HPLC-MS/MS法同时测定人血浆中依那普利和依那普利拉的浓度  

Simultaneous determination of enalapril and enalaprilat in human plasma by high-performance liquid chromatography tandem mass spectrometry

作　　者：张勇[1] 施振国[1] 

机构地区：[1]解放军总医院医务部药材处,北京100853

出　　处：《实用药物与临床》2015年第12期1469-1472,共4页Practical Pharmacy and Clinical Remedies

摘　　要：目的建立人血浆中依那普利和依那普利拉含量测定的高效液相色谱-串联质谱（HPLC-MS/M S）方法。方法血浆样品加入内标（贝那普利拉）,以含0.1%甲酸的甲醇沉淀蛋白后,进行HPLC-M S/M S分析。色谱柱为Hedera ODS-2 C18（150 mm×2.1 mm,5μm）,流动相为甲醇-0.5%甲酸水溶液梯度洗脱,流速为0.4 m L/min,柱温为30℃,采用多反应监测（M RM）方式进行定量分析,用于监测的离子质荷比分别为m/z377.2→m/z 234.3（依那普利）、m/z 349.3→m/z 206.2（依那普利拉）和m/z 397.4→m/z 351.4（内标,贝那普利拉）。结果人血浆中依那普利和依那普利拉的线性范围分别为0.2~200 ng/m L（r=0.999 9）、0.5~120 ng/m L（r=0.999 3）;批内、批间精密度均〈11.3%。结论该方法快速、灵敏、专属性强,可用于人血浆中依那普利和依那普利拉浓度的测定。Objective To establish a method for determination of enalapril and enalaprilat in human plasma by high-performance liquid chromatography tandemmass spectrometry. Methods After being mixed with the internal standard benazeprilat,plasma samples were deproteinized with methanol（ 0. 1% formic acid） and separated by HPLCMS / MS on a 30 ℃ Hedera ODS-2 C18（ 150 mm× 2. 1 mm,5 μm） column with a gradient elution by the mobile phase of methanol（ A） and 0. 1 % formic acid water solution（ B） at a flowrate of 0. 4 mL / min. Quantification was performed using multiple reaction monitoring（ MRM） of the transitions of m/ z 377. 2 → m/ z 234. 3 for enalapril,m/ z349. 3 → m/ z 206. 2 for enalaprilat and m/ z 397. 4 → m/ z 351. 4 for IS（ benazeprilat）,respectively. Results Calibration curves for enalapril and enalaprilat were linear over the range of 0. 2 ~ 200 ng / mL（ r = 0. 999 9）,0. 5 ~ 120 ng / mL（ r = 0. 999 3）,respectively. The intra-/ inter-batch RSD was less than 11. 3%. Conclusion The established method is rapid,specific and sensitive,it could be used for the quality control for the quantification of enalapril and enalaprilat in human plasma.

关 键 词：依那普利 依那普利拉 高效液相色谱-串联质谱法 人血浆 

分 类 号：R96[医药卫生—药理学] O657.63[医药卫生—药学]