• Title/Summary/Keyword: Liquid Liquid Extraction

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Simultaneous detection of residual fungicide in Bean Sprouts by Solid-phase Extraction (고체상 추출법에 의한 콩나물 중의 잔류농약 동시 검출)

  • Lee, Myunghwoon;Lee, Taejoon;Pyo, Dongjin
    • Analytical Science and Technology
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    • v.6 no.5
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    • pp.509-514
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    • 1993
  • Benomyl, topsin-M and thiram been known as one of the seed disinfectant. For these studies benomyl, topsin-M and thiram simultaneously had been analyzed by high performance liquid chromatographic method using ODS cartridge, benomyl, topsin-M and thiram was chromatographed using an ODS column and eluent 40% Acetonitrile at a flow rate of 1ml/min. The UV Detector responses at 276nm.

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Optimization of Solid Phase Extraction Method for Quantitative Analysis of Perfluorooctanoic Acid in Serum using Liquid Chromatography-Tandem Mass Spectrometry

  • Lee, Hyun-Seok;Yim, Yong-Hyeon
    • Mass Spectrometry Letters
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    • v.5 no.1
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    • pp.30-33
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    • 2014
  • A solid phase extraction (SPE) method was optimized for the quantitative analysis of perfluorooctanoic acid (PFOA) in serum using hydrophilic-lipophilic balance SPE and LC-MS/MS. Fetal bovine serums spiked with $^{13}C_8$-PFOA before or after SPE were used as test samples for evaluation of the SPE efficiency. Simultaneous evaluation of matrix effects and absolute SPE recovery for $^{13}C_8$-PFOA in serum using different sample pre-treatments and SPE conditions allowed optimization of SPE process efficiency with minimal matrix effect and decent SPE recovery. Introduction of protein precipitation as a sample pre-treatment procedure for serum samples before SPE generally decreased matrix effect in LC-MS/MS analysis and provided more stable recovery of PFOA.

Comparative Study on the HPLC Determination of Aflatoxins Coupled with Extraction and Clean-up Methods (Aflatoxin 분석법에 관한연구;추출 및 정제방법의 비교)

  • 김종규
    • Journal of Food Hygiene and Safety
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    • v.8 no.4
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    • pp.251-254
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    • 1993
  • Extraction and Clean-up procedures coupled with quantitation by high performance liquid chromatography(HPLC) was evaluated for the detection of 4 aflatoxins, B1, B2, G1 and G2, in peanut butter. The Sep-pak clean-up method showed poorer separation and repeatability than did the modified DeVries' and an immunoaffinity column clean-up methods. No significant difference of detected aflatoxins between the affinity column clean-up and modified DeVries' method. The coefficients of variation for the 4 aflatoxins were ranging from 6.3∼32.3 by the modified DeVries' method and 5.3∼9.8 by the affinity column clean-up.

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Extraction and Characterization of an Anti-wrinkle Elastase Inhibitor from Rheum undulatum L. (대황(Rheum undulatum L.)으로부터 항주름성 Elastase 저해제의 추출 및 특성)

  • Lee, Jae-Won;Lee, Ji-Su;Lee, Jong-Soo
    • The Korean Journal of Food And Nutrition
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    • v.21 no.2
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    • pp.143-147
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    • 2008
  • To develop a new anti-wrinkle agent from medicinal plants, this study investigated the optimal conditions for extracting elastase inhibitor from Rheum undulatum L. Maximal extraction occurred by using 70% methanol at $50^{\circ}C$ for 24 hr; the elastase inhibitory activity was 60.4%($IC_{50}:6.7{\times}10^3{\mu}g/m{\ell}$). Systematic solvent extraction, thin layer chromatography, silica gel column chromatography, Sephadex LH-20 column chromatography, and reverse-phase high performance liquid chromatography were used in the partial purification of the elastase inhibitor. The compound was soluble in dimethylsulfoxide, methanol, and ethanol, and had maximum absorption spectra at 231.5 nm and 275.5 nm.

