\\nWe are honored to be among such prestigious publishers and we hope to continue to spearhead that growth in our quest to promote Open Access as a true pioneer in OA book publishing.
\\n\\n\\n\\n
\\n"}]',published:!0,mainMedia:null},components:[{type:"htmlEditorComponent",content:'
Simba Information has released its Open Access Book Publishing 2020 - 2024 report and has again identified IntechOpen as the world’s largest Open Access book publisher by title count.
\n\nSimba Information is a leading provider for market intelligence and forecasts in the media and publishing industry. The report, published every year, provides an overview and financial outlook for the global professional e-book publishing market.
\n\nIntechOpen, De Gruyter, and Frontiers are the largest OA book publishers by title count, with IntechOpen coming in at first place with 5,101 OA books published, a good 1,782 titles ahead of the nearest competitor.
\n\nSince the first Open Access Book Publishing report published in 2016, IntechOpen has held the top stop each year.
\n\n\n\nMore than half of the publishers listed alongside IntechOpen (18 out of 30) are Social Science and Humanities publishers. IntechOpen is an exception to this as a leader in not only Open Access content but Open Access content across all scientific disciplines, including Physical Sciences, Engineering and Technology, Health Sciences, Life Science, and Social Sciences and Humanities.
\n\nOur breakdown of titles published demonstrates this with 47% PET, 31% HS, 18% LS, and 4% SSH books published.
\n\n“Even though ItechOpen has shown the potential of sci-tech books using an OA approach,” other publishers “have shown little interest in OA books.”
\n\nAdditionally, each book published by IntechOpen contains original content and research findings.
\n\nWe are honored to be among such prestigious publishers and we hope to continue to spearhead that growth in our quest to promote Open Access as a true pioneer in OA book publishing.
\n\n\n\n
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One of the biggest milestones in the therapy of ventricular arrhythmias was the invention of cardiac defibrillation. There were several important developments in the last decades, making nowadays automated external and internal defibrillators widely available. However, the rapid evolution and high differentiation of available options presents a challenge to be kept "up-to-date". With this book, we would like to review the actual guidelines and give practical advices concerning of indications in cardiomyopathy patients, possible contraindications and complications, the perioperative management including anticoagulation and antibiotics, and the programming and follow-up of defibrillator devices.',isbn:null,printIsbn:"978-953-51-0931-0",pdfIsbn:"978-953-51-7059-4",doi:"10.5772/45990",price:119,priceEur:129,priceUsd:155,slug:"cardiac-defibrillation",numberOfPages:188,isOpenForSubmission:!1,isInWos:1,hash:"37b5f2758b30dc35fb41750fa68d2725",bookSignature:"Damir Erkapic, Tamas Bauernfeind",publishedDate:"January 9th 2013",coverURL:"https://cdn.intechopen.com/books/images_new/3289.jpg",numberOfDownloads:17596,numberOfWosCitations:1,numberOfCrossrefCitations:5,numberOfDimensionsCitations:9,hasAltmetrics:0,numberOfTotalCitations:15,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"April 17th 2012",dateEndSecondStepPublish:"May 8th 2012",dateEndThirdStepPublish:"August 4th 2012",dateEndFourthStepPublish:"September 3rd 2012",dateEndFifthStepPublish:"October 3rd 2012",currentStepOfPublishingProcess:5,indexedIn:"1,2,3,4,5,6",editedByType:"Edited by",kuFlag:!1,editors:[{id:"156236",title:"Dr.",name:"Damir",middleName:null,surname:"Erkapic",slug:"damir-erkapic",fullName:"Damir Erkapic",profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:"Dr. Erkapic finished medicine study at J.W. 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The genus Smilax (Smilacaceae), commonly called sarsaparilla, consists of about 350 species. About 79 species are natives of China, 24 species are from India and 29 species are from Central America. The plants of this genus are climbers, have long, thin, thorny stems and have tendrils which attach to other plants or objects to climb steadily (\nFigure 1\n).
\n(A) S. bracteata, (B) S. china, (C) S. fluminensis, (D) S. glyciphylla, images from https://www.inaturalist.org/taxa. (E) S. campestris, image courtesy of Mauricio Bonifacino Ph.D. (Universidad de la República, Montevideo, Uruguay). (F)–(I) S. domingensis.
The rhizome, roots, stems and, occasionally, leaves of sarsaparilla are used as food and in traditional medicine. These plants are known to have immunomodulatory, antioxidant, antibacterial, antifungal and diuretic properties. Additionally, they are used for relief from climatery [1]. Also, the genus Smilax has pharmacological properties and is used to treat different types of cancer, diabetes, skin diseases, ulcers, as well as fever, gout and ophthalmic diseases [2].
\nIn recent years, interest in the study of the genus Smilax has increased, mainly in Europe and Asia, due to the presence of phenolic compounds. Some species have also proven effective in the prevention and treatment of several cancers. In addition, extracts from the genus Smilax exhibit pro-apoptotic activity and antioxidant activity [3].
\nThere are reports about the antioxidant property expressed as DPPH• radical scavenging activity of species of the genus Smilax, as Smilax bockii [4], Smilax campestris [5], Smilax glabra [6], Smilax lanceifolia [7], Smilax perfoliata [8], Smilax riparia [9], Smilax scobinicaulis [10] and Smilax sebeana [11]. This property is attributed to phenolic compounds such as stilbenes, flavones, flavanones, flavonols, smilasides, smiglasides and helionosides, among others. Phenolic compounds have a unique chemical structure for stabilizing free radicals in an aromatic system. Flavonoids and stilbenes have been identified as beneficial agents for the treatment of various diseases such as cardiovascular and neurodegenerative diseases, as well as cancers [12].
\nTherefore, this review will describe Smilax species that have been studied for their antioxidant and anticancer properties with special emphasis on reports of phenolic compounds such as smilasides, smiglasides and helionosides. These compounds are phenols with antioxidant activity and are constituted of a sucrose substituted with feruloyl and coumaril groups. These three groups of compounds are evidence of chemotaxonomy in genus Smilax.
\nThe review is organized by species, and the principal uses in traditional medicine for every species discussed are described. The methods of extraction and purification of phenolic compounds are briefly mentioned. Also, the methods used to evaluate antioxidant and anticancer activities are discussed. Various reports make evident the diversity of the chemical structure of phenolic compounds and their relation to corresponding biological properties.\n
\n\nSmilax aspera has been used to treat diseases such as syphilis, rheumatism and diabetes, and as an antioxidant to reduce the discomforts of menopause [13].
\nLongo et al. isolated and identified anthocyanins from the skin of S. aspera berries [14]. The anthocyanins were extracted with 0.1% HCl (v/v) in methanol. Then, the extract was carried to clean process using solid phase extraction (SPE) of reverse phase C-18. This clean process allowed the removal of sugars, acids and other water-soluble compounds. Finally, the fraction, with a large quantity of phenolic compounds, was subjected to chromatographic purification by High-Performance Liquid Chromatography-Diode Array Detector-Mass Spectrometry (HPLC-DAD-MS). The result of this study was the isolation and characterization of four anthocyanins: two pelargonidins (1, 3) and two cyanidins (2, 4) (\nFigure 2\n) [14]. The principal anthocyanin was identified as pelargonidin 3-O-rutinoside. The anthocyanins are responsible for the color of the S. aspera fruits.
\nAnthocyanin glycosides isolated from S. aspera fruits.
\nS. bockii is a plant used in traditional Chinese medicine with anti-inflammatory and anti-rheumatic properties. Xu et al. prepared a 70% aqueous ethanol extract from roots of S. bockii [4]. Then the extract was partitioned with chloroform, ethyl acetate and butanol successively. The butanol fraction was subjected to chromatographic purification leading to the separation of four flavonols (kaempferol (5), kaempferol-7-O-β-D-glucopyranoside (6), quercetin (7) and isorhamnetin (8), as well as three flavanone ((+)-dihydrokaempferol (9), engeletin (10) and isoengeletin (11)), and a phenylpropanoid, caffeic acid n-butyl ester (12) (\nFigure 3\n). Additionally, the anti-inflammatory activities of a 70% aqueous ethanol extract and chloroform, ethyl acetate and butanol fractions were evaluated and the results showed the butanol fraction had a relevant inhibitory activity against TNF-α-induced NF-κB activation with an IC50 value of 44.8 μg/mL. This activity can be attributed to phenolic compounds present in the butanol fraction.
