Panchal Jayesh G, Patel Ravindra V, Menon Shobhana K
Department of Chemistry, School of Science, Gujarat University, Navrangpura, Ahmedabad, Gujarat, India.
Biomed Chromatogr. 2011 Apr;25(4):524-30. doi: 10.1002/bmc.1478.
A simple, rapid and sensitive method has been developed and validated for the determination of pramipexole in rat plasma by using gas chromatography mass spectrometry. The lower limit of quantification (LLOQ) is superior to the other reported LC-MS/MS methods. After being made alkaline with NaOH, plasma samples (0.1 mL) were subjected to liquid-liquid extraction using methyl-t-butyl ether. Analytes were determined using electron impact ionization in a single quadrupole mass spectrometer. GC/MS was performed in the selected ion monitoring mode using target ions at m/z 211, 212 and 152 for pramipexole and m/z 194 and 165 for caffeine as internal standard. A linear calibration curve was plotted over the range of 20-1000 pg/mL for pramipexole (r(2) > 0.996). The LLOQ was 20.0 pg/mL, respectively, which offered high sensitivity and selectivity enough for bioanalytical investigation. Inter- and intraday precisions ranged from 0.3 to 8.8% and from 0.9 to 11.33%, respectively. The recovery of pramipexole from plasma ranged from 82.4 ± 7.1 to 87.8 ± 5.7%. The method fulfills all standards required for bioanalytical methods and can be successfully applied to a pharmacokinetic study of pramipexole in rats.
已开发并验证了一种简单、快速且灵敏的方法，用于通过气相色谱 - 质谱法测定大鼠血浆中的普拉克索。定量下限（LLOQ）优于其他已报道的液相色谱 - 串联质谱法。用氢氧化钠碱化后，取0.1 mL血浆样品，用甲基叔丁基醚进行液 - 液萃取。在单四极杆质谱仪中使用电子轰击电离测定分析物。气相色谱/质谱在选择离子监测模式下进行，使用普拉克索的m/z 211、212和152以及咖啡因（作为内标）的m/z 194和165作为目标离子。普拉克索在20 - 1000 pg/mL范围内绘制线性校准曲线（r(2) > 0.996）。LLOQ分别为20.0 pg/mL，为生物分析研究提供了足够高的灵敏度和选择性。日间和日内精密度分别为0.3%至8.8%和0.9%至11.33%。普拉克索从血浆中的回收率为82.4 ± 7.1%至87.8 ± 5.7%。该方法满足生物分析方法所需的所有标准，可成功应用于大鼠体内普拉克索的药代动力学研究。
