Quantitative determination of paclitaxel in human plasma using semi-automated liquid-liquid extraction in conjunction with liquid chromatography/tandem mass spectrometry

被引:42
|
作者
Basileo, G [1 ]
Breda, M [1 ]
Fonte, G [1 ]
Pisano, R [1 ]
James, CA [1 ]
机构
[1] Pharmacia SPA, Global Drug Metab, I-20014 Milan, Italy
关键词
paclitaxel; semi-automated liquid-liquid extraction; LC-MS; human plasma;
D O I
10.1016/S0731-7085(03)00166-3
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
This paper describes a high-throughput sample preparation procedure combined with LC-MS/MS analysis to measure paclitaxel in human plasma. Paclitaxel and an internal standard were extracted from plasma by a semi-automated robotic method using liquid-liquid extraction. Thereafter compounds were separated on a RP C18 column. Detection was by a PE Sciex API 3000 mass spectrometer equipped with a TurbolonSpray(TM) interface. The compounds were detected in positive ion mode using the mass transition m/z 854.6-->286.2 and m/z 831.6-->263.2 for paclitaxel and the internal standard, respectively. The limit of quantitation for paclitaxel was 1 ng/ml with an imprecision of 5.2% following extraction of 0.1 ml of plasma. Linearity was confirmed over the whole calibration range (1-1000 ng/ml) with correlation coefficients higher than 0.99 indicating good fits of the regression models. The inter and intra-day precision was better than 9.5% and the accuracy ranged from 90.3 to 104.4%. The assay was simple, fast, specific and exhibited excellent ruggedness. (C) 2003 Elsevier Science B.V. All rights reserved.
引用
收藏
页码:591 / 600
页数:10
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