论文部分内容阅读
目的建立快速、灵敏的液相色谱-串联质谱法测定人血浆中倍他米松(BOH)浓度的方法。方法采用Agilent Zorbax C_(18)(2.1mm×150mm,5μm)色谱柱,柱温25℃,流动相为甲醇-水(85:15,V/V),流速为0.2mL·min~(-1),电喷雾(ESI)离子源,多反应离子监测(MRM)的扫描方式。BOH采用负离子检测,二丙酸倍氯米松(内标,IS)采用正离子检测,BOH和IS的离子通道分别选择为m/z 361.0→m/z307.2和m/z 543.1→m/z 433.2。结果 BOH在0.1～30μg·L~(-1)浓度范围内有良好的线性关系(r~2=0.999 1),定量下限(LOQ)为0.1μg·L~(-1),日内、日间精密度(RSD)均小于15%,提取回收率均在65%左右,相对回收率均在85%～115%范围内。结论该方法简便、准确、灵敏,可用于人血浆中BOH的浓度检测、人体药动学和生物等效性研究。
Objective To establish a rapid and sensitive method for the determination of beta-hydroxybutyrate (BOH) in human plasma by liquid chromatography-tandem mass spectrometry. Methods The mobile phase consisted of methanol - water (85:15, V / V) and a mobile phase of 0.2 mL · min ~ (-1) at a column temperature of 25 ℃ on an Agilent Zorbax C 18 (2.1 mm × 150 mm, ), Electrospray (ESI) ion source, multi-reactive ion monitoring (MRM) scanning mode. BOH was detected by negative ions, and beclomethasone dipropionate (IS) was detected by positive ion. The ion channels of BOH and IS were selected as m / z 361.0 → m / z 307.2 and m / z 543.1 → m / z 433.2. Results BOH had a good linear relationship (r ~ 2 = 0.999 1) and a lower limit of quantitation (LOQ) of 0.1 μg · L -1 in the concentration range of 0.1 ~ 30μg · L -1. The precision (RSD) was less than 15%, the recovery rate was about 65%, and the relative recoveries were in the range of 85% ~ 115%. Conclusion The method is simple, accurate and sensitive and can be used for the determination of BOH in human plasma, human pharmacokinetics and bioequivalence studies.