• 제목/요약/키워드: Drug determination

검색결과 578건 처리시간 0.029초

Simultaneous determination of sildenafil and its active metabolite in human plasma using LC/MS/MS

  • Ji, Hye-Young;Kim, Sook-Jin;Lee, Hong-Il;Lee, Seung-Seok;Lee, Hye-Sook
    • 대한약학회:학술대회논문집
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    • 대한약학회 2002년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.2
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    • pp.402.1-402.1
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    • 2002
  • The LC/MS/MS method for the simultaneous determination of sildenafil and its active metabolite N-demethylsildenafil in human plama was developed. Sildenafil. its active metabolite and the internal standard. DA-8159 were extracted form human plasma by liquid-liquid partitioning. A reverse-phase HPLC separation was performed on Luna phenylhexyl column with the mixture of acetonitrile-5 mM ammonium formate (55:45. v/v) as mobile phase. (omitted)

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농산물 중 메펜트리플루코나졸 및 트리티코나졸 살균제의 동시 분석법 개발 및 검증 (Development and Validation of a Simultaneous Analytical Method for the Detection of Mefentrifluconazole and Triticonazole Fungicide in Agricultural Crops)

  • 박지수;이한솔;이수정;신혜선;심재한;윤상순;정용현;오재호
    • 한국환경농학회지
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    • 제39권2호
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    • pp.130-137
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    • 2020
  • BACKGROUND: Mefentrifluconazole and triticonazole are the triazole fungicides. The maximum residue levels for agricultural products need to be set up. Therefore, development of the official analytical method for determination of mefentrifluconazole and triticonazole residues from agricultural crops was necessary due to safety management, and then a simultaneous analytical method was developed for the determination of mefentrifluconazole and triticonazole in agricultural crops. METHODS AND RESULTS: Samples were extracted using acetonitrile and purified using dispersive solid phase extraction, and then detected with liquid chromatograph-tandem mass spectrometry (LC-MS/MS). Matrix-matched calibration curves (0.0025-0.25 ㎍/mL) were linear into a sample extract with r2>0.99. For validation, the recovery test was carried out at three fortification levels (LOQ, 10 LOQ and 50 LOQ) from agricultural samples. The results for mefentrifluconazole and triticonazole ranged between 92.3 to 115.3% and 91.4 to 108.5%, respectively and RSD (relative standard deviation) values were also below 6.0%. Furthermore, inter-laboratory was conducted to validate the method. CONCLUSION: All values were corresponded with the criteria ranges requested by both the CODEX (CAC/GL 40-1993, 2003) and MFDS guidelines (2016). Therefore, the proposed method can be used as an official analytical method for determination of mefentrifluconazole and triticonazole (triazole fungicides) in the Republic of Korea.

Potentiometric Sensor for the Determination of Dibucaine in Pharmaceutical Preparations and Electrochemical Study of the Drug with BSA

  • Ensafi, Ali A.;Allafchian, A.R.
    • Bulletin of the Korean Chemical Society
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    • 제32권8호
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    • pp.2722-2726
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    • 2011
  • Plasticized poly(vinyl chloride), PVCs, with different membrane compositions tested for use in the construction of an ion-selective sensor for the determination dibucaine. A prepared membrane with dioctyl phthalate-PVC and ion-pair of N-(1-naphthyl)ethylenediamine dihydrochloride-tetraphenyl borate had a good potential to acts as a potentiometric sensor for the analysis of dibucaine. A linear relationship was obtained between potential and logC varying between $1.0{\times}10^{-6}$ and $1.0{\times}10^{-2}$ M dibucaine with a good repeatability and reproducibility. The sensor was applied for the determination of the drug in pharmaceuticals and biological fluids such as plasma and urine samples with satisfactory results. The drug electrode has also been used to study the interaction of bovine serum albumin (BSA) with dibucaine. The saturated quantities of dibucaine binding were 13.04, 5.30 and 9.70 mol/mol in 0.01, 0.02 and 0.1% of protein, respectively.

