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摘要
A high throughput and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for the determination of clopidogrel in human plasma, using clopidogrel-d3 as internal standard. Detection was performed by positive ion electrospray tandem mass spectrometry on a HPLC Agilent 1200 Triple Ouad 6410 System. The mass transition of the ion-pair was followed for m/z 322.1 -> 212.1, for clopidogrel and m/z 327 -> 217, for clopidogrel-d3, in multiple reaction monitoring mode (MRM). The plasma samples were buffered (pH 2.0), extracted using a mixture hexan-ethyl acetate and then 104 of the sample extract was injected into the LC-MS/MS system. Clopidogrel and the internal standard were separated on a Zorbax SB-C8 column using a mobile phase consisting of 50:50 (v/v) mixture of acetonitrile and 0.1% formic acid aqueous solution, with a flow rate of 1 mL/min. The proposed method has been validated for a linear range of 10-10000 mg/mL and the value of the regression coefficient was >= 0.99. The precision (CV%) and accuracy (%) were lower than 6.1 % for infra- and inter-days assays. The overall recoveries for clopidogrel and clopidogrel-d3 were 81 and 84%, respectively. The overall time of the analysis was 7 min. The method is sensitive, specific and reproducible and can be used for the therapeutic drug monitoring of clopidogrel.
- 出版日期2014-7
