کد مقاله | کد نشریه | سال انتشار | مقاله انگلیسی | نسخه تمام متن |
---|---|---|---|---|
1217645 | 1494175 | 2008 | 7 صفحه PDF | دانلود رایگان |
![عکس صفحه اول مقاله: Preparative chromatographic purification of diastereomers of silybin and their quantification in human plasma by liquid chromatography–tandem mass spectrometry Preparative chromatographic purification of diastereomers of silybin and their quantification in human plasma by liquid chromatography–tandem mass spectrometry](/preview/png/1217645.png)
A novel preparative HPLC method separating silybin has been developed to meet the need for both silybin A and silybin B standard. After the preparation of silybin A and silybin B standard, a simple, sensitive, selective and reproducible liquid chromatography–tandem mass spectrometry (LC–MS–MS) method with negative electrospray ionization (ESI) was developed for the quantification of silybin A and silybin B in human plasma. Following rapid sample preparation, silybin A, silybin B and naringin (internal standard, ISTD) were separated on a Zorbax Eclipse XDB-C18 column, using methanol–water containing 0.1% formic acid (48:52, v/v) as the mobile phase. The mass spectrometer was operated in selected reaction monitoring (SRM) mode using the transition m/z 481.1 → 300.9 for both silybin A and silybin B and m/z 579.2 → 271.1 for naringin, respectively. Linear calibration curves were obtained in the concentration range of 2–5000 ng/ml with a lower limit of quantitation (LLOQ) of 2 ng/ml for both silybin A and silybin B, respectively. The intra- and inter-day precision values were below 7.5% and accuracy was within ±4.9% at all three quality control (QC) levels, for both silybin A and silybin B, respectively. This method was successfully applied to the stereospecific analysis of silybin in plasma samples from a pharmacokinetic study of silybin A and silybin B in 22 healthy male Chinese volunteers after a single oral dose of silybin–phosphatidylcholine complex (equivalent to 280 mg silybin, including 133 mg silybin A and 147 mg silybin B).
Journal: Journal of Chromatography B - Volume 862, Issues 1–2, 1 February 2008, Pages 51–57