LC-MS/MS法测定人血浆中盐酸右美托咪定的浓度

目的:建立测定人血浆中盐酸右美托咪定浓度的方法。方法:血浆样品用乙酸乙酯-二氯甲烷(4∶1)萃取浓缩后进样。采用液-质联用(LC-MS/MS)法进样测定,以替米沙坦为内标,色谱柱为Agilent Eclipse Plus C18,流动相为甲醇-1%甲酸水(75∶25,V/V);采用电喷雾离子源(ESI),以多反应离子检测(MRM)方式进行检测。右美托咪定和内标检测离子对的m/z分别为201.1/95.1、512.2/276.1。结果:右美托咪定血药浓度在20⁶ 000 ng/L范围内线性关系良好(r=0.995 1),最低定量限为20 ng/L,提取回收率为82.20%6 000 ng/L范围内线性关系良好(r=0.995 1),最低定量限为20 ng/L,提取回收率为82.20%⁹6.37%,日内、日间RSD均在11%之内。结论:本方法具有快速、灵敏、重现性好等特点,可用于临床上盐酸右美托咪定血药浓度监测及药动学研究。

Determination of Dexmedetomidine Hydrochloride in Human Plasma by LC-MS/MS

OBJECTIVE： To establish a method for the determination of dexrnedetomidine hydrochloride in human plasma. METHODS： Dexmedetomidine was extracted with acetic ether-dichloromethane （4：1） and LC-MS/MS was adopted using telmisartan as internal standard. The separation was performed on Agilent Eclipse Plus C18 column with mobile phase consisted of methanol-1% formic acid （75：25, V/V）. ESI. source was applied. Dexmedetomidine and telmisartan （IS） were detected on multiple reaction monitoring （MRM） mode by the transitions from the precursor to the production （m/z 201.1/95.1,512.2/276.1）. RESULTS： The linear range of dexmedetomidine were 20-6 000 ng/L （r=0.995 1）, and the lowest quantification limit was 20 ng/L. The relative recoveries were 82.20%-96.37%, and the RSDs of intra-day and inter-day were less than 11%. CONCLUSIONS： The method is proved to be rapid, sensitive and reproducible for the determination of dexmedetomidine in human plasma and pharmacokinetic study.