Solid-Phase Extraction of Sulfamerazine from Shrimp Residue and Determination by Reversed Phase High Performance Liquid Chromatography

  • Jang, Won-Cheoul;Heo, Gang-Joon
    • Toxicological Research
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    • v.12 no.2
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    • pp.163-169
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    • 1996
  • The focus of this study was to investigate the suitable analytical methods for measurement of sulfamerazine and its metabolite in shrimp hepatopancreas and tail tissue, in addition to the methods for the optimization of solid-phase extraction cartridge conditions and the elucidation of sulfamerazine concentrations in aqueous buffer using HPLC with UV and EC detectors. Compared with UV detector the EC detector appears to be 10 times more sensitive than that of the UV detector. After the shrimp was exposed to 10 ppm sulfamerazine, the accumulation levels of sulfamerazine and its metabolite in tail tissue, which is edible portion, were considerably lower than 0.1 ppm. The data indicate that sulfamerazine continues to be a candidate for use at levels of sulfamerazine concentration used in aquaculture of shrimp.

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Development of Quantitative Extraction Method of Amygdalin without Enzymatic Hydrolysis from Tonin(Persicae Semen) by High Performance Liquid Chromatography

  • Lee, Sang-Soo;Hwang, Eun-Young;Koh, Jung-A;Kim, Dong-Min;Lee, Je-Hyun;Lee, Yong-Moon;Hong, Seon-Pyo
    • Proceedings of the PSK Conference
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    • 2002.10a
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    • pp.389.2-389.2
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    • 2002
  • Tonin(Persicae Semen)is the herb medicine that cntains amygdalin as a major ingredient. Amygdalin in water is decomposed into benzaldehyde. HCN. and glucoseby emulsin. a hydrolysis enzyme intonin. A useful and practical method for the optimum extraction condition of amygdalin without enzymatic hydrolysis is required. The extraction yield of amygdalin of natural formula tonin was 0.1 % from crude powers. 1.4% from small pieces. 3.5% from half pieces and 2.4% from whole pieces. (omitted)

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Natural Dye Extraction from Merbau (Intsia bijuga) Sawdust: Optimization of Solid-Solvent Ratio and Temperature

  • Aswati MINDARYANI;Ali SULTON;Felix Arie SETIAWAN;Edia RAHAYUNINGSIH
    • Journal of the Korean Wood Science and Technology
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    • v.51 no.6
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    • pp.481-492
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    • 2023
  • The ecofriendly lifestyle has attracted considerable support for sustainable development. Natural dyes, as sustainable products, have become a research focus and development area for many scientists. Ecofriendly processing also supports circular sustainable development. This study effectively obtained tannins as a natural dye from merbau (Intsia bijuga) sawdust using water as an ecofriendly solvent. Merbau sawdust is an underutilized industrial waste. Temperature and solid-solvent ratio variations were performed to extract tannins from merbau sawdust. Temperature and solid-solvent ratio positively affected solution yield and tannin concentration. The optimal condition was identified using response surface methodology and experimental observations. A yield of 0.2217 g tannins/g merbau was obtained under the conditions of 333.15 K and 0.125 solid-solvent ratio. Extraction was controlled by convective mass transfer at the interface of solid particles.

Simultaneous Determination of Ultra-Trace Pesticides and Synthetic Materials in Surface Water by LC-ESI-MS/MS (하천수에서 LC-ESI-MS/MS에 의한 극미량 농약류 및 합성원료의 동시분석법)

  • Hong, Seon-Haw;Lee, Jun-Bae;Lee, Soo-Hyung;Cho, Young-Hwan;Shin, Ho-Sang
    • Journal of the Korean Chemical Society
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    • v.59 no.3
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    • pp.225-232
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    • 2015
  • A liquid chromatography-electrospray ionization-tandem mass spectrometry method (LC-ESI-MS/MS) was used for determining seven pesticides (2,4-dichlorophenoxyacetic acid, methomyl, aldicarb, 2-methyl- 4-chlorophenoxy- acetic acid, molinate, carbaryl and carbofuran) and two synthetic materials (quinoline and bisphenol-A) in surface water. The analytes were extracted using solid-phase extraction (SPE). The eluate was concentrated by nitrogen gas. 100 microliters of 30% (v/v) methanol aqueous solution were used to dissolve the residue and an aliquot of the reconstituted solution was directly injected into LC-ESI-MS/MS after the filtration using 0.2 μm polytetrafluoroethylene (PTFE) syringe filter. Under the established condition, the calibration curves of the analytes were linear with correlation coefficients of above 0.997. The quantification limit was 0.002~0.011 μg/L and the relative standard deviations were less than 16.4%. In addition, accuracy was in the range of 84~107% and the recoveries were values between 56.2 and 98.6%. In this study, the developed method was applied to the analysis of real surface water samples.

