• Title/Summary/Keyword: Gas Chromatographic Analysis

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Constructing Database for Drugs and its Application to Biological Sample by HPTLC and GC/MS (HPTLC와 GC/MS를 이용한 의약품의 데이타베이스화 및 생체시료에의 응용)

  • Yoo, Young-Chan;Park, Sung-Woo;Lim, Mie-Ae;Baeck, Seung-Kyung;Park, Seh-Youn;Lee, Ju-Seon;Lho, Dong-Seok
    • Analytical Science and Technology
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    • v.13 no.2
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    • pp.136-150
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    • 2000
  • For the identification of unknown drugs in biological samples, we attempted rapid high performance thin layer chromatographic method which is sensitive and selective chromatographic analysis of high performance thin layer chromatography (HPTLC) with automated TLC sampler and ultra-violet (UV) scanner. We constructed HPTLC database (DB) on two hundred five drugs by using the data of Rf values and UV spectra (scan 200-360 nm) as well as gas chromatography/mass spectrometry (GC/MS) DB on ninety six drugs by using the data of relative retention time (RRT) on lidocain and mass spectra. After extracting drugs in biological sample by solid phase extraction (Clean Screen ZSDAU020), we applied them to HPTLC and GC/MS DB. Drugs, especially extracted from biological samples, showed good matching ratio to HPTLC DB and these drugs were confirmed by GC/MS. In conclusion, this DB system is thought to be very useful method for the screening of unknown drugs in biological samples.

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High-Performance Liquid Chromatographic Determination of Phenothrin and Silafluofen Residues in Crops with Mass Spectrometric Confirmation (고성능 액체크로마토그래피와 질량분석법을 이용한 농산물 중 Phenothrin 및 Silafuofen의 정밀 잔류분석법 개발)

  • Lee, Young-Deuk;Oh, Jae-Ho;Jang, Sang-Won
    • The Korean Journal of Pesticide Science
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    • v.15 no.4
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    • pp.389-400
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    • 2011
  • A high-performance liquid chromatographic (HPLC) method was developed to determine residues of phenothrin and silafluofen, known as synthetic pyrethroids, in agricultural commodities. Insecticide residues were extracted with acetone from representative samples of four crops which comprised rice, apple, pepper and cabbage. The extract was purified serially by liquid-liquid partition and Florisil column chromatography. For rice and pepper samples, acetonitrile/n-hexane partition was additionally adopted to remove nonpolar interferences. Reversed phase HPLC using an octadecylsilyl column was successfully applied to separate two phenothrin isomers and silafluofen from sample co-extractives. Intact parent compounds were sensitively detected by ultraviolet absorption at 226 nm. Recovery experiment at the quantitation limit validated that the proposed method could apparently determine phenothrin and silafluofen residues at 0.02 and 0.01 mg/kg, respectively. Mean recoveries of phenothrin and silafluofen from four crop samples fortified at three levels in triplicate were in the range of 82.4~109.8% and 83.7~109.8%, respectively. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types and spiking levels. A selected-ion monitoring (SIM) LC/mass spectrometry (MS) with electrospray ionization was provided to confirm the suspected residue of phenothrin, even though no sufficient ionization of silafluofen was obtained. Both phenothrin and silafluofen could be successfully confirmed by gas chromatography/MS SIM with electron impact at 70 eV. The proposed method is sensitive, repeatable and rapid enough to apply to officially routine inspection of agricultural products.

Gas Chromatographic Analysis on the Residual of Fungicide Fenhexamid in Crops(Cucumber, Strawberry and Grape) (작물(오이, 딸기, 포도) 중 살균제 Fenhexamid의 잔류성에 대한 기체 크로마토그래피 분석)

