• Title/Summary/Keyword: HPLC separation

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Simultaneous Determination of Quinolones in Flatfish and Egg Using liquid Chromatography with Fluorescence Detection (액체크로마토그래피를 이용한 광어 및 계란 중 퀴놀론계의 동시분석법 개발)

  • Lee, Sang-Hee;Shim, You-Shin;Kim, Hyun-Ju;Choi, Yoon-Hee;Shin, Dong-Bin
    • Journal of Food Hygiene and Safety
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    • v.23 no.4
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    • pp.324-329
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    • 2008
  • An analytical method for the simultaneous determination of nine quinolones (QNs) namely, marbofloxacin, norfloxacin(IS), ciprofloxacin, danofloxacin, enrofloxacin, sarafloxacin, difloxacin, oxolinic acid, and flumequine in flatfish and egg was developed and validated using liquid chromatography with fluorescence detection (LC-FD). The samples were extracted using a traditional liquid-liquid extraction process; deproteinization was accomplished by the addition of trichloroacetic acid and acetonitrile (ACN), and defatting was performed with hexane. Chromatographic separation was achieved on a reverse phase C8 column with gradient elution using a mobile phase of 200 mM ammonium acetate buffer (pH 4.5) and ACN. The proposed method was validated according to the CODEX guideline. Mean recoveries of QNs from flatfish and egg were 89.6-106.5% with relative standard deviations (RSDs) below 15% at three different concentrations of 50, 100 and $500{\mu}g/kg$. Linearity was obtained with a correlation coefficient ($r^2$) of 0.9989-1.0000. The LOD for the investigated QNs was $1-16{\mu}g/kg$ depending on flatfish and egg. The present method can be applied simultaneously to determine QNs in muscle of flatfish and egg.

The Determination of Perfluorooctane sulfonate in Food Packing Materials by HPLC-MS/MS (식품 포장재 중의 퍼플루오르옥탄설포네이트 분석)

  • Kim, Il-Young;Kim, Au-Kyoung;Jung, Bo-Kyoung;Shin, Young;Kim, Ji-Young;Kim, Jung-Han;Chae, Young-Zoo
    • Journal of Food Hygiene and Safety
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    • v.28 no.4
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    • pp.376-380
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    • 2013
  • Determination of PFOS in instant food packing materials by LC-MS/MS was developed. The procedure involves an extraction of the Food Packing Materials with 100% methanol soxcelet extraction method. The LC separation was performed by Hypersil Gold ($150mm{\times}2.1mm$ 5 um) with mobile phases of 2 mM amoniumacetate solution and acetonitrile. The Mass spectral acquisition was done in negative ESI/SRM using the TSQ Quantum Ultra. With this method, good linear relationship, sensitivity and reproducibility were obtained. The rate of recoveries of PFOS from paper material spiked with 1.0 ug/L were 99.84%, respectively. The limit of quantitation and limit of detection were below 0.03 ug/L and 0.009 ug/L. The method had been applied to determination of PFOS in instant food packing materials.

Action Patterns of Chitinase and Separations of Chitooligosaccharides Produced by Chitinolytic Hydrolysis (키티나제에 의한 키토올리고당의 생성활성 규명과 올리고당의 당별 분리 생산)