Multi-class, Multi-residue Analysis of 59 Veterinary Drugs in Livestock Products for Screening and Quantification Using Liquid Chromatography-tandem Mass Spectrometry

  • Yu Ra Kim;Sun Young Park;Tae Ho Lee;Ji Young Kim;Jang-Duck Choi;Guiim Moon
    • 한국환경농학회지
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    • 제41권4호
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    • pp.288-309
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    • 2022
  • BACKGROUND: The objective of this study was to develop a comprehensive and simple method for the simultaneous determination of 59 veterinary drug residues in livestock products for safety management. METHODS AND RESULTS: For sample preparation, we used a modified liquid extraction method, according to which the sample was extracted with 80% acetonitrile followed by incubation at -20℃ for 30 min. After centrifugation, an aliquot of the extract was evaporated to dryness at 40℃ and analyzed using liquid chromatography combined with tandem mass spectrometry. The method was validated at three concentration levels for beef, pork, chicken, egg, and milk in accordance with the Codex Alimentarius Commission/Guidelines 71-2009. Quantitative analysis was performed using a matrix-matched calibration. As a results, at least 52 (77.6%) out of 66 compounds showed the proper method validation results in terms of both recovery of the target compound and coefficient of variation required by Codex guidelines in livestock products. The limit of quantitation of the method ranged from 0.2 to 1119.6 ng g-1 for all matrices. CONCLUSION(S): This method was accurate, effective, and comprehensive for 59 veterinary drugs determination in livestock products, and can be used to investigate veterinary drugs from different chemical families for safety management in livestock products.

LC-MS/MS를 이용한 농산물 중 제초제 Sulfonylurea계 36종 동시 시험법 개발 (Development of the Simultaneous Analysis of 36 Sulfonylurea Herbicide Residues in Agricultural Products Using LC-MS/MS)

  • 이수정;이정미;장귀현;김현경;김지영
    • 한국환경농학회지
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    • 제42권2호
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    • pp.139-151
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    • 2023
  • Sulfonylurea herbicides are widely used in agriculture because they have a long residual period and high selectivity. An analytical method was developed using QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) technique for simultaneous determination of sulfonylurea herbicide residues in agricultural products by liquid chromatography tandem mass spectrometry and for establishment MRL (Maximum Residue Limit) of those herbicides in Korea. Extraction was performed using acetonitrile containing 0.1% formic acid with MgSO4 (anhydrous magnesium sulfate) and NaCl (sodium chloride) and the extract was cleaned up using MgSO4 and C18 (octadecyl). The matrix-matched calibration curves were composed of 7 concentration levels from 0.001 to 0.25 mg/kg and their coefficients of determination (R2) exceeded 0.99. The recoveries of three spiking levels (LOQ, 10LOQ, 50LOQ, n=5) were in the range of 71.7-114.9% with relative standard deviations of less than 20.0% for all the five agriculture products. All validation values met criteria of the European Union SANTE/11312/2021 guidelines and Food and Drug Safety Evaluation guidelines. Therefore, the proposed analytical method was accurate, effective, and sensitive for sulfonylurea herbicide residues determination in agricultural commodities.

생약복방 드링크제 중 계피성분의 확인 및 계피산의 분리정량 (Identification of Cinnamon Components and Quantitative Determination of Cinnamlc Acid from Crude Drug Drink Preparations)

  • 고성룡;김나미
    • Journal of Ginseng Research
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    • 제15권1호
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    • pp.1-5
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    • 1991
  • For the quality control of crude drug drink preparations, methods for identification of cinnamon components and quantitative determination of cinnamic acid were established. Cinnamon components were identified by TLC with benzene/ethyl acetate (1:1, v/v) on silica gel plate by spraying p-anisaldehyde-sulfuric acid. Cinnamic acid contents were determined at UV 280 nm by HPLC on $\mu$-Bondapak Cls column with acetonitrile/water/acetic acid (40:60:2, v/v). Recoveries of cinnamic acid in three crude drug drink preparations were between 84.1-90.2% compared to the content of the cinnamon extract.

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광곽향(Pogostemon cablin Benth.)으로부터 Patchouli alchol의 분리 및 함량분석 (Isolation and Quantitative Determination of Patchouli alcohol from Pogostemon cablin Benth.)

  • 김주선;지형준;원도희;강삼식
    • 생약학회지
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    • 제29권1호
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    • pp.18-21
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    • 1998
  • A method for isolation and quantitative determination of patchouli alcohol from Pogostemonis Herba (Pogostemon cablin) has been developed. Isolation of patchouli alcohol was achieved by column chromatography employing the normal-phase gradient separation system n-hexane-ether on silica gel column. The GC method for quantitative determination of patchouli alcohol provided a method for standardization of the raw drug. It suggested that the average content of patchouli alcohol in Pogostemonis Herba is about 0.26%.

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