  • Han, Seong-Soo;Lo, Seog-Cho;Kim, Won-Ju;Park, PiII-Jae;Kim, Il-Kwang
    • Analytical Science and Technology
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    • v.16 no.1
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    • pp.70-77
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    • 2003
  • The optimum conditions for the residue analysis of hydroxyanilide fungicide fenhexamid on cucumber, strawberry and grape were investigated by gas chromatography equipped with electron capture detector (GC-ECD) and the residual amount was determined by sprayed days before harvest. Each samples were extracted with acetone, filtered and concentrated to 50 mL. The concentrated extracts were transferred to dichloromethane and then thoroughly concentrated. The concentrated phase was loaded on the filtration column stuffed with silica gel and purified with acetone:hexane (5:95, 15:85, v/v) mixed solvent. The regression equation and linearity of the standard calibration curves between 0.05~2.00 ng were as follows : cucumber; Y=312.40X+10.26, $R^2=0.9996$, strawberry; Y=313.33X+5.54, $R^2=0.9998$, grape; Y=253.27X-2.23, $R^2=0.9994$. From the standard additional experiments with 0.10 mg/L and 0.40 mg/L, the average recoveries of cucumber, strawberry and grape were 94.8%, 88.1% and 93.7%, respectively and the detection limits were all the same as 0.01 mg/L. Residual amounts in crops were ranged from 0.01 to 0.58 mg/L.

Gas Liquid Chromatographic Analysis of Fatty Acids in Ginseng Products (Gas Liquid Chromatography에 의한 인삼(人蔘) 제품(製品) 중의 지방산(脂肪酸) 분석(分析))

  • Yoon, Tai-Heon;Kim, Eul-Sang
    • Korean Journal of Food Science and Technology
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    • v.11 no.3
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    • pp.182-187
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    • 1979
  • Six commercial ginseng products, red ginseng, white ginseng I and II, red ginseng extract, white ginseng extract I and II were extracted with ethyl ether. Total fatty acid composition of the extracted free lipids was analyzed by gas liquid chromatography and digital integrator was used to measure the area of each peak. Crude lipid contents of red and white ginsengs were similiar. Those of red ginseng extract, white ginseng extract I and II were 1.10, 1.13 and 0.40%, respectively. It was found that 22 kinds of fatty acids existed in red and white ginsengs. Among them, 16 kinds of even numbered fatty acids were identified. Linoleic acid in red and white ginsengs was the most abundant. The contents of that in red ginseng, white ginseng I and II were 63.33, 45.55 and 41.06%, respectively. The next most abundant acid was palmitic acid, the contents of which were 11.30, 14.4 and 18.10% for red ginseng, white ginseng I and II, respectively. Major fatty acids for red ginseng extract and white ginseng extract I were linoleic and palmitic acids in the same order of magnitude. Linoleic and palmitic acids for red ginseng extract were 15.93 and 15.71 %, respectively, while linoleic and palmitic acids for white ginseng extract I were 21.94 and 19.15%, respectively. However, white ginseng extract II contained only 9.21% of linoleic acid and 16.13% of palmitic acid which was the major fatty acid.

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Optimization of Analytical Methods for Octacosanol in Related Health-functional Foods with GC-MS (GC-MS를 이용한 건강기능식품 중 옥타코사놀 분석법 개발 연구)

  • Lee, Jin Hee;Oh, Mi Hyune;Lee, Kyung Jin;Kim, Yang Sun;Keum, Eun Hee;Park, Ji Eun;Cho, Mee Hyun;Seong, Min Hye;Kim, Sang A;Kim, Mee hye
    • Journal of Food Hygiene and Safety
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    • v.33 no.4
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    • pp.266-271
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    • 2018
  • The Ministry of Food and Drug Safety (MFDS) is amending its test methods for health-functional foods (dietary food supplements) to establish regulatory standards and specifications in Korea. In this regard, we continue our research on developing analytical methods for the items. Octacosanol is the major component of polycosanol and is a high-molecular-mass primary fatty alcohol, obtained from sugar cane wax. Previous researchers have shown that octacosanol can lower cholesterol and has antiaggregatory properties, cytoprotective uses, and ergogenic properties for human health. Recently, octacosanol products have been actively introduced into the domestic market because of their functional biological activity. We have developed a sensitive and selective test method for octacosanol that the TMS derivatives by means of gas-chromatographic-tandem mass spectrometry (GC-MS). The trimethylsilyl ether derivative of the target analyte showed excellent chromatographic properties. The procedure was validated in the range of $12.5{\sim}200{\mu}g/L$. Standard calibration curves presented linearity with the correlation coefficient ($r^2$) > 0.999, and the limits of detection (LOD) and limits of quantitation (LOQ) were $4.5{\mu}g/L$ and $13.8{\mu}g/L$, respectively. The high recoveries (92.5 to 108.8%) and precision (1.8 to 2.4%) obtained are in accordance with the established validation criteria. Our research can provide scientific evidence to amend the octacosanol test method for the Health-Functional Food Code.