  • Kim, Kwang
    • KSBB Journal
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    • v.17 no.1
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    • pp.100-105
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    • 2002
  • N-acetyl-D-glucosamine oligosaccharides [(GlcNAc)n] whose degree of polymer-ization is from one to ten (n=1-10) were fractionated by column chromatography on CM-Sephadex. Electro dialysis from a partially deacetylated chitosan hydrolysate prepared crudely with the N-acetyl-D-glucosaminidase(chitinase) and exo-N, N'-diacetylchito-biohydrolase(chitobiase) of Serratia marcescens QM B1466. Reducing sugar compositions and sequences of the N-acetyl-glucosamine oligosaccharides were identified by N-acetylation, randomly cleavage with chitinase and ego-splitting with chitobiase. N-acetyl-glucosamine heterochitooligosaccharides with glucosamine oligosaccharides, (GlcN)n at the reducing end residues together with $(GlcN)_1\sim(GlcN)_4$ were detected. Separation was accomplished by prefractionation with election by 0 to 1.0 M NaCl gradient solution. $(GlcNAc)_1 =4.25%,\; (GlcNAc)_2=4.49%,; (GlcNAc)_3=11.1%,\; (GlcNAc)_4=2.5%,$$ $(GlcNAc)_{5}$=0.64%, $(GlcNAc)_{6}$=2.12% and $(GlcNAc)_{7}$=1.21%, respectively, were crystallized after electrodialysis and lyophilization Each N-acetyl-D-glucosamine oligosaccharides content were detected by HPLC.

Changes of saccharide content in fruitbody composition of Flammulina velutipes during storage (팽이버섯의 저장기간 및 품종별 자실체내의 당 함량 변화)

  • Jhune, Chang-Sung;Yun, Hyung-Sik;Leem, Hoon-Tae;Kong, Won-Sik;Lee, Kang-Hyo;Sung, Gi-Ho;Cho, Jae-Han
    • Journal of Mushroom
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    • v.9 no.3
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    • pp.123-131
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    • 2011
  • Winter mushroom was monitored to investigate the influence of storage temperature on its quality during the storage and distribution phase. In measuring its quality, the contents of saccharides were quantified with its fruiting bodies using HPLC. Although it has been known to be difficult to separate saccharide isomers, our results indicated that Grace Prevail carbohydrate ES $5{\mu}column$ was the best in the separation to analyze the saccharide out of six columns used in this study. In our results, xylose was the main component of saccharide in the fruiting body of winter mushroom(White line mushroom:47.68mg/g, brown line mushroom: 63.28mg/g). In long-term storage, the total amount of saccharide tended to increase, but trehalose content of the disaccharide decreased. In comparison with the paramount amount of lactose and myo-inositol contents in long-term storage at $4^{\circ}C$, lactose wasn't detected when stored at $-1^{\circ}C$.

A Study on the Elution Behavior of Pd-Isonitroso ethylacetoacetate imine Chelates by Reversed-phase High Performance Liquid Chromatography (역상 고성능 액체 크로마토 그래피에 의한 Pd(II) - isonitrosoethylacetoacetate imine 유도체 킬레이트의 용리거동에 관한 연구)

  • Kim, Hyun
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.19 no.1
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    • pp.20-30
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    • 1993
  • Liquid Chromatographic behavior of Pd(II) in Isonitosoethylacetoacetate imine IEAA-NR: R=H, CH3, C2H5, n-C3H7, n-C4H9, C6H5-CH2) Chelates were investigated by reversed phase high performance 1iquid chromatography on Micropak MCH-5 Column using Methanol /water as mobile phase. The optimum condition for the separation of Pd-Isonitrosoethylacetoacetate imine chelates were examined with respect to the flow rate, mobile phase strength. It was found that Pd(IEAA-NR)2 chelates were eluted in an acceptable range of the capacity factor value (0 $\leq$ log k' $\leq$ 1), The dependence of the logarithm of capacity factor(k') on the volume fraction of water in mixture with in the binary mobile phase was examined. Also, the dependence of k'on the liquid-liquid extraction distribution constant in methanol-water / n-alkane extraction system was on system was invert tigated for Pd(IEAA-NR)2. Both kinds of dependence are linear, which suggests that the retention of the electroneutral metal chelates be largely due to the solvophobic effect.

