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  • P-ISSN1225-0163
  • E-ISSN2288-8985
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  • P-ISSN 1225-0163
  • E-ISSN 2288-8985

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22권 5호
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Gas Chromatography/Mass Spectrometry를 이용한 Pravastatin 투여 쥐의 뇨 중 Cholesterol, Desmosterol, Lanosterol의 동시분석법

Simultaneous quantitative determination of urinary cholesterol, desmosterol and lanosterol in pravastatin treated rats by gas chromatography/mass spectrometry

분석과학 / Analytical Science and Technology, (P)1225-0163; (E)2288-8985
2009, v.22 no.5, pp.407-414
정병화 (한국과학기술연구원 생체대사연구센터)
Bhowmik Salil Kumar (한국과학기술연구원 생체대사연구센터,과학기술연합대 생물분석과학전공)
정봉철 (한국과학기술연구원)
이영주 (경희대학교 약학대학)
이홍재 (경희대학교 약학대학)
정병화, Bhowmik, S. K. , 정봉철, 이영주, & 이홍재. (2009). Gas Chromatography/Mass Spectrometry를 이용한 Pravastatin 투여 쥐의 뇨 중 Cholesterol, Desmosterol, Lanosterol의 동시분석법. , 22(5), 407-414.

초록

가스크로마토그래피-질량분석기 (GC/MS)를 이용하여 뇨 중의 cholesterol, lanosterol, desmosterol 의 동시분석법을 개발하였다. 뇨 시료는 ${\beta}$-glucuronidase/arylsulfatase를 첨가하여 효소가수분해한 후 에틸아세테이트-헥산 (2:3, v/v)으로 추출하였으며 추출한 잔사를 MSTFA/TMSI/TMCS (100:2:5 v/v/v)로 유도체화한 후 GC/MS의 selective ion monitoring mode에서 분석하였다. 개발된 분석방법은 검량선에서 좋은 직선성 ($r^2

keywords
cholesterol, desmosterol, lanosterol, pravastatin, GC/MS

Abstract

A simultaneous determination method for cholesterol, lanosterol and desmosterol was developed using gas chromatography/mass spectrometry. Urine was enzymatically hydrolyzed with β-glucuronidase/arylsulfatase. Samples were prepared using extractions with a mixture of ethyl acetate-hexane (2:3, v/v), followed by derivatization with a mixture of MSTFA/TMSI/TMCS (100:2:5 v/v/v). All analyses were performed using GC/ MS in selective ion monitoring mode. Good linearities (r2=0.998~0.999) in calibration curve and a satisfactory recovery (80.0%~113%) were achieved. Accuracy and precision values within ±15% in the concentration range of 5 to 200 ng/mL were also observed for all compounds. The developed method was applied to pravastatintreated (70 and 250 mg/kg/day for 7 days, oral) hyperlipidemia rats. Those sterols were significantly lower in drug-treated rats compared to the controls, which justifies the drug efficacy. Therefore, these results indicate that the developed method was successfully applied to examine statin drug efficacy with urine sample.

keywords
cholesterol, desmosterol, lanosterol, pravastatin, GC/MS

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