Qualitative and quantitative analysis of the saponins in Panax notoginseng leaves using ultra-performance liquid chromatography coupled with time-of-flight tandem mass spectrometry and high performance liquid chromatography coupled with UV detector

  • Liu, Fang;Ma, Ni;He, Chengwei;Hu, Yuanjia;Li, Peng;Chen, Meiwan;Su, Huanxing;Wan, Jian-Bo
    • Journal of Ginseng Research
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    • v.42 no.2
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    • pp.149-157
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    • 2018
  • Background: Panax notoginseng leaves (PNL) exhibit extensive activities, but few analytical methods have been established to exclusively determine the dammarane triterpene saponins in PNL. Methods: Ultra-performance liquid chromatography coupled with time-of-flight mass spectrometry (UPLC/Q-TOF MS) and HPLC-UV methods were developed for the qualitative and quantitative analysis of ginsenosides in PNL, respectively. Results: Extraction conditions, including solvents and extraction methods, were optimized, which showed that ginsenosides Rc and Rb3, the main components of PNL, are transformed to notoginsenosides Fe and Fd, respectively, in the presence of water, by removing a glucose residue from position C-3 via possible enzymatic hydrolysis. A total of 57 saponins were identified in the methanolic extract of PNL by UPLC/Q-TOF MS. Among them, 19 components were unambiguously characterized by their reference substances. Additionally, seven saponins of PNL-ginsenosides Rb1, Rc, Rb2, and Rb3, and notoginsenosides Fc, Fe, and Fd-were quantified using the HPLC-UV method after extraction with methanol. The separation of analytes, particularly the separation of notoginsenoside Fc and ginsenoside Rc, was achieved on a Zorbax ODS C8 column at a temperature of $35^{\circ}C$. This developed HPLC-UV method provides an adequate linearity ($r^2$ > 0.999), repeatability (relative standard deviation, RSD < 2.98%), and inter- and intraday variations (RSD < 4.40%) with recovery (98.7-106.1%) of seven saponins concerned. This validated method was also conducted to determine seven components in 10 batches of PNL. Conclusion: These findings are beneficial to the quality control of PNL and its relevant products.

Studies on the Analysis of Benzo(a)pyrene and Its Metabolites on Biological Samples by Using High Performance Liquid Chromatography/Fluorescence Detection and Gas Chromatography/Mass Spectrometry

  • Lee, Won;Shin, Hye-Seung;Hong, Jee-Eun;Pyo, Hee-Soo;Kim, Yun-Je
    • Bulletin of the Korean Chemical Society
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    • v.24 no.5
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    • pp.559-565
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    • 2003
  • An analytical method the determination of benzo(a)pyrene (BaP) and its hydroxylated metabolites, 1-hydroxybenzo(a)pyrene (1-OHBaP), 3-hydroxybenzo(a)pyrene (3-OHBaP), benzo(a)pyrene-4,5-dihydrodiol (4,5-diolBaP) and benzo(a)pyrene-7,8-dihydrodiol (7,8-diolBaP), in rat urine and plasma has been developed by HPLC/FLD and GC/MS. The derivatization with alkyl iodide was employed to improve the resolution and the detection of two mono hydroxylated metabolites, 1-OHBaP and 3-OHBaP, in LC and GC. BaP and its four metabolites in spiked urine were successfully separated by gradient elution on reverse phase ODS $C_{18}$ column (4.6 mm I.D., 100 mm length, particle size 5 ㎛) using a binary mixture of MeOH/H₂O (85/15, v/v) as mobile phase after ethylation at 90 ℃ for 10 min. The extraction recoveries of BaP and its metabolites in spiked samples with liquid-liquid extraction, which was better than solid phase extraction, were in the range of 90.3- 101.6% in n-hexane for urine and 95.7-106.3% in acetone for plasma, respectively. The calibration curves has shown good linearity with the correlation coefficients (R²) varying from 0.992 to 1.000 for urine and from 0.996 to 1.000 for plasma, respectively. The detection limits of all analytes were obtained in the range of 0.01-0.1 ng/mL for urine and 0.1-0.4 ng/mL for plasma, respectively. The metabolites of BaP were excreted as mono hydroxy and dihydrodiol forms after intraperitoneal injection of 20 mg/kg of BaP to rats. The total amounts of BaP and four metabolites excreted in dosed rat urine were 3.79 ng over the 0-96 hr period from adminstration and the excretional recovery was less than 0.065% of the injection amounts of BaP. The proposed method was successfully applied to the determination of BaP and its hydroxylated metabolites in rat urine and plasma for the pharmacokinetic studies.