\nFour flavonols (three aglycones and one glucoside), three flavanones (one aglycone and two glycosides) and one phenylpropanoid ester isolated from S. bockii roots.
\nS. bracteata is a little-studied species. However, there are two representative chemical studies that describe the isolation and characterization of phenolic compounds. The first study was conducted by Li et al. who isolated and identified phenolic compounds from a methanol extract of S. bracteata rhizomes [15]. The air-dried and sliced rhizomes were extracted by maceration with methanol over 24 h. The extract was evaporated and re-dissolved in water and partitioned successively with dichloromethane, ethyl acetate and butanol. The butanol fraction was subjected to column chromatography and six new phenolic compounds were isolated and identified: two flavan-3-ol glucosides (13, 14), one stilbene (15) (\nFigure 4\n) and three phenylpropanoid glycosides (16–18) (\nFigure 5\n). In the same study, Li et al. evaluated antioxidant activity of the six smilasides using the DPPH• radical scavenging activity. The smilasides J to L (22–24) showed an antiradical activity similar to α-tocopherol [15].
\nTwo flavan-3-ol glycosides and one stilbene isolated from S. bracteata rhizomes.
Phenylpropanoid glycosides with a sucrose core isolated from S. bracteata aerial parts.
In a later study, Zhang et al. obtained a 95% aqueous ethanol extract from stems of S. bracteata [16]. The extract was concentrated and redissolved in water and successively extracted with hexane, dichloromethane and butanol. The dichloromethane fraction was purified with chromatography in several steps until smilasides G to L (19–24) were obtained (\nFigure 5\n).
\n\nS. campestris is commonly called sarsaparilla blanca [5]. Its roots and rhizomes have been used in folk medicine to treat skin diseases. An infusion from the leaves and aerial stems of S. campestris is used to relax the digestive system [5]. Rugna et al. reported antioxidant activity from 50% aqueous methanol extract from S. campestris rhizomes; the activity was expressed as total reactive potential (TRAP) [5]. Morais et al. obtained an ethanol extract by maceration and fractions from fresh stems of S. campestris [17]. The ethanol extract was concentrated, and the dried extract was re-dissolved in aqueous ethanol (7:3) and partitioned with hexane, dichloromethane, ethyl acetate and butanol. The antioxidant activity as DPPH• radical scavenging was evaluated for all fractions. The ethanol extract and butanol fraction exhibited a strong antioxidant activity and was higher than Butylated hydroxytoluene (BHT), a commercial antioxidant. Also, Morais et al. reported that rutin (25) (\nFigure 6\n) and quercetin (7) (\nFigure 3\n) flavonol glycosides were the most abundant phenolic compounds present in ethanol extract and butanol fraction, respectively [17].
\nChemical structure of rutin, a flavonol glycoside isolated from S. campestris rhizomes.
\nS. china is the most studied species of genus Smilax. Lee et al. evaluated antioxidant activity of S. china root using DPPH• radical scavenging activity, cell viability, lipid peroxidation activity, superoxide dismutase (SOD) activity, catalase (CAT) activity and glutathione peroxidase (GPX) activity. These authors obtained a 70% aqueous methanol extract from the root of S. china. The extract was concentrated and partitioned with hexane, dichloromethane, ethyl acetate and butanol. The extract and its fractions were evaluated for antioxidant activity. The antiradical activity expressed as IC50 of the extract is about 8 μg/mL, while the ethyl acetate fraction exhibited the principal antiradical activity (IC50 approximately 5 μg/mL) [18]. Jeong et al. obtained several fractions with solvents of different polarity from S. china root and evaluated the antioxidant activity using DPPH• radical scavenging activity, ABTS•+ radical scavenging activity, reducing power, ferric reducing/antioxidant power, ferric thiocyanate assay, malondialdehyde assay using mouse brain homogenates methods, and finally determined total phenols and phenolic composition [19]. The extraction was carried out with methanol at 70°C for 2 h. The methanol extract was evaporated to dryness. The dried extract was re-dissolved in water and the solution was consecutively partitioned with chloroform, ethyl acetate and butanol. The results obtained by Jeong et al. show that the ethyl acetate fraction had the highest total phenol concentration, 401.62 ± 3.13 mg GAE/g of extract and the most abundant phenols were (+)-catechin (26) and (−)-epicatechin (27) (\nFigure 7\n) with a concentration of 135.26 ± 10.08 and 58.10 ± 0.51 mg/100 g, respectively. Consequently, this extract showed the most important antioxidant activity.
\nTwo flavan-3-ol aglycones isolated from S. china roots.
Kuo et al. obtained a 70% aqueous ethanol extract from dried stems of S. china. The extracts were concentrated and suspended in water. The resulting suspension was partitioned with hexane and chloroform [20]. The chloroform fraction was purified by silica gel column chromatography. The purification conducted to isolate smilasides A to F (\nFigures 5\n and \n8\n), heloniosides A (33) and B (34) and smiglaside E (35) (\nFigure 8\n). The anticancer activity of smilasides A to F was evaluated in vitro and showed cytotoxic activity against cervical cancer cells (KB and HELA) and colon cancer cells (DLD-1).
\nPhenylpropanoid glycosides with a sucrose core (five smilasides, two helionoside and one smiglaside) isolated from S. china stems.
Li et al. performed another study related to the evaluation of anticancer activity of S. china extracts with a high content of phenolic compounds [21]. Researchers in this study performed a bioassay-guided separation and purification of kaempferol-7-O-β-D-glucoside (6) from S. china rhizome. First, a 70% aqueous ethanol extract was obtained under reflux. Then the solvent was removed and residue was extracted with ethyl acetate, and butanol, sequentially, in a Soxhlet apparatus. Both ethyl acetate and butanol fractions were subjected to column chromatography separately. Several fractions with large amounts of flavonoid were obtained and each fraction was evaluated for in vitro anticancer activity. The human cells used in this study included liver cancer BEL-7402, cervical epithelial carcinoma HeLa, high metastatic lung carcinoma 95-D, melanoma A375, gastric cancer MKN-45, epithelial carcinoma A431, human acute leukemia HL60, normal embryonic kidney HEK293 and normal embryonic liver L-O2. Li et al. found eight extracts of S. china tubers with anticancer activity against HeLa cells. Also, a bioassay-guided isolation of the polled extract lead to the detection of kaempferol-7-O-β-D-glucoside (6). This flavonoid induces apoptosis as an anti-proliferative action related to radical scavenging activity [21]. Shao et al. developed a specific HPLC method for determination of the six major phenolic compounds active in S. china: taxifolin-3-O-glycoside (36), scirpusin A (37), piceid (38), oxyresveratrol (39), resveratrol (40) (\nFigure 9\n) and engeletin (10) (\nFigure 3\n). These compounds were extracted from the tuber of S. china with 95% aqueous ethanol and the concentrated extract was partitioned with petroleum ether, ethyl acetate and butanol. The ethyl acetate fraction was subjected to repeated silica gel chromatography. Finally, the purification of phenolic compounds was performed by HPLC [22]. Wu et al. also reported other study related to anticancer activity of phenolic compounds from S. china [12]. These authors obtained a 95% aqueous ethanol extract from the tuber of S. china, which was concentrated and suspended in water. The suspension was partitioned with petroleum ether, ethyl acetate and butanol. The ethyl acetate was the most bioactive fraction. This fraction was subjected to chromatographic purification. Three sub-fractions and six bioactive phenolic compounds bioactives: three flavonoids (kaempferol-7-O-β-D-glucoside (6), dihydrokaempferol (9) and dihydrokaempferol-3-O-α-L-rhamnoside (10)) and three stilbenoids (37, 39 and 40), were isolated from the ethyl acetate fraction. These compounds were found to induce apoptosis in anti-breast tumor cells MCF-7 and MDA-MB-231. The results showed that resveratrol and oxyresveratrol had the highest apoptosis rates [12].
\nOne flavanonol (36) and four stilbenes (37–40) isolated from 95% ethanol extracts of S. china tubers.
