• 제목/요약/키워드: liquid recovery

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Validation of the Analysis of Domoic Acid using High Performance Liquid Chromatography (HPLC에 의한 Domoic acid 분석법 검정)

  • Mok, Jong-Soo;Lee, Ka-Jeong;Song, Ki-Cheol;Kim, Ji-Hoe
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.43 no.4
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    • pp.293-297
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    • 2010
  • To prevent amnesic shellfish poisoning (ASP) resulting from the consumption of shellfish contaminated with domoic acid, the quantitative analysis of domoic acid is very important. We validated a high performance liquid chromatography (HPLC) method for accurate and precise quantification of domoic acid. A clear peak and the isolation of domoic acid resulted on injecting a 50% methanol extract of CRM-ASP-Mus-c mussel reference material using HPLC. The limit of detection of domoic acid under the established HPLC conditions was $0.10\;{\mu}g/g$, and the limit of quantification of the toxin under the same conditions was $0.25\;{\mu}g/g$. The intra-accuracy and precision for domoic acid in CRM-ASP-Mus-c were 90.7-95.7% and 0.28-22.25%, respectively. The inter-accuracy and precision for domoic acid were 89.1-97.1% and 1.7-4.1%, respectively. The mean recovery of domoic acid in methanol extracts from ten species of marine invertebrates was 88.6-1105.1%.

Simultaneous Determination of Glutamate, Glycine, and Alanine in Human Plasma Using Precolumn Derivatization with 6-Aminoquinolyl-N-hydroxysuccinimidyl Carbamate and High- Performance Liquid Chromatography

  • Li, Qing Zhong;Huang, Qing Xian;Li, Shu Cui;Yang, Mei Zi;Rao, Bin
    • The Korean Journal of Physiology and Pharmacology
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    • v.16 no.5
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    • pp.355-360
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    • 2012
  • A simple, sensitive and reproducible high-performance liquid chromatography (HPLC) method has been validated for determining concentrations of glutamate, glycine, and alanine in human plasma. Proteins in plasma were precipitated with perchloric acid, followed by derivatization with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC). Simultaneous analysis of glutamate, glycine, and alanine is achieved using reversed-phase HPLC conditions and ultraviolet detection. Excellent linearity was observed for these three amino acids over their concentration ranges with correlation coefficients (r)>0.999. The intra- and inter-day precision were below 10%. This method utilizes quality control samples and demonstrates excellent plasma recovery and accuracy. The developed method has been successfully applied to measure plasma glutamate, glycine, and alanine in twenty volunteers.

Chiral Purity Test of Bevantolol by Capillaryelectrophoresis and High Performance Liquid Chromatography

  • Long, Pham Hai;Trung, Tran Quoc;Oh, Joung-Won;Kim, Kyeong-Ho
    • Archives of Pharmacal Research
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    • v.29 no.9
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    • pp.808-813
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    • 2006
  • Two methods for the chiral purity determination of bevantolol were developed, namely capillary electrophoresis (CE) using carboxymethyl-${\beta}$-cyclodextrin (CM-${\beta}$-CD) as a chiral selector and high-perfomance liquid chromatography (HPLC) using a chiral stationary phase. In the HPLC method, the separation of bevantolol enantiomers was performed on a Chiralpak AD-H column by isocratic elution with n-hexane-ethanol-diethylamine (10:90:0.1, v/v/v) as mobile phase. In the CE method, bevantolol enantiomers were separated on an uncoated fused silica capillary with 50 mM amonium phosphate dibasic adjusted to a pH 6.5 with phosphoric acid containing 15 mM CM-${\beta}$-CD as running buffer. Validation data such as linearity, recovery, detection limit, and precision of the two methods are presented. The detection limits of S-(-)-bevantolol were 0.1% and 0.05% for CE and HPLC method, respectively and R-(+)-bevantolol were 0.15% and 0.05% for CE and HPLC method, respectively. There was generally good agreement between the HPLC and CE results.

