目的:以益心酮片为例建立超高效液相色谱-串联质谱(UPLC-MS/MS)法同时检测37个非法添加化合物。方法:采用UPLCHSS T3 C18色谱柱(100 mm×2.1 mm,1.8 μm)分离,以0.1%甲酸-乙腈为流动相进行梯度洗脱。在电喷雾离子源正离子或负离子模式下,以多反应监测方式(MRM)检测,外标法定量。结果:37个待测化合物在相应的线性范围内呈良好的线性关系,相关系数(R2)均大于0.99;定量下限为3～10 μg·L-1;37个待测化合物的平均回收率为63.4%～138.3%。检测46批共78个样品,37个待测化合物中除了阿司匹林外,其他化合物均未检出。阿司匹林含量范围为每片0.847～3.261 μg,含量极低,不具有非法添加的意义。结论:本方法灵敏、高效,准确可靠,适用于益心酮片中非法添加具有解热镇痛效果化合物的检测。
Objective: To develop a method based on ultra-high-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) for the simultaneous detection of 37 compounds illegally added in Yixintong tablets as an example. Methods: The samples were separated on the UPLC HSS T3 C18(100 mm×2.1 mm, 1.8 μm) chromatographic column by gradient elution using 0.1% formic acid and acetonitrile as the mobile phase. The electrospray ion source was operated in both the positive and negative ion mode using the multi-reaction monitoring(MRM) method, and the results were quantified by the external standard method. Results: The correlation coefficients(R2) of the linear calibration curves were greater than 0.99 in the corresponding mass concentration ranges, and the limits of quantification(LOQs) for the analytes were 3-10 μg·L-1. The average recoveries ranged from 63.4% to 138.3%. Among the 37 compounds to be tested in 78 samples of 46 batches, no other compounds were detected except aspirin. The content of aspirin was 0.847-3.261 μg per tablet, the content was very low and had no significance of illegal addition. Conclusion: The established method is sensitive, rapid, accurate, reliable, and applicable for the detection of the illegal addition of antipyretic and analgesic affect compounds in Yixintong tablets.
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