Distribution and Content of Geometric Isomers of Conjugated Linoleic Acid in Dairy Foods from the Quebec Province of Canada

  • Park, Seung-Yong;Ahn, Jae-Eun;Kim, Geun-Bae;Jung, Mun-Yhung;Lee, Byong-H.
    • Food Science and Biotechnology
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    • v.17 no.1
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    • pp.31-37
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    • 2008
  • The distributions and content of geometrical isomers of conjugated linoleic acids (CLA) in dairy foods such as milk, yogurt, and cheese, produced or being sold in the Quebec province of Canada, were investigated by gas chromatographic analysis. The mean contents of total CLA (mg/g fat) were $5.06{\pm}0.74$ in 4 low-fat milk samples, $14.14{\pm}4.95$ in 6 yogurt samples, and $18.22{\pm}7.89$ in 5 natural ripened cheeses. Among the yogurt samples, YY contained the highest content of total CLA ($20.68{\pm}5.17\;mg/g$ fat). Among the cheese samples, Gruyere contained the highest amount of total CLA ($29.86{\pm}0.62$) as well as c-9,t-11 ($22.03{\pm}0.36\;mg/g$ fat), followed by Jarlsberg ($22.76{\pm}0.14$), Provolone ($16.42{\pm}0.52$), Cheddar ($13.83{\pm}0.81$), and Swiss ($8.23{\pm}1.11$). Based on the distribution ratios of CLA isomers in these dairy foods, the c-9,t-11 isomer appeared to be the major CLA isomer in both the low-fat milk ($89.87{\pm}2.39%$) and yogurt ($90.98{\pm}4.42%$). In the cheeses, however, the ratio of c-9,t-11 ($54.86{\pm}13.06%$) was slightly higher than that of c-10,c-12 ($40.81{\pm}13.40%$).

Development of a Rapid Method for the Screening of Conjugated Linoleic Acid (CLA)-Producing Strains of Bifidobacterium breve

  • Choi, Sun-Hae;Lee, Kyoung-Min;Kim, Kwan-Hu;Kim, Geun-Bae
    • Food Science of Animal Resources
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    • v.38 no.4
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    • pp.806-815
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    • 2018
  • This study was performed to isolate some strains of Bifidobacterium breve from fecal materials of neonates and to screen them for the biotransformation activity of converting linoleic acid into conjugated linoleic acid (CLA). Fecal samples were collected from twenty healthy neonates between 14 and 100 days old, and four hundred colonies were randomly selected from a Bifidobacterium selective transoligosaccharide medium. A duplex polymerase chain reaction technique was developed for the rapid and accurate molecular characterization of the B. breve strains that have been reported to show the species-specific characteristic of CLA production. They are identified by 16S ribosomal DNA, fructose-6-phosphate phosphoketolase encoding genes (xfp), and rapid pulsed field gel electrophoresis. Thirty-six isolates were identified as B. breve, and just two of the 12 neonates were harboring B. breve strains. Each isolate showed different CLA-producing ability in the spectrophotometric assay. All of the positive strains from the primary spectrophotometric assay were confirmed for their CLA-producing activities using gas-chromatographic analysis, and their conversion rates were different, depending on the strain isolated in this study. Some strains of B. breve were successfully isolated and characterized based on the CLA-producing activity, and further studies are necessary to characterize the enzyme and the gene responsible for the enzyme activity.