\nS. corbularia is used in traditional Thai medicine for the ailments treatment caused by the menopause, as well as for ovarian and breast cancer. For this reason, Wungsintaweekul et al. isolated and characterized the phenolic compounds of methanol extract from S. corbularia rhizome [23]. They also evaluated the cell proliferation stimulation of the isolated compounds against human cancer cell lines MCF-7 and T47D. The major compounds present in the rhizome of S. corbularia were rhamnosides dihydroflavonol derivatives, which represent 15% of methanol extract by weight. The results showed that the extract did not exhibit cytotoxicity against breast cancer cell lines MCF-7 and T47D. However, the flavanonol rhamnosides (engeletin (10) and isoengeletin (11)) (\nFigure 3\n); as well as, astilbin (41), isoastilbin (42), neoastilbin (43) and neoisoastilbin (44) (\nFigure 10\n), showed a suppressive effect on estradiol at concentration of 1 μM as evidenced by human breast cancer cell proliferation.
\nFlavononol rhamnosides (41–44) with activity against human breast cancer isolated from methanol extract of S. corbularia rhizomes.
\nS. domingensis is used in Central America by the pharmaceutical and cosmetics industries. The most representative studies of S. domingensis are related to cytotoxicity to cancer cells [24], inhibitory activity of estrogen [25] and antioxidant activity [26]. The chemical studies of S. domingensis only cover qualitative identification of flavonoids and anthocyanins using thin-layer chromatography (TLC) [27].
\n\nS. excelsa is used in Turkey’s traditional medicine to treat breast cancer, stomach pain and bloating [28]. Ozsoy et al. evaluated antioxidant activity of infusion, decoction, ethanol and ethyl acetate extracts from S. excelsa leaves using the inhibition of lipid peroxidation, metal ion chelating, reducing power, DPPH• radical scavenging, superoxide, hydroxyl radicals and hydrogen peroxide [29]. Also, total phenols, total flavonoid and anthocyanin were quantified in the extracts. The content of total phenols and total flavonoid was found in the intervals of 8.8–35.7 GAE mg/g of dry matter and 0.61–28.7 catechin equivalents mg/g of dry matter, respectively. The extract with the highest content of total phenols was the infusion. The decoction and infusion showed major DPPH• radical scavenging. These results agree with the high content of phenols and flavonoids present in the infusion and decoction. On other hand, Khaligh et al. isolated and elucidated three phenol compounds (trans-resveratrol (40) (\nFigure 9\n), 5-O-caffeoylshikimic acid (45) and 6-O-caffeoyl-β-D-fructofuranosyl-(2→1)-α-D-glucopyranoside (46)) from ethyl acetate extract of S. excelsa (\nFigure 11\n) [30]. The extraction was a maceration performed at room temperature. After the solvent was removed, the extract was separated using silica gel column chromatography. In these study, also was evaluated the cytotoxicity of isolated compounds against human breast adenocarcinoma MCF-7cell lines. The 6-O-caffeoyl-β-D-fructofuranosyl-(2→1)-α-D-glucopyranoside showed a promising activity against MCF-7 cell lines [30].
\nTwo phenylpropanoids (45 and 46) derivates of caffeic acid with activity against human breast cancer.
\nS. fluminensis has a wide geographical distribution in Brazil, and propagation studies have shown it to grow relatively easily. Hence, it is a promising species for growing demand from the pharmaceutical industry [31, 32] have published the only chemical study of S. fluminensis thus far. They obtained extracts from leaves and isolated phenolic compounds. Two flavonol glycosides were isolated and characterized, rutin (25) (\nFigure 6\n) and quercetin-3-O-β-D-galactopyranoside (47) (\nFigure 12\n).
\nFlavonol glycoside (47) isolated from branches of S. fluminensis.
The second most-studied species, after S. china is S. glabra. This species has been used in Chinese folk medicine for the treatment of acute bacterial dysentery, syphilis, acute and chronic nephritis [33], hyperinsulinemia [34] and cancer [35]. She et al. evaluated the effect of aqueous extract of S. glabra on cancer cell adhesion, migration and invasion of HepG2, MDA-MB-231 and T24 cells in vitro and the metastasis suppression of MDA-MB-231 cells in vivo [36]. Gao et al. showed 95% aqueous ethanol extracts of S. glabra rhizomes to be effective against cancer via mitochondrial apoptosis in human breast cancer MCF7, colon carcinoma HT-29 and gastric cancer cell line BGC-823 [3]. The results obtained by these authors point out that the aqueous extract of S. glabra possibly promotes cell adhesion by increasing the size and strength of focal adhesions and inhibits the invasion of HepG2, MDA-MB-231 and T24 cells.
\nXia et al. performed an evaluation of the protective effect of 60% aqueous ethanol extract of S. glabra rhizome against lead-induced oxidative stress in rats and quantified total phenols and total flavonoids [37]. The results of this study proved that the extract of S. glabra could minimize damages caused by the lead. The protective effect can be attributed to high concentrations of total phenols and total flavonoids in the extract. Total phenols reported were 262 ± 12.7 mg gallic acid equivalents (GAE)/g dry weight of the extract and total flavonoids were 203.4 ± 9.1 mg rutin equivalents/g dry weight of the extract [37].
\nTrinh et al. evaluated the antioxidant activity of 95% aqueous ethanol extract of S. glabra roots. They obtained two fractions from a partitioning with hexane and ethyl acetate, and astilbin (41) (\nFigure 10\n) isolated from the ethyl acetate fraction [38]. The fractions were obtained from 95% aqueous ethanol previously dried. The extract was suspended in 50% aqueous ethanol and partitioned with hexane and ethyl acetate. The extract, hexane and ethyl acetate fractions, and 41 were subjected to evaluation of DPPH• radical scavenging activity, thiobarbituric acid-reactive species (TBARS) and 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) cell viability assay for hepatoprotective effect via H2O2-injured mouse hepatocytes. The astilbin was isolated from the ethyl acetate fraction. The results of this study showed the ethyl acetate fraction has the principal antioxidant activity and MTT, attributed to the presence of astilbin, the main phenolic compound present in S. glabra rhizome [38]. Astilbin (41), a rhamnosyl flavanonol, besides exhibiting antioxidant activity, has coenzyme A reductase-inhibiting [39], aldose reductase-inhibiting [40], hepatoprotective [41], anti-oedemaogenic [42] and anti-arthritis [43] activities.
\nZhang et al. obtained two aqueous and methanolic extracts, from S. glabra rhizomes and evaluated their antioxidant activity using DPPH• radical scavenging, ABTS radical cation scavenging, reducing power, superoxide anion radical scavenging activity and antioxidant activity in a linoleic acid emulsion system. They carried out quantification of total phenols [44]. The results showed that the methanol extract had the highest content of total phenols (152.28 ± 10.57 mg GAE/g of extract) and astilbin (245.65 ± 8.21 mg/g of extract). In general, the methanol extract has more antioxidant activity than aqueous extract and this behavior is attributed to the presence of 41 in the methanol extract [44]. Lu et al. evaluated antioxidant and anti-inflammatory activities of 70% aqueous ethanol extract from S. glabra rhizomes [45]. The methods used to evaluate antioxidant activity were DPPH• radical scavenging, ABTS radical cation scavenging and reducing power. Anti-inflammatory activity was evaluated with MTT cell viability, measuring of nitric oxide/nitrite and enzyme-linked immunosorbent assay for IL-6 and TNF-α cytokines detection. The study also involved quantification of total phenols and total flavonoids. This was done by separation and identification of major phenols using ultrahigh pressure liquid chromatography coupled to electrospray mass spectrometry (U-HPLC-ESI-MS). The results obtained showed the 70% aqueous ethanol extract of S. glabra rhizome has a radical scavenging on DPPH• statistically equal to ascorbic acid (P > 0.05). The results regarding anti-inflammatory activity showed that accumulation of NO, IL-6, and TNF-α in lipopolysaccharides (LPS)-stimulated groups was higher than the group used as the positive control. Dexamethasone was employed as a positive control. Finally, 17 phenolic compounds were isolated and identified from the 70% aqueous ethanol extract of S. glabra rhizome, including engeletin (10) and isoengeletin (11) (\nFigure 3\n); astilbin (41), isoastilbin (42), neoastilbin (43), neoisoastilbin (44) (\nFigure 10\n); and 5-O-caffeoylshikimic acid (45) (\nFigure 11\n).
