Research Center for Drug Metabolism, College of Life Science, Jilin University, Changchun 130021, PR China.
J Pharm Biomed Anal. 2010 Nov 2;53(3):546-51. doi: 10.1016/j.jpba.2010.03.025. Epub 2010 Mar 30.
A rapid and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was established for the determination of sarpogrelate in human plasma. One-step protein precipitation with acetonitrile was used to extract the analytes from the plasma. Sarpogrelate and tramadol (internal standard, I.S.) were separated on a Venusil MP-C(18) column within 1.7 min, using acetonitrile:ammonium acetate (10 mM, pH 6.8) (55:45, v/v) as mobile phase at a flow rate of 1.2 mL/min with an approximately 1:1 split entering the mass spectrometer. Detection was performed on electrospray positive ionization mass spectrometry by multiple reaction monitoring of the transitions of sarpogrelate at m/z 430.3-->135.3 and of I.S. at m/z 264.1-->58.0. The assay was validated over the concentration range of 1-1000 ng/mL with a lower limit of quantitation (LLOQ) of 1 ng/mL using 50 microL of plasma. The intra- and inter-day precision (relative standard deviation, R.S.D.) were <or=6.4% and <or=5.4%, respectively, with accuracy (relative error, R.E.) in the range 0.5-3.6%. The method was successfully applied to a pharmacokinetic and bioequivalence study enrolling 22 Chinese volunteers administered sarpogrelate tablets.
建立了一种灵敏、快速的液相色谱-串联质谱（LC-MS/MS）法，用于测定人血浆中的沙格雷酯。采用乙腈一步蛋白沉淀法从血浆中提取分析物。沙格雷酯和曲马多（内标，IS）在 Venusil MP-C（18）柱上分离，流动相为乙腈：乙酸铵（10 mM，pH 6.8）（55：45，v/v），流速为 1.2 mL/min，大约 1：1 分流进入质谱仪。检测采用电喷雾正离子化质谱法，通过沙格雷酯的 m/z 430.3-->135.3 和 IS 的 m/z 264.1-->58.0 的过渡进行多重反应监测。该测定法在 1-1000 ng/mL 浓度范围内进行验证，LLOQ 为 1 ng/mL，使用 50 μL 血浆。日内和日间精密度（相对标准偏差，RSD）分别<或=6.4%和<或=5.4%，准确度（相对误差，RE）在 0.5-3.6%范围内。该方法成功应用于一项纳入 22 名中国志愿者的沙格雷酯片药代动力学和生物等效性研究。
