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目的:建立HPLC-QTOF MS测定马来酸依那普利及中间体N-[1-(S)-乙氧甲酰基-3-苯丙基]-L-丙氨酸中对甲苯磺酸乙酯的方法。方法:采用Eclipse plus C18色谱柱(3.0 mm×100 mm,1.8μm),以20 mmol·L-1甲酸铵水溶液(A)-乙腈(B)为流动相,梯度洗脱(0～2 min,10%→50%B;2～4 min,50%→60%B;4～7 min,60%→90%B;7～8 min,90%B),流速1.0 mL·min-1,柱温50℃;采用正离子模式采集数据。结果:对甲苯磺酸乙酯浓度在0.20～5.01μg.mL-1范围内线性关系良好(r=0.9955);日内和日间精密度良好,RSD小于6.7%;定量限和检测限分别为0.4 ng、0.2 ng;马来酸依那普利及中间体回收率(n=9)分别为102.6%和90.8%。结论:本法简便、灵敏,可用于对甲苯磺酸乙酯的定量研究。
OBJECTIVE: To establish HPLC-QTOF MS for the determination of enalapril maleate and intermediate N- [1- (S) -ethoxycarbonyl-3-phenylpropyl] -L-alanine Ester method. Methods: The mobile phase was eluted with Eclipse plus C18 column (3.0 mm × 100 mm, 1.8 μm) with 20 mmol·L -1 ammonium formate (A) -acetonitrile (B) as mobile phase (0-2 min, 10% → 50% B; 2-4 min, 50% → 60% B; 4-7 min, 60% → 90% B; 7-8 min, 90% B) Temperature 50 ℃; Positive ion mode data acquisition. Results: The ethyl p-toluenesulfonate showed good linearity (r = 0.9955) in the range of 0.20 ~ 5.01μg.mL-1. The intra-day and inter-day precision was good with RSD less than 6.7%. The limits of quantitation and detection limits were 0.4 ng, 0.2 ng; enalapril maleate and intermediate recovery (n = 9) were 102.6% and 90.8%, respectively. Conclusion: This method is simple and sensitive and can be used for the quantitative study of ethyl p-toluenesulfonate.