Shah Jaivik V, Shah Priyanka A, Shah Priya V, Sanyal Mallika, Shrivastav Pranav S
Department of Chemistry, School of Sciences, Gujarat University, Ahmedabad 380009, India.
Department of Pharmacy, M. S. University, Pratapgunj, Vadodara 390002, India.
J Pharm Anal. 2017 Jun;7(3):163-169. doi: 10.1016/j.jpha.2016.11.004. Epub 2016 Nov 25.
A sensitive and rapid liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed for the simultaneous determination of lisinopril (LIS) and hydrochlorothiazide (HCTZ) in human plasma using their labeled internal standards (ISs). Sample pre-treatment involved solid phase extraction on Waters Oasis HLB cartridges using 100 µL of plasma, followed by liquid chromatography on Hypersil Gold C (50 mm×3.0 mm, 5 µm) column. The analytes were eluted within 2.0 min using acetonitrile-5.0 mM ammonium formate, pH 4.5 (85:15, v/v) as the mobile phase. The analytes and ISs were analyzed in the negative ionization mode and quantified using multiple reaction monitoring. The method showed excellent linearity over the concentration range of 0.50-250.0 ng/mL for both the analytes. The intra-batch and inter-batch precision (% CV) was ≤5.26% and their extraction recoveries were in the range of 96.6%-103.1%. Matrix effect evaluated in terms of IS-normalized matrix factors ranged from 0.97 to 1.03 for both the analytes. The validated method was successfully applied to determine the plasma concentration of the drugs using 10 mg lisinopril and 12.5 mg hydrochlorothiazide fixed dose formulation in 18 healthy Indian volunteers.
已开发出一种灵敏且快速的液相色谱 - 串联质谱（LC-MS/MS）方法，用于使用标记内标（IS）同时测定人血浆中的赖诺普利（LIS）和氢氯噻嗪（HCTZ）。样品预处理包括使用100μL血浆在Waters Oasis HLB柱上进行固相萃取，然后在Hypersil Gold C（50mm×3.0mm，5μm）柱上进行液相色谱分析。使用乙腈 - 5.0mM甲酸铵，pH 4.5（85:15，v/v）作为流动相，在2.0分钟内洗脱分析物。在负离子模式下分析分析物和内标，并使用多反应监测进行定量。该方法在两种分析物的0.50 - 250.0 ng/mL浓度范围内显示出良好的线性。批内和批间精密度（％CV）≤5.26％，其提取回收率在96.6％ - 103.1％范围内。根据IS归一化基质因子评估的基质效应，两种分析物的范围均为0.97至1.03。经验证的方法成功应用于18名健康印度志愿者，以测定使用10mg赖诺普利和12.5mg氢氯噻嗪固定剂量制剂时药物的血浆浓度。