\nMoreover, there have been several chemical studies to isolate and characterize phenolic compounds from different parts of S. glabra. Chen et al. obtained a methanol extract of S. glabra rhizome. After solvent removal, the dry extract was suspended in water and partitioned with ether petroleum and ethyl acetate. The ethyl acetate extract was purified by chromatographic column to separate the phenolic compounds. The compounds isolated were five flavonoids (engeletin (10), astilbin (41), smitilbin (48), taxifolin or dihydroquercetin (49) and eucryphin (50), \nFigure 13\n), and two phenylpropanoids, resveratrol (40) and 5-O-caffeoylshikimic acid (45) [33]. Cheng et al. isolated new five phenylpropanoid glycosides, containing a sucrose core, smiglasides A–E (35, 51–54, (\nFigures 8\n and \n13\n) from S. glabra rhizomes, [46]. The extraction and isolation procedures were followed exactly as was described by Chen et al. [33].
\nFlavonoids and smiglasides isolated from S. glabra rhizome.
Xu et al. conducted a comprehensive chemical study of S. glabra rhizomes [47]. The air-dried and powdered rhizomes of S. glabra were extracted with 95% aqueous ethanol and 50% aqueous ethanol under reflux, consecutively. The extracts were combined and evaporated until to dryness and the residue was suspended in water and partitioned with petroleum ether, ethyl acetate and butanol. The ethyl acetate and butanol fractions were subjected to chromatographic separation. The purification allowed to the isolation 13 flavanones (dihydrokaempferol (9), engeletin (10), astilbin (41), isoastilbin (42), neoastilbin (43), neoisoastilbin (44), taxifolin (49), naringenin (55), sakuranetin (56), arthromerin B (57), sinesin (58), (2R,3R)-taxifolin-3′-O-β-D-glucopyranoside (59) and (2S,3S)-glucodistylin (60); 3 flavanes: (+)-catechin (26), (−)-epicatechin (27) and cinchonain 1b (60)); 2 flavanones (luteolin (62) and apigenin (63)); two flavonols (quercetin (7) and myricetin (64)); 1 chalcone, kukulkanin B (65); 3 stilbenes (piceid (38), piceatannol (39), and resveratrol (40)); 6 phenylpropanoids (5-O-caffeoylshikimic acid (45), caffeic acid (66), 3-O-p-coumaroylshikimic acid (67), smiglycerol (68), juncusyl ester B (69) and 1-O-p-coumarylglycerol (70), \nFigure 14\n). It is noteworthy that in this study no smiglasides were detected, despite an intensive separation of phenolic compounds having conducted. One explanation for these results is that possibly the high temperatures used for extraction caused smiglasides degradation.
\nFlavonoids and phenylpropanoids isolated from S. glabra rhizome.
\nS. glycyphylla is a plant endemic to Australia and its leaves and fruits have a sweet taste like honey grass. The sweet principle of S. glycyphylla is called glycyphyllin A (71) and identified as a phenol compound with a structure of dihydrochalcone, phloretin-2′-α-L-rhamnose [48]. Cox et al. evaluated aqueous extracts of leaves and stems of S. glyciphylla [49]. The methods used to evaluate antioxidant activity were lipid peroxidation using thiobarbituric acid reactive substances (TBARS), superoxide quenching by coupling superoxide generation to the reduction of nitroblue tetrazolium (NBT), inhibition of deoxyribose-driven fenton degradation and total radical-antioxidant potential (TRAP) using free radicals derived from ABTS (2,2′-azinobis(3-ethylbenzothiazoline 6-sulphonate). The results showed that S. glycyphylla extract inhibited deoxyribose degradation. The total radical-antioxidant potential was seven times that the trolox a water-soluble analog of vitamin E with a high antioxidant activity.
\nHuang et al. performed a study of phenolic profile and antioxidant activity of S. glycyphylla leaves [50]. The leaves of S. glycyphylla previously dried and blended were extracted with 80% aqueous ethanol. Then, the extract was concentrated and partitioned with hexane and butanol, consecutively. The butanol fraction was subjected to chromatographic separation. The separation produced eight phenolic compounds such as the glycyphyllin A previously mentioned, two new dihydrochalcones (glycyphyllin B (72) and C (73)) and five flavonoids (catechin (26), (2R,3R)-dihydrokaempferol-3-O-β-D-glucopyranoside (57), kaempferol-3-O-β-D-glucopyranoside (74), quercetin-3-O-β-D-glucopyranoside (75) and kaempferol-3-O-β-neohesperidoside (76), \nFigures 14\n and \n15\n). The antioxidant activity of pure compounds was evaluated using ferric reducing ability of plasma (FRAP) and DPPH• radical scavenging. The flavonoids showed a good antioxidant activity; contrary to this, the dihydrochalcones showed weak antioxidant activity [50].
\nPhenolic compounds isolated from 80% ethanol extract of S. glycyphylla leaves.
The root of S. lanceifolia prepared as a decoction is used in traditional Indian medicine to soothe stomach pain and rheumatism. The boiled extract is used to expel gallbladder and kidney stones. It was also found that the aqueous extract of S. lanceifolia contains compounds with a high affinity for binding proteins, specifically by active sites joining reverse transcriptase. Therefore, it can be used to inhibit proliferation of retroviruses-agents in viral diseases such as AIDS and T-cell leukemia [51]. Laintojam and Kongbrailatpam performed a study on the chemical constituents and antioxidant activiy of S. lanceifolia roots extracts [7]. The extracts were obtained from petroleum ether, chloroform and methanol, successively. Antioxidant activity of the extracts was evaluated by DPPH• radical scavenging and it was found that the methanol extract had the principal antiradical activity attributed to phenolic compounds. The only compound isolated from methanol extract was flavanonol glycoside, quercitrin (77, \nFigure 16\n) [7].
\nFlavanonol glycoside from methanol extract of S. lanceifolia roots.\n
The roots and rhizomes of S. riparia, commonly called “Niu-Wei-Cai” in China, are used in traditional Chinese medicine as diuretics, treatments for inflammation and cancer [52], and in some cases as food [53]. Sun et al. isolated three phenylpropanoid glycosides (the smilasides M (78) and N (79), and 2′,6′-diacetyl-3,6-diferuloylsucrose (80), \nFigure 16\n) from a 95% aqueous ethanol extract of S. riparia roots and rhizomes. The concentrated extract was suspended in water and subjected to D101 macroporous resin column chromatography and eluted with water and 30% and 70% ethanol, successively. The fraction eluted with 70% ethanol was suspended in water and partitioned with chloroform, ethyl acetate and butanol. The ethyl acetate fraction was chromatographed over a silica gel column, followed by thin-layer chromatography (TLC) and finally, the fractions were subjected to C18 reversed-phase silica gel column to obtain the afore-mentioned compounds, [54].
\nWang et al. isolated five phenylpropanoids with a sucrose core (helonioside B (18), smiglaside A (51), smiglaside B (52), and smilaside P (81), \nFigures 5\n, \n13\n and \n17\n) [55]. The phenylpropanoid compounds were obtained from a 95% aqueous ethanol extract of S. riparia roots and rhizomes. The extract was subjected to macroporous resin HPD-600 and eluted with 95% aqueous ethanol and ethyl acetate. Subsequently, the ethyl acetate fraction was subjected to silica gel column chromatography, and from this fraction were obtained the phenylpropanoids compounds. The five compounds were subjected to cytotoxicity test against human promyelocytic leukemia (HL-60), human hepatocellular carcinoma (SMMC-7721), human lung cancer (A-549), human breast cancer (MCF-7) and human colon cancer (SW480) using 3-(4,5-dimethylthiazol-2-yl)-5-(3-carboxymethoxy-phenyl)-2-(4-sulfophenyl)-2H-tetrazolium (MTS). The five compounds were evaluated for anticancer activity. Antioxidant activity was also evaluated using DPPH• radical scavenging activity. The results showed the phenylpropanoid compounds with three feruloyl and acetyl groups exhibited the primary antitumoral and antioxidant activities. The proposed explanation of these results was that the feruloyl and acetyl groups confer a minor polarity to the compounds with the most activity and are key to inducing antitumoral activity [55].
\nPhenylpropanoids from 95% ethanol extract of S. riparia roots and rhizomes.
