目的:建立超高效液相色谱-串联质谱(UPLC-MS/MS)结合标准加入法测定生脉注射液、参麦注射液、注射用益气复脉(冻干)中多效唑残留量。方法:采用Thermo Hypersil Gold色谱柱(100 mm×2.1 mm, 1.9 μm),以0.1%甲酸溶液和甲醇为流动相进行梯度洗脱,电喷雾电离源(ESI),正离子模式下多反应监测(MRM)。采用标准加入法进行样品测定。结果:线性关系良好,相关系数均>0.998,加样回收率全部指标在94.5%~119.8%,RSD为1.4%~2.5%,定量限为0.7~0.8 ng·mL-1。共筛查47批样品,其中85%的样品未检出多效唑,总体上安全可控,但3种注射液中均有部分批次样品有多效唑检出,具有一定安全风险。结论:标准加入法可有效克服基质效应,操作方便,该方法灵敏、准确、可靠。
Objective: To establish an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) combined with standard addition method for the determination of paclobutrazol residues in Shengmai injection, Shenmai injection and Yiqi Fumai injection (freeze-dried). Methods: Thermo Hypersil Gold column (100 mm×2.1 mm, 1.9μm) was used for gradient elution with 0.1% formic acid solution and methanol as mobile phase. Electrospray ionization (ESI) and multiple reaction monitoring (MRM) in positive ion mode were applied. Standard addition method was used in sample pretreatment. Results: The linear relationship of the method was good, and the correlation coefficients were greater than 0.998. The recoveries were in the ranges of 94.5%-119.8%, RSD was in the range of 1.4%-2.5%, and the lower limit of detection was in the range of 0.7-0.8 ng·mL-1. A total of 47 batches of samples were screened, of which 85% were not detected with paclobutrazole, which was generally safe and controllable. However, paclobutrazole was detected in some batches of samples in all three injections, which had a certain safety risk. Conclusion: The standard addition method can effectively overcome matrix effect and is easy to operate. The method is sensitive, accurate and reliable.
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