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Identification of C3G(cyanidin-3-glucoside) from Mulberry Fruits and Quantification with Different Varieties (오디에서 C3G(cyanidin-3-glucoside)의 분리, 동정 및 계통별 함량분석)

  • 김현복;김선림
    • Journal of Sericultural and Entomological Science
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    • v.45 no.2
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    • pp.90-95
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    • 2003
  • This study was carried out to identify of C3G (cyanidin-3-glucoside) from mulberry fruits and quantify with different varieties. C3G of mulberry fruits was extracted with 1% HCl-MeOH and purified with open column (5${\times}$90cm) which filled with Amberlite IRC-50 ion exchange resin. The $\lambda$max ranges of the purified C3G on UV/vis spectrum were 516nm and 280nm. Also, molecular weight of C3G from mulberry fruits by LC-Mass was determined as 449. From above results, we concluded that anthocyanin pigment of mulberry fruits was C3G only. The cyanidin-3-glucoside (C3G) was separated and quantified by High Performance Liquid Chromatography (HPLC) system using a Nova-Pack C$\_$18/ column. Mean content of the 35 tested accessions was 0.89%. Also fruity characteristics as well as C3G content to select the desirable mulberry varieties for the production of fruit were researched and analyzed. We selected three suitable varieties such as 'Susungppong', 'Kangsun', and 'Jeolgokchosaeng(Chungpuk)'.

Development and validation of an LC-MS/MS method for the simultaneous analysis of 26 anti-diabetic drugs in adulterated dietary supplements and its application to a forensic sample

  • Kim, Nam Sook;Yoo, Geum Joo;Kim, Kyu Yeon;Lee, Ji Hyun;Park, Sung-Kwan;Baek, Sun Young;Kang, Hoil
    • Analytical Science and Technology
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    • v.32 no.2
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    • pp.35-47
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    • 2019
  • In this study, high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was employed to detect 26 antidiabetic compounds in adulterated dietary supplements using a simple, selective method. The work presented herein may help prevent incidents related to food adulteration and restrict the illegal food market. The best separation was obtained on a Shiseido Capcell Pak(R) C18 MG-II ($2.0mm{\times}100mm$, $3{\mu}m$), which improved the peak shape and MS detection sensitivity of the target compounds. A gradient elution system composed of 0.1 % (v/v) formic acid in distilled water and methanol at a flow rate of 0.3 mL/min for 18 min was utilized. A triple quadrupole mass spectrometer with an electrospray ionization source operated in the positive or negative mode was employed as the detector. The developed method was validated as follows: specificity was confirmed in the multiple reaction monitoring mode using the precursor and product ion pairs. For solid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL, and for liquid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL. Satisfactory linearity was obtained from calibration curves, with $R^2$ > 0.99. Both intra and inter-day precision were less than 13.19 %. Accuracies ranged from 80.69 to 118.81 % (intra/inter-day), with a stability of less than 14.88 %. Mean recovery was found to be 80.6-119.0 % and less than 13.4 % RSD. Using the validated method, glibenclamide and pioglitazone were simultaneously determined in one capsule at concentrations of 1.52 and 0.53 mg (per capsule), respectively.

Survey of Beet Red Contents in Foods using TLC, HPLC (TLC, HPLC를 이용한 식품 중 비트레드 함량조사)

  • Jang, Yaung-Mi;Lee, Tal-Soo;Hong, Ki-Hyoung;Park, Sung-Kwan;Park, Sung-Kug;Kwon, Yong-Kwan;Park, Jae-Seok;Chang, Sun-Young;Hwang, Hye-Shin;Kim, Eun-Jeong;Han, Yeun-Jeong;Kim, Byung-Sub;Won, Hye-Jin
    • Journal of Food Hygiene and Safety
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    • v.20 no.4
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    • pp.244-252
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    • 2005
  • This study was performed far development of new analytical method of beet red in foods. In this study, analysis of beet red in foods has been carried out by detection of betanine and isobetanine, the main color component of beet red as indicator compounds. The qualitative analysis technique consisted of clean-up of the colors with a $C_{18}$ cartridge, separation of the colors by cellulose TLC plate using acetone:3-methyl-1-butanol:distilled water (7:7:6) as a solvent system. Also, the quantitative analysis was performed using X-terra RP at wavelength 538 nm and $0.1\%$ phosphoric acid : methanol (90:10) as a solvent. The quantitative results of beet .ed were as follows:900.22$\∼$27701.60 $\mu$g/g for 60 item in nutrient supplement food, $21.95\∼713.40{\mu}g/g$ for 30 items and N.D. for 18 items in cindy, and $155.85{\∼}505.37{\mu}g/g$ for 12 items in ice creams, $43.52\∼64.75{\mu}g/g$ for 18 items and N.D. for 54 item in sauce, N.D. for 12 items in retort food.