The roots of S. scobinicaulis, also called “Hei Ci Ba Quia” in Chinese, are used in traditional Chinese medicine for the treatment of arthritis, gout and inflammatory diseases [10]. Zhang et al. studied the chemical composition of S. scobinicaulis. These researchers first obtained a 95% aqueous ethanol extract from S. scobinicaulis roots and rhizomes. The extract was concentrated, suspended in water and partitioned with petroleum ether, ethyl acetate and butanol, successively. The ethyl acetate fraction was subjected to column chromatography. The purification was done to isolate and characterize two new flavones (7,3′,5′-trihydroxy-5,6,4′-trimethoxyflavone (82) and 7-hydroxy-5,6,3′,5′-pentamethoxyflavone (83), \nFigure 18\n). The new flavones were evaluated for cell proliferation and viability assay against human breast adenocarcinoma (MCF-7) and human lung carcinoma (H520). The results showed a weak activity for 82, but 7-hydroxy-5,6,3′,5′-pentamethoxyflavone, 83 was inactive [10].
\nFlavones from 95% ethanol extract of S. scobinicaulis roots.
\nS. sebeana is used in traditional Japanese and Chinese medicine to treat syphilis, arthritis and gout [11]. Ao et al. evaluated antioxidant activity in isolated phenolic compounds from methanol extracts of S. sebeana rhizomes and roots [11]. The methanol extract was obtained from maceration of fresh rhizomes and roots with methanol at room temperature. The methanol extract was concentrated, suspended in water and partitioned with hexane, ethyl acetate and butanol, successively. The ethyl acetate fraction was purified in two steps. First, it was subjected to column chromatography packed with sephadex LH-20. Some of the fractions collected were selected to evaluate by HPLC to evaluate their components. Finally, the fractions with similar composition were pooled and purified by preparative HPLC. Also, the total phenol content and antioxidant activity expressed by DPPH radical scavenging were evaluated for methanol, ethyl acetate and butanol fractions. The major content of total phenols was found in the ethyl acetate fraction, 238.5 mg catechin/g extract. This fraction also showed the principal DPPH• radical scavenging activity, IC50 of approximately 10.4 μg/mL. The compounds isolated from the ethyl acetate fraction were one phenylpropanoid (chlorogenic acid (84), \nFigure 19\n) and three cinchonain (1b (61), 1a (85) and 11a (86), \nFigures 14\n and \n19\n) [11].
\nPhenolic compounds from methanol extract of S. sebeana rhizomes and roots.
\nS. trinervula is a plant used in traditional Chinese medicine. The rhizomes and roots are sources of the Chinese drug “Ba-Quia” used as a diuretic and to treat pelvic inflammation [56]. Shu et al. carried out the first chemical designed to isolate phenolic compounds from rhizomes of S. trinervula. These researchers obtained a 70% aqueous ethanol extract and removed the solvent [56]. The extract was partitioned with ethyl acetate and butanol. The butanol fraction was subjected to macroporous resin column chromatography. The fractions obtained from this separation were subjected to repeated silica gel and sephadex LH-20 column chromatography. Finally, the fractions were subjected to semipreparative HPLC. From this separation process were isolated eight phenolic compounds, three phenylpropanoids and five neolignans. These compounds were evaluated against five human cell lines (SH-SY5Y, SGC-7901, HCT-116, Lovo and Vero) using the MTT method. The anticancer evaluation showed (7S,8R)-4,7,9,9′-tetrahydroxy-3,3′-dimethoxy-8-O-4′-neolignan (87) and (7R,8R)-4,7,9,9′-tetrahydroxy-3,3′-dimethoxy-8-O-4′-neolignan (88) (\nFigure 20\n) had cytotoxic activity against Lovo [56].
\nTwo neolignans (87 and 88) with colon anticancer activity isolated of 70% ethanol extract from S. trinervula rhizomes.
The polar extracts of Smilax species have high concentrations of phenolic compounds with high antioxidant activity. The main investigations of Smilax species are oriented to evaluate cytotoxicity against human cancer of cervical, lung, breast adenocarcinoma, liver and colon. The results of this review chapter showed flavonol, astilbin and phenylpropanoids binding to the sucrose nucleus (three moieties of ferulic acids and acetyl group to maximize activity) have a high potential as anticancer compounds. The anticancer activity with high concentrations of phenol compounds is attributed to antioxidant activity that induces cell apoptosis. The flavonols and phenylpropanoids can be isolated from ethyl acetate fractions obtained from a 95% aqueous ethanol extract of rhizomes and roots. Also, areal parts of Smilax plants contain phenolic compounds, for example, leaves and fruits. \nTable 1\n shows a resume of total phenols content and DPPH• radical scavenging activity of extracts and fractions obtained from five Smilax species. The leaves and fruits of Smilax plants contain phenolic compounds. The fruits are also a source of anthocyanins. The chemical studies based on isolation and evaluation of phenolic compounds are few and do not cover more than 10% of the total Smilax species. Most studies have been carried out on species that grow in Asia. Hence, it is necessary continue studying the phenolic compound content of Smilax species, as well as evaluating their antioxidant, antidiabetic and anticancer properties.
\nSpecie (part of plant) Extract/fraction | \nTotal phenols (mg GAE/g dm) | \nDPPH●\n Radical scavenging activity IC50 (μg/mL) | \n
---|---|---|
\n\nS. campestris\n (aerial) | \n\n | Ref. [17] | \n
Ethanol extract | \n– | \n13.6 | \n
Hexane fraction | \n– | \n405.5 | \n
Dichloromethane fraction | \n– | \n298.9 | \n
Ethyl acetate fraction | \n– | \n108.9 | \n
Butanol fraction | \n– | \n2.1 | \n
\n\nS. china\n (roots) | \nRef. [19] | \nRef. [19] | \n
Methanol extract | \n– | \n– | \n
Chloroform fraction | \n142.6 | \n302.2 | \n
Ethyl acetate fraction | \n401.6 | \n85.5 | \n
Butanol fraction | \n206.8 | \n210.9 | \n
Water fraction | \n97.3 | \n224.9 | \n
\n\nS. excelsa\n (leaves) | \nRef. [29] | \nRef. [29] | \n
Water extract | \n30.6 | \n1190 | \n
Infusion | \n35.7 | \n1240 | \n
Ethanol extract | \n30.1 | \n1490 | \n
Ethyl acetate extract | \n8.8 | \n2660 | \n
\n\nS. glabra\n (rhizomes) | \nRef. [44] | \nRef. [44] | \n
Water extract | \n29.41 | \n236 | \n
Ethanol fraction\na\n\n | \n109.8 | \n58 | \n
Methanol extract | \n152.3 | \n43 | \n
\n\nS. riparia\n (rhizomes and roots) | \n\n | Ref. [55] | \n
95% ethanol extract | \n– | \n2520 | \n
95% ethanol fraction | \n– | \n1460 | \n
Ethyl acetate fraction | \n– | \n1330 | \n
Methanol fraction | \n– | \n1000 | \n
Total phenols, antioxidant activity expressed as DPPH radical scavenging activity of Smilax genus species.
This fraction was obtained from water extract.
GAE mg: milligrams of gallic acid equivalent, dm: dry matter, IC50: extract concentration necessary to decrease 50% the initial concentration of DPPH•. The fractions were obtained from a partition of corresponding extract.
The authors thank Carol Ann Hayenga for her English assistance in the preparation of this manuscript. Support was provided by the Universidad Tecnológica de la Mixteca.
\nAn optical fiber is an extended cylindrical optical waveguide. In its simplest form, it consists of a core having a certain refractive index nc and is surrounded by a clad (sometimes called skin) of refractive index ncl (or ns). An optical fiber is used to guide light through its core, from one end to another, based on the principle of total internal reflection which mandates that nc must be always higher than ncl. Basically, optical fibers are made of highly pure silica glass doped with some impurities in order to increase nc or decrease ncl [1, 2, 3]. Recently, polymeric optical fibers got more attention as alternatives of some glass based optical fibers [1, 4].
Optical fibers are involved in many technological applications such as telecommunications, sensing [4, 5]; fiber lasers and fiber amplifiers [6]; fiber gratings which can act as mirrors [7, 8]; mode converters [9]; modulators; and couplers and switches [10, 11]. Optical fibers are considered ideal optical transmission media since communication cables hundreds of kilometers in length can be obtained with low absorption and low loss due to the purity and cross-sectional uniformity of the manufactured optical fibers. Moreover, accurate tuning of the refractive indices of both core and clad guarantee extremely low scattering loss at the interfaces [1].
