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目的:建立HPLC-ESI/MS分析方法测定人血浆中枸橼酸喷托维林的浓度。方法:采用Inertsil ODS-3C18(150mm×2.1mm,5μm)色谱柱,流动相为0.1mol.L-1醋酸铵溶液(甲酸调pH4.4)-甲醇(35:65),流速0.20mL.min-1,柱温为25℃;内标为盐酸洛拉曲克;质谱用电喷雾电离源正离子模式(ESI+),选择离子监测(SIR);样品用固相萃取法处理。结果:枸橼酸喷托维林的线性范围为0.78～300ng.mL-1,r=0.998,喷托维林提取回收率>70%,相对回收率在85%～115%范围内,日内、日间RSD均<15%。结论:该方法专属性强,灵敏度高,结果准确,可用于枸橼酸喷托维林血药浓度测定。
OBJECTIVE: To establish a HPLC-ESI / MS method for the determination of pentotaveline citrate in human plasma. Methods: Inertsil ODS-3C18 (150 mm × 2.1 mm, 5 μm) was used as the mobile phase. The mobile phase was 0.1 mol·L-1 ammonium acetate solution (pH = 4.4) -1 with a column temperature of 25 ° C; the internal standard was latrexate hydrochloride; the mass spectrometry was electrospray ionization source positive ion mode (ESI +), selective ion monitoring (SIR); and the sample was treated with solid-phase extraction. Results: The linear range of pentobarbitone citrate was 0.78 ~ 300 ng.mL-1, r = 0.998, the recovery of pentotoxin was> 70% and the relative recovery was within the range of 85% ~ 115% Daytime RSDs were <15%. Conclusion: This method is specific, sensitive and accurate. It can be used to determine the concentration of pentobarbital citrate.