Isolation and Characterization of Mucous Exopolysaccharide (EPS) Produced by Vibrio furnissii Strain VB0S3

  • Bramhachari P.V.;Kishor P.B. Kavi;Ramadevi R.;Kumar Ranadheer;Rao, B. Rama;Dubey Santosh Kumar
    • Journal of Microbiology and Biotechnology
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    • v.17 no.1
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    • pp.44-51
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    • 2007
  • Marine bacterial strains were isolated trom coastal regions of Goa and screened for the strains that produce the highest amount of mucous expolysaccharide (EPS). Our screening resulted in the identification of the strain Vibrio furnissii VB0S3 (hereafter called VB0S3), as it produced the highest EPS in batch cultures during the late logarithmic growth phase. The isolate was identified as VB0S3 based on morphological and biochemical properties. Growth and EPS production were studied in mineral salts medium supplemented with NaCl (1.5%) and glucose (0.2%). The exopolymer was recovered from the culture supernatant by using three volumes of cold ethanol precipitation and dialysis procedure. Chemical analyses of EPS revealed that it is primarily composed of neutral sugars, uronic acids, and proteins. Fourier-transform infrared (FT-IR) spectroscopy revealed the presence of carboxyl, hydroxyl, and amide groups, which correspond to a typical heteropolymeric polysaccharide, and the EPS also possessed good emulsification activity. The gas chromatographic analysis of an alditol-acetate derivatized sample of EPS revealed that it was mainly composed of galactose and glucose. Minor components found were mannose, rhamnose, fucose, ribose, arabinose, and xylose. EPS was readily isolated from culture supernatants, which suggests that the EPS was a slime-like exopolysaccharide. This is the first report of exopolysaccharide characterization that describes the isolation and characterization of an EPS expressed by Vibrio surnissii strain VB0S3. The results of the study contribute significantly and go a long way towards an understanding of the correlation between growth and EPS production, chemical composition, and industrial applications of the exopolysaccharide in environmental biotechnology and bioremediation.

Evaluation of Polychlorinated Biphenyls(PCBs) and Organochlorine Insecticide Residues in Irrigation Waters in the Periphery of Suwon (수원근교(水原近郊) 관개수중(灌漑水中)의 PCBs 및 유기염소계(有機鹽素系) 살충제(殺蟲劑)의 잔류평가(殘留評價))

  • Lee, Youn-Hyung;Hwang, Eul-Chul;Park, Chang-Kyu
    • Korean Journal of Environmental Agriculture
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    • v.4 no.2
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    • pp.95-101
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    • 1985
  • Water samples collected monthly between November 1982 and October 1983 from seven reserviors and a river in the periphery of Suwon, Korea were subjected to gas chromatographic analysis for PCBs and organochlorine insecticide residues. PCBs were positively detected in the most samples. The average residue levels of PCBs were found in the range of 0.009${\sim}$0.5 ppb while those of organochlorine insecticides were in the range of "not detected"${\sim}$0.008 ppb. The ratio of average residue levels of PCBs to those of total DDT was found to vary with sampling sites. The highest ratio of 500 was found in the water samples of Han River and the lowest in water of Won-chun Reservior. Both industrial and urban waste appear to be responsible for PCBs in the irrigation waters.

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The Effects of Starch Addition on Acid Production By Lactic Acid Bacteria and Quality of Curd Yogurt (전분의 첨가가 호상요구르트에서 젖산균의 산생성과 요구르트의 품질에 미치는 영향)

  • Em, Sung-Sin;Yoo, Ji-Chang;Ko, Young-Tae
    • Korean Journal of Food Science and Technology
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    • v.25 no.6
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    • pp.747-752
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    • 1993
  • A curd yogurt was prepared from milk added with skim milk powder or four kinds of starch such as rice starch, wheat starch, corn starch and potato starch. The effects of starch addition at 2%(w/v) level on acid production by lactic acid bacteria in milk was investigated. The effects of starch addition on quality of curd yogurt in terms of apparent viscosity, sensory property and volatile aroma compounds were also examined. Addition of starch markedly stimulated the acid production by lactic acid bacteria. Among four organisms tested, Lactobacillus jugurti produced the highest amount of acid. Apparent viscosity of curd yogurt added with starch was significantly higher than that of control. Curd yogurt fermented with L. jugurti showed pseudoplastic and thixotropic characteristics. Sensory property of curd yogurt added with corn starch or rice starch was evaluated as slightly better than reference sample, but that with potato starch was evaluated as the worst among all samples. Acetaldehyde, acetone, ethanol and butanol were detected by gas chromatographic analysis.

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