The commonly known optical fibers are step index and graded index (GR-IN) optical fibers. The former means that the core’s refractive index is homogeneous while it suffers an abrupt change at the boundary with the clad. For a GR-IN optical fiber, the core does not have a constant value of refractive index but it rather has a radial distribution of refractive index. These two types of optical fibers can be classified into either single-mode or multi-mode optical fibers. Single-mode optical fiber only sustains one mode of propagation while the multi-mode optical fiber can sustain up to hundreds of propagation modes [1, 3]. The number of the propagation modes is related to the numerical aperture of the fiber, which, in turn, depends on the refractive indices of both core and clad.
Accurate characterization of optical fibers is required in order to know about their functions and performances. There are many methods of optical fibers characterization such as optical microscopy, electron microscopy, X-ray spectrometry, infrared spectroscopy, light diffraction, light scattering, optical interferometry, and digital holography [1, 3, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29]. Optical interferometry is an effective accurate tool for studying and characterizing optical fibers. It depends on the determination of the phase difference between a ray of light transmitting the fiber’s cross-section and a reference ray reaching the interference plane directly without crossing the fiber. This phase shift can be transformed into a refractive index map representing the radial distribution of the refractive index across the fiber or, in other words, the refractive index profile (RIP). Interferometry can detect tiny changes in refractive index if an external effect is applied on the fiber. The change of refractive index can be in situ detected if the interferometer is developed to achieve this task. Interference patterns can be digitally processed and analyzed in order to increase the accuracy of the obtained results [1, 17, 22, 26, 27, 30, 31, 32, 33, 34, 35].
Interference techniques can be classified into either two-beam interferometers such as Michelson, Mach-Zehnder, Pluta polarizing microscope, Lioyd’s mirror, etc., or multiple-beam interferometers such as Fabry-Pérot and Fizeau interferometers [1, 3, 25, 36, 37, 38, 39]. A two-beam interferometer produces a pattern of alternate bright and dark fringes of equal thicknesses when two beams, usually, of equal intensities Io suffering a relative phase difference δ are superposed. The resultant intensity distribution I of the interference pattern is given as:
Multiple-beam interference takes place when light rays fall on two parallel optical plates enclosing a small distance between each other while their inner surfaces are highly reflecting and partially transparent. The intensities of both reflected, I(r), and transmitted, I(t), light distributions that are redistributed due to the multiple-beam interference are given as [40]
where, I(i) is the intensity of the incident light, T and R are the products of the transmission and reflection coefficients of the two surfaces, respectively, while δ is the phase difference between any two consecutive interfered rays.
On the other hand, holography was firstly presented by Gabor in 1947 as a lens-less process for image formation by reconstruction of wave-fronts [41, 42, 43]. It offers 3D characterization such as the depth of field from recording and reconstructing the whole optical wave field, intensity, and phase [41, 42]. Holographic interferometry is a non-destructive, contactless tool that can be used for measuring shapes, deformations and refractive index distributions [44, 45]. The modern digital holography was introduced in 1994 [46, 47, 48]. Moreover, the phase shifting interferometric (PSI) technique was introduced by Hariharan et al. as an accurate method for measuring interference fringes in the real time [49]. Recently, digital holographic phase shifting interferometry (DHPSI) was used to investigate some optical parameters of fibrous materials [17, 18, 21, 26, 27, 28, 29].
In DHPSI, frequently a set of four [20] or five [23, 33] phase shifted holograms with known mutual phase shifts starting with 00 and having 900 separations have to be recorded [21]. These recorded holograms can be represented by:
where a(ζ, η) and b(ζ, η) are the additive and the multiplicative distortions and
or,
In digital holography, the recorded wavefield is reconstructed, based on Fresnel diffraction integral, by multiplying the stored hologram by the complex conjugate of the reference wave r*(ζ, η) to calculate the diffraction field b’(x’, y’) in the image plane, see Figure 1. This can be calculated using the finite discrete form of the Fresnel approximation to the diffraction integral as:
Geometry of digital holographic axes and the planes systems.
The parameters used in this formula depend on the used CCD array of N × M pixels and the pixel pitches Δζ and Δη. The distance between the hologram and the image plane is denoted by d’. The pixel spacings in the reconstructed field of image are:
The convolution of h(ζ, η)r*(ζ, η) can be used as alternative of Fresnel approximation [37]. The resulting pixel spacing for this convolution approach is
In addition, the phase shifted holograms are used to overcome the problems of the d.c. term and twin image, in which the calculated complex wavefield is used instead of a real hologram in the convolution approach.
The intensity and phase distributions in the reconstruction plane are given by
So, the optical phase differences due to phase objects can be extracted.
Mach-Zehnder interference-like system is used as a digital holographic setup as shown in Figure 2 [20, 23, 29, 33]. The optical waveguide sample, such as optical fiber, is immersed in a liquid of refractive index nL near or matching the cladding refractive index nclad of the sample. The interference patterns are recorded using a charge-coupled device, that is, CCD camera.
Mach-Zehnder digital holographic interferometric set-up, S F: spatial filter, L: collimating lens, BS: beam splitter, M: mirror, and MO: microscopic objective.
In this chapter, we illustrate some featured work on interferometric characterization (sometimes, implying digital holographic interferometry) of different optical fibers done by our research group during the last three decades. In Section 2, interferometric characterization of conventional step-index and GR-IN optical fibers is presented. Section 3 illustrates characterization of the conventional optical fibers when they are suffering mechanical bending. In Section 4, interferometric characterization of a special type of optical fibers called polarization maintaining (PM) optical fibers is presented. In the last section, we elucidate thick optical fibers and their interferometric characterization with a special interferometric system, developed in our laboratory, called lens-fiber interferometry (LFI).
In 1994, Hamza et al. derived a mathematical expression to calculate the RIP of an optical fiber by considering the refraction of optical rays at the liquid-clad and clad-core interfaces, see Figure 3 [12]. It was the first time to consider the refraction of the transmitted rays to reconstruct the RIP of a fiber. The derived expressions for calculating the RIP in case of two-beam and multiple-beam interferences, based on Figure 3, are given by Eqs. (12) and (13), respectively.
An incident ray (object ray) is refracted due to a clad-core fiber causing a fringe shift Z when interferes with a reference ray.
where, R is the fiber’s radius and e is the skin’s thickness. nL, ns, and nc are the refractive indices of the immersion liquid, skin, and core, respectively. λ is the wavelength of the used illuminating source. Ls and Lc are the geometrical path lengths inside the skin and the core, respectively. Z is the fringe shift due to the presence of the fiber while h is the interfringe spacing and d is the distance measured from the center of the fiber to the position of the incident ray.
In that work, they used Fizeau interferometer to determine the refractive index profile of FOS Ge-doped step-index multi-mode optical fiber with a core radius 19.5 μm. The fiber was immersed in a liquid of refractive index nL = 1.4665, which was a little bit greater than ns while the wavelength of the used illuminating source was λ = 546.1 nm. The Fizeau interferogram of this fiber is shown in Figure 4a. The obtained RIP was compared with the profile calculated for the same fiber when the refraction of light through the fiber was neglected as was usually done by other authors before this work. There was a significant difference between the two profiles, see Figure 4b. Therefore, the refraction through the fiber was recommended to be considered for calculating RIPs particularly when the refractive index of the immersion liquid is not close to the fiber’s refractive index.
(a) An interference pattern of Fizeau fringes, in transmission, for a FOS step-index optical fiber. (b) RIPs of this fiber in case of considering and neglecting the retraction of the crossing rays inside the fiber.
In 2008, another mathematical model was derived in order to determine RIPs of fibers having regular and/or irregular cross-sections [38]. This method was based on immersing the investigated fiber in two liquids with different, but so closed, refractive indices. They applied this method on a single-mode optical fiber, having a small core of radius <5 μm while the fiber’s radius was 60.6 μm, as shown by Fizeau interferograms in Figure 5 when the fiber was immersed in two liquids with refractive indices (a) 1.4589 and (b) 1.4574. The obtained RIP of this fiber is illustrated in Figure 5c showing that this fiber has nc = 1.4630 and ncl = 1.4596. This method was simple and accurate enough to detect such a small core of a step-index optical fiber.
Fizeau interferograms, in transmission, for a single-mode optical fiber when it was immersed in two liquids of refractive indices (a) 1.4589, (b) 1.4574. (c) RIP of the single-mode optical fiber having the interferograms shown in (a) and (b).
