• 제목/요약/키워드: gas-liquid chromatographic determination

검색결과 26건 처리시간 0.023초

First Derivative Spectrophotometric and Gas-Liquid Chromatographic Determination of Caffeine in Foods and Pharmaceuticals III. Simultaneous assay of caffeine and some antihistaminics

  • Abdel-Moety, Ezzat M.;El-Tarras, Mohamed F.;El-Zeany, Badr-Eldin A.;Kelani, Khadiga O.
    • Archives of Pharmacal Research
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    • 제13권3호
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    • pp.215-220
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    • 1990
  • Two different, derivative spectrophotometric and gas-liquid chromatographic, procedures for direct quantitation of caffeine and some commonly dispensed antihistaminics in bulk forms, in their laboratory prepared mmixtures and in dosage formulations, have been investigated. The limit, sensitivity reproducibility and accuracy of each method were studied for each individual drug substance and in some usual pharmaceutical formulations.

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Gas Liquid Chromatography에 의한 Dienestrol Cream 중의 Dienestrol 정량 (Determination of Dienestrol in Dienestrol Cream by Gas Liquid Chromatography)

  • 백남호;박만기;염정록
    • 약학회지
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    • 제23권1호
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    • pp.7-10
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    • 1979
  • A gas chromatographic determination of dienestrol in dienestrol cream has been studied. Dienestrol cream was dissolved in pyridine and silylation was done by using N, O-bis (trimethylsilyl) trifluoroacetamide. The derivative was injected into 3% silicone OV-17 column for chromatographic estimation. The dienestrol peak was found to be well separated from the other components of the cream. The detection limit was obtained to be $5.6{\times}10^{11}$ mol of dienestrol for this method. As there is no need for prior separation procedure, this experiment is extremely simple and less time consuming as compared to the conventional methods for estimation of dienestrol in cream.

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Quantitative Determination of Styrene in Blood and Mandelic Acid in Urine of the Occupationally Styrene-exposed Workers

  • Yang, Jeong-Sun
    • Archives of Pharmacal Research
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    • 제17권2호
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    • pp.76-79
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    • 1994
  • The concentration of styrne in blood of the occupationally syrene-exposed workers was checked by gas chromatographic headspace analysis. Mandelic acd in urine, that is a major metabolite of styrene, and hippuric acid wre also analyzed by high performance liquid chromatography. For the biological monitoring of styrene-exposed workers, the routine method of the quantitative determination of styrene nad its metabolites in the biolgical samples were studied.

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Determination of Monocrotophos Residues by HPLC

  • Lee, Young-Deuk;Kwon, Chan-Hyeok
    • 한국환경농학회지
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    • 제23권4호
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    • pp.245-250
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    • 2004
  • An analytical method was developed to determine monocrotophos residues in apple, citrus, and soil using high-performance liquid chromatography (HPLC) with ultraviolet absorption detection. Monocrotophos was extracted with acetone from apple, citrus and moist soil samples. The extract was concentrated, added with saline water, and subjected to n-hexane washing to remove nonpolar co-extractives. Dichloromethane partition was then followed to recover monocrotophos from the aqueous phase. Silica gel column chromatography was employed to further purify the extract prior to HPLC determination. Reverse-phase HPLC using an oct-adecylsilyl column was successfully applied to separate and quantitate the monocrotophos residue in sample extracts at the wavelength of 230 nm. Overall recoveries of monocrotophos from fortified samples averaged $95.3{\pm}2.1%$ (n=6), $970{\pm}0.7%$ (n=6), and $92.8{\pm}4.3%$ (n=12) for apple, citrus, and soil, respectively. The proposed method was quite reproducible and sensitive enough to replace the troublesome gas-liquid chromatographic analysis for monocrotophos residues.

기체크로마토그래피를 이용한 잔류농약 동시다성분 분석법 (Determination of Simultaneous Analytical Method of Residual Pesticides by Gas Chromatography)

  • 최원조;최계선;이희정;원영준;박흥재;김우성
    • 한국환경과학회지
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    • 제18권12호
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    • pp.1369-1381
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    • 2009
  • The simultaneous determination of residual pesticides was developed using a gas chromatography. In this study, a simple and reliable methodology was improved to detect 175 kinds of residual pesticides by a liquid-liquid extraction procedure, followed by chromatographic analysis by gas chromatography. The 175 kinds of residual pesticides was classified into 4 groups according to the chemical structure, column type, resolution and sensitivity. The soybean sample selected for recovery experiment was not detected any pesticides. The recovery rates were ranged from 70.6% to 119.7% in most pesticides. The relative standard deviation (RSD 0.3~5.6%) was lower than 5.6% in all cases. The limits of detection (LOD) was lower than the maximum residue levels established by Korean legislations. The method has been successfully applied to the analysis of approximately 130 real samples.

