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.
ZUO Tian-tian, ZHANG Lin-lin, JIN Hong-yu, WANG Dan-dan, FANG Cui-fen, MA Lin-ke, CHEN Bi-lian, ZAN Ke, MA Shuang-cheng
. Detection of 37 compounds illegally added in Yixintong tablets by ultra- high performance liquid chromatography-tandem mass spectrometry*[J]. Chinese Journal of Pharmaceutical Analysis, 2021
, 41(10)
: 1739
-1747
.
DOI: 10.16155/j.0254-1793.2021.10.11
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