A GR-IN optical fiber with a radial refractive index distribution was suggested to be divided into a finite number (M) of concentric layers where each layer has its own value of refractive index, see Figure 6a. The thickness (a) of each layer equals R/M, where R is the radius of the graded-index part. When the ray falls on the fiber at a distance dQ apart from the fiber’s center, the ray refracts through Q layers. The nearest layer to the fiber’s center has a refractive index nQ. The fiber’s RIP can be calculated using Eq. (14) in case of two-beam interference and Eq. (15) in case of multiple-beam interference [13]. Another model was presented in order to get RIP of a GR-IN optical fiber by considering the real path of the optical ray due to the refraction in the core region as well as adding a correction for the ray passing through the immersion liquid [50], see Figure 6b. In this case, the fringe shift was obtained by assuming values for both the profile shape parameter (α) and the difference between refractive indices of core and clad (Δn). A prepared software was programmed to iterate and get the best values of α and Δn and comapre the calculated fringe shift with the experimentally obtained one.
(a) A schematic diagram shows the path of an optical ray crossing Q layers in the core region. (b) A schematic diagram shows the path of an optical ray crossing a GR-IN core optical fiber.
According to Figure 6b, the optical pathlengths of the ray crossing the core
where, R is the core’s radius, k is the minimum distance between the fiber’s center and the bent ray, ε is the half of the angle determined by the two radii that are enclosing the bent ray inside the graded-index region, and γ is the half of the angle between the incident and the emerged rays. Figure 7 shows the interferograms of LDF GR-IN optical fiber when it was investigated by (a) Pluta and (b) Fizeau interferometers. Figure 8 shows the RIPs calculated by these last models for the LDF optical fiber. The last model, presented in 2001 [50], provided more accurate values of the RIP of a GR-IN optical fiber compared with its previous presented model in Ref. [13].
(a) Pluta duplicated image of LDF GR-IN optical fiber and (b) Fizeau interferogram of the same sample. Reference [50] with permission.
A comparison between RIPs of LDF GR-IN optical fiber using the model in Ref. [27] (dots) and model in Ref. [28] (solid curve) in case of (a) multiple-beam Fizeau interference and (b) two-beam Pluta interference. Ref. [50] with permission.
However, the former requires knowing the function describing the index profile while the aim is to find the parameters of this function.
Optical fibers, which are isotropic materials, can suffer a birefringence under external mechanical bending effects [1, 22, 33, 51]. The induced birefringence can be used in sensing applications [52, 53, 54]. However, bending has an unfavorable effect on the optical fibers used in telecommunications where it, sometimes, causes a mode disturbance and consequently a signal attenuation [55, 56]. An approach to calculate the refractive index profile of a bent optical fiber was proposed where the fiber was divided into layers and slabs simultaneously [22]. The refraction of the optical rays at the liquid-clad and clad-core interfaces was considered. Unfortunately, this approach did not consider the change of refractive index inside each slab. Also, the expected change of refractive index due to the release of stresses near the fiber’s free surface has not been considered. However, this approach succeeded to present good information about the variation of mode propagation due to bending.
In 2014, Ramadan et al. calculated the refractive index and the induced birefringence profiles of bent step-index optical fibers using digital holographic Mach-Zehnder interferometer [33]. In that work, they considered two different processes controlling the variations of the refractive index of the bent fiber: (1) the linear refractive index variation due to the applied stress along the bent radius and (2) the release of this stress on the fiber’s surface. The first one is dominant when approaching the center of the fiber while the second one is dominant near the fiber’s free surface and decays on moving toward the fiber’s center. Figure 9 shows the difference between the paths of optical rays through the bent fiber in the compressed and expanded parts. The stress release was supposed to have a radial dependence on the fiber’s radius, which enabled the construction of 2D RIP of the investigated bent homogeneous optical fiber. Based on the expected stress values due to the bending effect, a function describing the RIP was proposed and used to integrate the optical path of the ray traversing the fiber [50]. By adapting the appropriate parameters of this function, the optical phase differences were estimated and matched those phase differences that were experimentally obtained. By this assumption, a realistic induced stress profile due to bending was obtained [33]. DHPSI was used in that study where the recorded phase shifted holograms were combined and processed to extract the phase map of the fiber [18]. By considering both of the mentioned effects, the following function was chosen to describe the RIP of the bent optical fiber [33].
A schematic diagram shows the path of an optical ray crossing a bent homogeneous optical fiber.
where ρ is the strain-optic coefficient, nbf is the refractive index of the bent-free fiber, R is the radius of bending, ro is the radius of the fiber, ncl is the clad’s refractive index, rs is the proposed parameter to control the distance suffering stress release from the surface of the fiber, and x is the distance between the center of the fiber and the position of the incident ray.
The first term of Eq. (18) gives the bent-induced birefringence,
which is correlated to the generated stress S (r,x) inside the fiber
Eq. (20) evaluates the distribution of stress over the fiber’s cross-section for different bending radii where E is the Young’s modulus of the bent fiber. The signs of Δn are opposite to the signs of tensile and compressive stresses. The tensile stress was chosen to be positive.
Since bending such a step-index optical fiber converts it into a weekly graded-index fiber, Bouguer’s formula [40] was used to correlate the radius, incidence angles, and refractive index of the bent fiber as follows:
where n(x,r) is the refractive index at radius r. By applying this formula at the incidence point, one obtains
This equation was numerically solved to get K satisfying the lower integration limit of the optical path difference for a certain value of x. Based on the model described in Ref. [50], the infinitesimal change in the geometrical distance along the path of the optical ray with respect to the radius variation was given as:
By integration with respect to r, the total path length inside the fiber is:
The optical path length difference between this ray, passed through the fiber, and the reference ray passed through the liquid is:
The phase difference is given as:
Figure 10 shows a set of five shifted holograms of a bent step-index optical fiber with a bending radius R = 8 mm when the incident light was vibrating parallel to the fiber’s axis. They were recorded in order to apply the DHPSI technique and reconstruct the RIP of the bent fiber. The 2π shifted interferogram was analyzed and its reconstructed interference phase map, enhanced phase map, and interference phase distribution are shown in Figures 11a–c, respectively. The refractive index cross-section distribution of the bent optical fiber is shown in Figure 12 while the strain-optic coefficients in compression and expansion were 0.208 and 0.224, respectively.
A set of five shifted interferograms of a bent step-index optical fiber.
(a) The reconstructed interference phase map modulo 2π, (b) its enhanced phase map, and (c) the interference phase distribution.
The refractive index cross-section distribution of the bent optical fiber, R = 8.
In 2017, Ramadan et al. presented a theory to recover the RIP of a bent GR-IN optical fiber inside the core region using DHPSI [35]. They assumed the two different processes controlling the shape of the RIP: (1) the linear variation due to stresses in the direction of the bent radius and (2) the release of the stresses near the fiber’s surface.
The total optical path length of the optical ray crossing the bent GR-IN optical fiber is given by Eq. (27), see Figure 13. The calculated optical path length differences of the interfered rays can be transformed, afterward, into a phase difference map using Eq. (26).
schematic diagram shows the ray tracing in case of traversing bent GR-IN fiber.
with,
Figure 14a shows a set of five phase shifted interferograms for the bent GR-IN optical fiber with bending radius R = 8 mm when the incident light was vibrating parallel to the fier’s axis. The enhanced reconstructed phase modulo 2π and the interference phase distribution of the bent fiber are shown in Figure 14b. Due to the bending process, the GR-IN optical fiber exhibited a birefringence where the RIPs when the incident light vibrated parallel and perpendicular to the fiber’s axis were different, see Figure 15.
(a) A set of five phase shifted interferograms of a bent GR-IN optical fiber. (b) The enhanced reconstructed phase modulo 2π and the interference phase distribution. Ref. [35] with permission.
Refractive index cross-section distribution of the bent GR-IN optical fiber when the incident light vibrates (a) parallel and (b) perpendicular to the fiber’s axis. (c) The birefringence cross-section distribution, R = 8 mm. Ref. [35] with permission.
