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毛细管气相色谱-质谱法测定血浆中舒洛芬及其[2H3]舒洛芬对映体

Determination of the enantiomers of suprofen and [2H3]suprofen in plasma by capillary gas chromatography-mass spectrometry.

作者信息

Shinohara Y, Kirii N, Tamaoki H, Magara H, Baba S

机构信息

Tokyo College of Pharmacy, Japan.

出版信息

J Chromatogr. 1990 Jan 26;525(1):93-104. doi: 10.1016/s0378-4347(00)83382-4.

DOI:10.1016/s0378-4347(00)83382-4
PMID:2338451
Abstract

A method for the stereoselective assay of the (+)- and (-)-enantiomers of suprofen and [2H3]suprofen in human plasma was developed using gas chromatography-mass spectrometry-selected-ion monitoring. (+/-)-[2H7]Suprofen was used as an internal standard. The method involved diethyl ether extraction and chiral derivatization with S-(-)-1-(naphthyl)ethylamine to form diastereomeric amide. The diastereoisomers were separated on a capillary gas chromatograph-mass spectrometer. Quantitation was achieved by selected-ion monitoring of the quasi-molecular ions of the diastereoisomers. The sensitivity, specificity, accuracy and reproducibility of the method were demonstrated to be satisfactory for application to pharmacokinetic studies of suprofen enantiomers.

摘要

建立了一种采用气相色谱 - 质谱 - 选择离子监测法对人血浆中舒洛芬及其[2H3]舒洛芬的(+)-和(-)-对映体进行立体选择性测定的方法。(±)-[2H7]舒洛芬用作内标。该方法包括用乙醚萃取,并用S - (-)-1 - (萘基)乙胺进行手性衍生化以形成非对映体酰胺。非对映异构体在毛细管气相色谱 - 质谱仪上分离。通过对非对映异构体的准分子离子进行选择离子监测来实现定量。该方法的灵敏度、特异性、准确性和重现性经证明适用于舒洛芬对映体的药代动力学研究,令人满意。

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