Simultaneous Determination of 8 Preservatives (6 Parabens, 2-Phenoxyethanol, and Chlorphenesin) in Cosmetics by $UPLC^{TM}$ ($UPLC^{TM}$를 이용한 화장품 중 보존제 8종(파라벤 6종, 페녹시에탄올, 클로페네신)의 동시분석)

  • Park, Jeong-Eun;Lee, So-Mi;Jeong, Hye-Jin;Chang, Ih-Seop
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.33 no.4
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    • pp.263-267
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    • 2007
  • Parabens are used in nearly all types of cosmetics and toiletries because they are formulated well and have broad spectrum of activity, interness, low costs and excellent chemical stability in relation to pH. 2-phenoxyethanol and chlorphenesin are common preservatives which are usually used in combination with parabens in cosmetics. Toxicity of parabens is generally low but application of parabens to damaged or broken skin has resulted in sensitization. Moreover, the possibility of their estrogenic potential, anesthetic effects and reproductive toxicity has been reported. Consequently there are some regulations in use of parabens. And the maximum permitted concentrations of chlorphenesin and 2-phenoxyethanol in cosmetic products are authorized by the same reasons. So it is important to control and estimate the amount of parabens in products. In this article, we proposed a valid method for the simultaneous determination of 8 preservatives including parabens in a short time using ultra performance liquid $chromatography^{TM}\;(UPLC^{TM})$. Separation of eight components was achieved in less than 10 min and resolutions were reasonable (USP resolution ${\geqq}\;2$). And limit of detection and quantification were evaluated. The method was suitably validated for specificity, linearity, precision (repeatability, intermediate precision) and accuracy for assay (recovery) based on International conference on harmonisation (ICH) guideline. The method was applicable to analysis of preservatives in cosmetic products.

Extraction & Purification of ${\beta}$-carotene from Recombinant Escherichia coli (재조합 대장균으로부터 고순도 베타-카로틴의 추출 및 정제)

  • Jo, Ji-Song;Nguyen, Do Quynh Anh;Yun, Jun-Ki;Kim, Yu-Na;Kim, You-Geun;Kim, Sung-Bae;Seo, Yang-Gon;Lee, Byung-Hak;Kang, Moon-Kook;Kim, Chang-Joon
    • Microbiology and Biotechnology Letters
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    • v.37 no.3
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    • pp.231-237
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    • 2009
  • This paper aimed to develop a solvent extraction and purification process to recover high-purified ${\beta}$-carotene from recombinant Escherichia coli. Cells harvested from the culture broth were treated through numerous steps: dehydration, solvent extraction, crystal formation and separation. To optimize the extracting condition, experiments were carried out to investigate the effect of cell disruption, temperature, organic solvents, solvent-biomass ratio on the yield of ${\beta}$-carotene extracted from cells. The result indicated that no significant differences of extraction yield were observed from cells with or without step of cell disruption. Among different extracting solvents, the highest extraction yield of ${\beta}$-carotene, 30.3 mg-${\beta}$-carotene/g-dry cells, was obtained with isobutyl acetate at solvent-biomass ratio 25 mL/g-dry cells at $50^{\circ}C$. Notably, in case of acetone, the extraction yield was quite low when using acetone itself, but increased almost up to the highest value when combining this solvent and olive oil. The purity of ${\beta}$-carotene crystals obtained from crystallization and separation was 89%. The purity degree was further improved up to 98.5% by treating crude crystals with additional ethanol washing.