Analysis of Heterocyclic Amines in Human Urine Using Multiple Solid-Phase Extraction by Liquid Chromatography/Mass Spectrometry

  • Cha, Hyun-Jeong;Kim, Nam-Hee;Jeong, Eun-Kyung;Na, Yun-Cheol
    • Bulletin of the Korean Chemical Society
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    • v.31 no.8
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    • pp.2322-2328
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    • 2010
  • A multiple solid-phase extraction (SPE) method was used with liquid chromatography, coupled with mass spectrometry (LC/MS), for the analysis of heterocyclic amines (HCAs) in human urine. Separation efficiencies based on the pH of the mobile phase and the types of columns were compared. An amide column showed better baseline separation and narrower HCA peak widths at pH 5.0 for the mobile phase than a $C_8$ column. Each SPE step, HLB, MCX, and HybridSPE, was optimized by controlling the pH conditions. The combined method with the three SPEs effectively removed interfering species that cause ion-suppression during HCA detection. Validation of the method, performed with SIM and SRM detection, showed correlation coefficients above 0.991 in the range 0.3 - 16.7 ng/mL. Recovery rates were 45.4 - 97.3% on the $C_8$ column and 71.8 - 101.4% on the amide column, and method detection limits were 0.11 - 0.65 ng/mL on the $C_8$ column and 0.12 - 0.48 ng/mL on the amide column. This method using multiple SPEs offers significant benefits for high-throughput determination of HCAs in urine.

A Study on the Recovery of Acetonitrile in the Process of Acrylonitrile (Acrylonitrile 제조공정에서 Acstonitrile의 회수에 관한 연구)

  • Lee, Jin-Woo;Park, Dong-Won
    • Applied Chemistry for Engineering
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    • v.5 no.6
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    • pp.1016-1023
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    • 1994
  • In process of manufacturing acrylonitrile azeotrope of acetonitrile-water was come into being as by-product. For the purpose of recovering acetonitrile through solvent extraction process benzene, toluene, o-xylene, ethylacetate and monochlorobenzene as solvents were selected in order to separate acetonitrile from azeotrope of acetonitrile-water. In this study liquid-liquid equilibrium data were determined and consistency of the experimental data was investigated. The tie line and plait point for solvent(1)-water(2)-acetonitrile(3) system were determined at $25^{\circ}C$. The parameters in the NRTL, UNIQUAC and modified UNIQUAC model were predicted, distribution coefficient and selectivity of each solvent were determined respectively.

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The Assessment of Carbendazim, Cyazofamid, Diethofencarb and Pyrimethanil Residue Levels in P. ginseng (C. A. Meyer) by HPLC

  • Choi, Jeong-Heui;El-Aty, A.M.Abd;Park, Young-Seok;Cho, Soon-Kil;Shim, Jae-Han
    • Bulletin of the Korean Chemical Society
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    • v.28 no.3
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    • pp.369-372
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    • 2007
  • A fast and simple high-performance liquid chromatography (HPLC) method for the simultaneous determination of four pesticides having fungicide properties has been proposed for Panax ginseng, C. A. Meyer grown for 4, 5, or 6 years. Analytical separation was performed on C18 columns using ultraviolet detector under gradient conditions. Spiked blank samples were used as standards to counteract the matrix effect observed in the chromatographic determination. The HPLC response for all pesticides was linear, with determination coefficients > 0.9986. The average rate of recovery for pesticides spiked with 2 fortification levels was > 72% with relative standard deviations < 9%. The limits of quantification (LOQ) ranged from 0.03 to 0.16 ppm. These LOQs were lower than the respective maximum residue limits (MRL) established by the Korean Food and Drug Administration (KFDA), except for cyazofamid. The proposed method was used to determine pesticide residue levels in samples of ginseng obtained from Jeonnam Province (Republic of Korea). None of the pesticides were found in ginseng samples grown for 4, 5, or 6 years.

Monitoring of Biotin Content in Frequently Consumed Foods in Korea (국내 다소비 식품의 biotin 함량 모니터링)

  • Kwon, Jihyun;Cheon, Wonyoung;Lee, Sang-Hoon;Choi, Youngmin;Kim, Younghwa
    • Journal of the Korean Society of Food Culture
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    • v.35 no.3
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    • pp.278-284
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    • 2020
  • In this study, biotin (vitamin B7) contents of frequently consumed foods in Korea were determined by using immunoaffinity column in conjunction with high-performance liquid chromatography (HPLC). The biotin contents of 24 foods of plant origin and 27 foods of animal origin were selected. The highest biotin contents in frequently consumed foods of plant origin were found in red beans (Huinguseul; 11.475 ㎍/100 g). On the other hand, biotin was not detected in any varieties of sorghum. For frequently consumed foods of animal origin, salted pollack roe (7.486 ㎍/100 g) showed the highest biotin content. However, beef and fish contained less biotin. All biotin analyses were conducted under analytical quality control. The limits of detection and limits of quantification of biotin were 0.007 and 0.023 ㎍/100 g, respectively, and the accuracy/recovery percentage was 95.35-105.02%. The precision values were 4.041% (repeatability) and 3.835% (reproducibility). Taken together, our data provide reliable data on the biotin contents of frequently consumed foods in Korea.