A PM fiber is any fiber that preserves and transmits the polarization state of the light launched into the fiber even if this fiber is subjected to environmental perturbations [57]. This advantage cannot be verified by conventional single-mode optical fibers outside the laboratory conditions. A PM fiber is tailored to oblige the two orthogonally polarized modes traveling with different velocities (i.e., different propagation constants). This difference in velocities prevents the optical energy from suffering a “cross-coupling” and preserves the polarization state of the transmitted light. Therefore, a PM fiber used in any application requires delivering a polarized light such as in telecommunications, medical applications, and sensing. In interferometric applications, it is used to affirm that the interfered rays have the same polarization states. To maintain such a difference of velocities, the core of the fiber has to be anisotropic either geometrically by making the core cross-section as an ellipse or by applying a uniaxial stress. The most known PM fibers used today are, PANDA, bow tie, and elliptical-jacket fibers. These types are designed by the same way where the cores are flanked by areas of high-expansion glass and shrunk-back more than the surrounding silica then the core is frozen under tension. The birefringence is induced due to this tension, which means creation of two different indices of refraction: a higher index in the direction parallel to the applied stress and a lower index perpendicular to the direction of the applied stress. In the next two subsections, we briefly illustrate both the manufacturing process and interferometric characterization of PANDA and bow tie PM optical fibers.
PANDA PM optical fiber is preferable in telecommunications [57, 58]. It is modified by insertion of stress rods to provide PM properties according to the procedure described in Figure 16. In this process, two holes are ultrasonically drilled along a single-mode optical fiber; then, the stress rods are inserted in these two holes and the fiber is finally drawn [57]. In 2014, Wahba used the off-axis DHPSI to reconstruct the 3D RIP of a PM PANDA optical fiber [23]. The multilayer model was used to calculate the RIP of this fiber in the directions of fast and slow axes. By rotating the PANDA fiber, different interferograms were recorded and analyzed in order to reconstrut the 3D RIP of this fiber, see Figure 17. The reconstructed 3D RIPs of PANDA fiber are shown in Figure 18 when the incident light was vibrating in the direction of (a) fast axis and (b) slow axis.
Manufacturing steps of a PANDA PM optical fiber.
The left column shows three orientations of PANDA PM optical fiber as it was rotated during the characterization process where the slow axis makes an angle (a-i) 0°, (b-i) 45° and (c-i) 90° with the horizontal axis. The middle column shows their reconstructed interference phase modulo 2π while the right column shows their phase difference maps. Ref. [23] with permission.
The 3D RIPs of PANDA PM optical fiber in the directions of (a) fast axis and (b) slow axes. Ref. [23] with permission.
A bow tie optical fiber is fabricated on a lathe using the inside vapor-phase oxidation (IVPO) via the process called gas-phase etching to create the required stress [57]. This process is summarized in Figure 19 where a ring of boron-doped silica is purely deposited of boron tribromide in combination with silicon tetrachloride. The rotation of the lathe stopped when a sufficiently thick layer was formed to allow two diametrically opposed sections to be etched away. The final shape of the bow tie and stress levels are controlled by varying the arc through which the etching burner is rotated. Recently, Ramadan et al. estimated the optical phase variations of optical rays traversing a PM optical fiber from its cross-section images [59]. They proposed an algorithm to recognize the different areas of the fiber’s cross-section, which was immersed in a matching liquid and investigated by Mach-Zehnder interferometer.
Manufacturing steps of a bow tie PM optical fiber.
These areas were scanned to calculate the optical paths for certain values of refractive indices and the optical phases across the PM optical fiber were recovered. The experimental interferograms of the bow tie PM optical fiber, shown in Figure 20, were analyzed to extract their optical phase distributions and compare them with the optimized estimated optical phase maps, see Figure 21. This was a direct and accurate method to get information about refractive index, birefringence, and the beat length of a PM optical fiber.
(a and c) Cross-sections of the bow tie optical fiber. (b and d) Experimentally obtained phase shifted interferograms when the incident light vibrates parallel and perpendicular to fiber’s axis, respectively. Ref. [59] with permission.
The calculated and the experimental phase differences of the bow tie optical fiber when the incident light vibrates (a) parallel and (b) perpendicular to the fiber’s axis. Ref. [59] with permission.
Optical fibers having diameters in the order of 100 μm, or less, are convenient to be investigated using interferometric methods when the samples are put in immersion liquids of refractive indices close to the refractive indices of the fibers as described in the previous sections [12, 13]. Optical fibers of diameters bigger than 150 μm cannot be investigated by normal interferometry where the planes of fringes in both liquid and fiber cannot be focused simultaneously. In 2000, Ramadan presented a novel interferometric method to recover such a problem for homogeneous thick optical fibers, commonly used in short-distance data transmission, without using immersion liquids [16]. This type of interference was called lens-fiber interferometry (LFI) since the interference fringes were produced by a combination of an aberrated cylindrical lens and a thick optical fiber. The aberrated cylindrical lens was used to focus a parallel beam on this fiber, which was located in the focal plane of the cylindrical lens [60], see Figure 22.
The ray tracing diagram of an optical ray crossing a homogeneous thick optical fiber.
Two-beam interference produced by the superposition of two optical rays emerging from the fiber was recorded and explained. Due to the aberration of the cylindrical lens, one of these two rays crossed the thick fiber before its center while the other ray crossed after the fiber?s center. Therefore, for each point in the image plane, two rays having two different initial incidence angles on the thick fiber are superposed, see Figure 23. The optical path length of each ray can be obtained by tracing this ray geometrically, as given by Eq. (30), which can be transformed into phase differences for the interfered rays using Eq. (31). The difference in the optical path lengths of each pair of interfered rays can be transformed into an intensity distribution describing the interference fringes using Eq. (32). On the other hand, the scattered rays from the outer surface of the fiber do not contribute in the interference because of the limited range of the incident rays on the fiber. This is in contrast with previous works done by Watkins [14, 15, 61]. By comparing the experimentally obtained interferograms with those reconstructed theoretically as shown in Figure 24, Ramadan was able to determine the refractive index of the investigated thick optical fiber. The advantage is that the used system requires no matching liquid where the experiment is performed when the thick fiber is just held in air. This enables monitoring the probable variation in radius or refractive index of the fiber particularly during the manufacturing process or under external effects.
The relation between the position of each two interfered rays on the screen and their incidence angles on the thick fiber.
(a) A selected and extended part of the obtained interferogram of a thick optical fiber, (b) the enhanced fringes of (a) and (c) the simulated fringes.
where Δ(z1) and Δ(z2) are the optical path lengths of the two interfered rays. In 2004, Hamza et al. developed LFI technique in order to determine the refractive index of the core of a skin-core thick optical fiber [60]. They derived a mathematical expression for the optical paths through the fiber in order to reconstruct the interfernce pattern due to the used fiber when it is used as a thick fiber in the LFI system. By comparing the experimentally obtained patterns with the theoretically reconstructed ones, they were able to estimate the core’s refractive index with an accuracy of 8 × 10−4. Due to its simplicity and applicability, LFI was used, afterward, to measure the refractive index of a liquid [62] and to monitor the thickness variations of a transparent sheet inserted between the cylindrical lens and the thick fiber [63].
This chapter is an attempt to highlight the interferometric techniques used for characterization of optical fibers. Application of two- and multiple-beam interference on different types of fibers is illustrated. Section 2 dealt with conventional optical fibers where we illustrated the theoretical models used to reconstruct the refractive index profiles of these fibers. In these models, the refraction of the light ray traversing the fiber has been considered. Digital holography was explained as an important candidate used for accurate retrieving of phase maps and consequently refractive index profiles of the fibers. In Section 3, we mentioned the problem of fiber bending. Recovering the refractive index profile and mode propagation of a bent fiber considering the refraction of the light rays traversing the fiber is a quite difficult task since bending-induced stresses are responsible for refractive index variations. Also, these stresses are released at the outer surface of the bent fiber. Therefore, we illustrated a successful model that was recently presented to recover the index profile in this case with experimental illustrative data. Another important type of optical fibers is the polarization maintaining optical fibers, which prevent cross-coupling by conserving the state of beam polarization during propagation. In Section 4, we presented interferometric techniques applied on two different polarization maintaining optical fibers, panda and bow tie, to reconstruct their refractive index profiles. Most interference techniques require immersing the fiber in a suitable liquid in order to minimize the phase difference between the fiber and its surrounding medium. In Section 5, an interference technique is presented and applied on a thick optical fiber to recover its refractive index without using an immersion liquid (i.e., in air), which makes the technique suitable for in-situ studying of thick fibers.
The authors would like to acknowledge Prof. A. Hamza, the leader of optics research groups in Mansoura and Damietta Universities, and Prof. T. Sokkar for their continuous support and useful discussions. Also, many thanks to the Optics Research Group members in Damietta University for their useful suggestions and comments.
The authors declare no conflict of interest.
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