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目的建立测定人血浆中丁螺环酮的LC-MS/MS方法,并用于缓释盐酸丁螺环酮胶囊的临床药动学试验。方法血浆样品经固相萃取后,以10mmol·L-1的甲酸铵溶液-含0.5‰甲酸的乙腈溶液为流动相,梯度洗脱,经SymmetryC18色谱柱(2.1mm×150mm,5μm)分离。通过电喷雾离子源,以多反应离子监测(MRM)方式进行检测。用于定量分析的离子反应分别为m/z386→121.7(丁螺环酮)和409→237.7(内标,氨氯地平)。结果LC-MS/MS测定人血浆中丁螺环酮的线性范围为0.025～12.8μg·L-1,r=0.9993。该方法的绝对回收率为74.97%～77.83%,相对回收率为93.67%～102.0%,日内、日间精密度(RSD)分别为0.9%～5.1%和1.9%～6.7%。在临床药动学研究中,应用此法测试了10名受试者口服盐酸丁螺环酮缓释胶囊后血浆中丁螺环酮的浓度。结论本法快速、准确,灵敏度高,重现性好,可以满足本试验低浓度药物测定及药动学研究要求。
Objective To establish a LC-MS / MS method for the determination of buspirone in human plasma and to study the pharmacokinetics of buspirone hydrochloride capsules. Methods The plasma samples were separated by a Symmetry C18 column (2.1 mm × 150 mm, 5 μm) using gradient elution with 10 mmol·L -1 ammonium formate solution containing 0.5 ‰ formic acid in acetonitrile as the mobile phase. Detection by multi-reactive ion monitoring (MRM) by electrospray ionization. The ion reactions used for the quantitative analysis were m / z 386 → 121.7 (buspirone) and 409 → 237.7 (internal standard, amlodipine), respectively. Results The linear range of LC-MS / MS for the determination of buspirone in human plasma ranged from 0.025 to 12.8 μg · L-1, r = 0.9993. The absolute recoveries of this method ranged from 74.97% to 77.83%, and the relative recoveries ranged from 93.67% to 102.0%. The intra-day and inter-day RSDs were 0.9% -5.1% and 1.9% -6.7%, respectively. In the clinical pharmacokinetic study, this method was used to test the concentration of buspirone in 10 subjects after oral administration of buspirone hydrochloride sustained-release capsules. Conclusion This method is rapid, accurate, sensitive and reproducible, which can meet the requirements of low concentration drug testing and pharmacokinetics research in this experiment.