Chemical Equilbrium Analysis of the $30\;ton_f$ - class KARI LRE Nozzle Flow (KARI 30톤급 액체 로켓 엔진 노즐 유동 화학 평형 해석)

  • Lee, Dae-Sung;Kang, Ki-Ha;Cho, D.R.;Choi, Jeong-Yeol;Choi, H.S.
    • Journal of the Korean Society of Propulsion Engineers
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    • v.12 no.3
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    • pp.9-15
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    • 2008
  • Nozzle flow analyses of $30\;ton_f$-class KARI liquid rocket engine for high altitude propulsion are carried out using a chemically frozen and equilibrium flow analysis code developed previously. It is considered that the combined frozen- and shifting- equilibrium analysis is cost-effective regarding the convergence characteristics and modeling uncertainties, though the non-equilibrium analysis is most reliable approach. A dependable performance prediction could be attainable through the present analyses that account for the recombination process and thermal and kinetic energy recovery during the expansion process with viscous effects.

Wet Air Oxidation Pretreatment of Mixed Lignocellulosic Biomass to Enhance Enzymatic Convertibility

  • Sharma, A.;Ghosh, A.;Pandey, R.A.;Mudliar, S.N.
    • Korean Chemical Engineering Research
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    • v.53 no.2
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    • pp.216-223
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    • 2015
  • The present work explores the potential of wet air oxidation (WAO) for pretreatment of mixed lignocellulosic biomass to enhance enzymatic convertibility. Rice husk and wheat straw mixture (1:1 mass ratio) was used as a model mixed lignocellulosic biomass. Post-WAO treatment, cellulose recovery in the solid fraction was in the range of 86% to 99%, accompanied by a significant increase in enzymatic hydrolysis of cellulose present in the solid fraction. The highest enzymatic conversion efficiency, 63% (by weight), was achieved for the mixed biomass pretreated at $195^{\circ}C$, 5 bar, 10 minutes compared to only 19% in the untreated biomass. The pretreatment under the aforesaid condition also facilitated 52% lignin removal and 67% hemicellulose solubilization. A statistical design of experiments on WAO process conditions was conducted to understand the effect of process parameters on pretreatment, and the predicted responses were found to be in close agreement with the experimental data. Enzymatic hydrolysis experiments with WAO liquid fraction as diluent showed favorable results with sugar enhancement up to $10.4gL^{-1}$.

Liquid Chromatography-Tandem Mass Spectrometry for the Determination of Lithospermic Acid B in Rat Serum

  • Kim, Hui-Hyun;Ji, Hye-Young;Lee, Hye-Won;Kim, Youn-Chul;Sohn, Dong-Hwan;Lee , Hye-Suk
    • Archives of Pharmacal Research
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    • v.27 no.12
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    • pp.1202-1206
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    • 2004
  • A rapid, sensitive and selective liquid chromatography-tandem mass spectrometric (LC-MS/ MS) method for the determination of lithospermic acid B (LSB) in rat serum was developed. LSB and internal standard, 7-hydroxy-3-phenyl-chromen-4-one (HPC) were extracted from rat serum with methyl-tert-butyl ether at acidic pH and analyzed on a Luna $C_8$ column with the mobile phase of acetonitrile-ammonium formate (10 mM, pH 6.5) (50:50, v/v). The analytes were detected using a negative electrospray ionization tandem mass spectrometry in the multiple- reaction-monitoring mode. The standard curve was linear $(r^2 = 0.997)$ over the concentration range of 10.0-500 ng/mL. The coefficient of variation and relative error for intra- and interassay at three QC levels were 1.1~6.2% and -10.3~-2.7%, respectively. The recovery of LSB from serum sample ranged from 73.2 to 79.5%, with that of HPC (internal standard) being 75.1 %. The lower limit of quantification for LSB was 10 ng/mL using 50 ${\mu}L$ of serum sample.