MSPD 전처리법과 HPLC를 이용한 Furazolidone의 계란내 잔류분석 (Matrix Solid-Phase Dispersion (MSPD) Isolation and Liquid Chromatographic Determination of Residual Furazolidone in Eggs)

  • 서계원;이재일;이채용;이정치
    • 한국식품위생안전성학회지
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    • 제18권2호
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    • pp.43-50
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    • 2003
  • A liquid chromatographic method, using matrix solid-phase dispersion (MSPD) is developed for the extraction of residual furazolidone in chicken eggs. Blank or fortified egg samples (0.5 g) were blended with Octadecylsilyl (Bulk $C_{18}$, 40${\mu}{\textrm}{m}$, 18%. load, endcapped. 2 g) derivatized silica. After homogenization, $C_{18}$/egg and Na$_2$S $O_4$matrix were transferred to a column made of 10 ml glass syringe and filter paper and compressed 4.0∼4.5 ml volume. The column was washed with 8 ml of hexane and dried under $N_2$ gas. Furazolidone was eluted with acetonitrile (8 ml) under gravity. The eluate containing furazolidone was free from interfering compounds when analyzed by HPLC with UV detection (365 nm, photodiode array). Calibration curves were linear (r = 0.99985) and inter- (1.47%) and intra-assay (5.29%) variabilities for the concentration range examined (7.8∼497 ng/g of eggs, 20 ${mu}ell$ injection volume) were indicative of an acceptable methodology for the analysis of furazolidone. Average recovery of furazolidone added to egg was 96.2%. The limit of detection for the proposed method was 1 ng/g for furazolidone. The method using MSPD is proposed as an alternative assay to the classical method which involves the use of large volumes of a harmful solvent and requires a long tedious separation and clean-up processes prior to its determination.

A Synthesis of Optically Active cis and trans 2-(5-Hydroxypoperidin-2-yl)acetates

  • P.N. Reddy;한상수;정교현
    • Bulletin of the Korean Chemical Society
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    • 제19권6호
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    • pp.617-618
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    • 1998
  • A simple and reproducible pretreatment method was developed for the determination of dioxins in milk sample. Liquid-liquid extraction (LLE) was used for the initial extraction of the analyte from milk. For the elimination of interferences coextracted from milk, acid treatment followed by multilayer silica gel, and then alumina column clean-up were performed. The clean extract could be obtained without carbon column or high performance liquid chromatographic (HPLC) clean-up procedure. Polychlorinated biphenyles (PCBs) and dioxins were separated on neutral alumina activated at 180 ℃ for 12 hours. The final extract was analyzed by HPLC and high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS). The recovery of dioxins spiked in milk at 75-300 ppt level was 83.3-98.9% and their relative standard deviation was 4.1-14%.

Analytical Method for Dioxin and Organo-Chlorinated Compounds : (I) Pretreatment of Milk Samples for Dioxin Analysis

  • 양정수;김진영;최용욱;이대운
    • Bulletin of the Korean Chemical Society
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    • 제19권6호
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    • pp.619-624
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    • 1998
  • A simple and reproducible pretreatment method was developed for the determination of dioxins in milk sample. Liquid-liquid extraction (LLE) was used for the initial extraction of the analyte from milk. For the elimination of interferences coextracted from milk, acid treatment followed by multilayer silica gel, and then alumina column clean-up were performed. The clean extract could be obtained without carbon column or high performance liquid chromatographic (HPLC) clean-up procedure. Polychlorinated biphenyles (PCBS) and dioxins were separated on neutral alumina activated at 180 ℃ for 12 hours. The final extract was analyzed by HPLC and high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS). The recovery of dioxins spiked in milk at 75-300 ppt level was 83.3-98.9% and their relative standard deviation was 4.1-14%.

Gas-liquid chromatography에 의한 한국(韓國) 주요식품(主要食品)의 아미노산(酸) 함량측정(含量測定) (Gas-Liquid Chromatographic Determination of Amino Acids in Some Korean Foods)

  • 박양자
    • Applied Biological Chemistry
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    • 제12권
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    • pp.43-51
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    • 1969
  • 우리나라 주요 식품들의 단백질 아미노산 함량을 최근에 와서 크게 실용화되고 있는 GLC 방법에 의해 분석함에 있어서 GLC의 기술적 재평가를 하고자 시험 하였든바 1. 우선 여러식품들의 단백질 질소함량을 조사하여 GLC 분석에 필요한 시료량을 정하였으며 2. GLC에 주입한 17종 아미노산들이 대하여 조사한 결과 Arginine, Cystine, Histidine, Tyrosine을 제외한 13종만이 주입한 량에 비례하여 detector response 를 얻었다. 3. 13종 아미노산에 대한 RMR 치(値)를 얻었다. 4. 아미노산에 대한 recovery 검정(檢定)을 하였든바 거의 100% 가까이 recover되었으며, 가수분해가 recovery에 미치는 영향을 조사하였든바 별 영향이 없었음을 알았다. 5. GLC와 ion-exchange chromatography 분석법을 비교시험하였든바 백어포 시료에 있어서는 Threonine과 Asparagine만이 두 방법에서 거의 같게 나왔고 다른 아미노산들은 GLC에서 보다 많은량이 나타났다. 6. 각식품들에 대한 단백질 아미노산함량을 측정하였든바 식품종류에 따라 그리고 보리 및 대두에 있어서는 품종에 따라서도 아미노산 함량이 다르게 나타났다.

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