Page 57 - 理化检验-化学分册2024年第十二期

黄晓姗，等：超高效液相色谱-串联质谱法同时测定抗骨增生片中41种消炎止痛类化合物的含量

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Simultaneous Determination of 41 Anti-Inflammatory and Analgesic Compounds
in Kangguzengsheng Tablets by Ultra-High Performance Liquid Chromatography-
Tandem Mass Spectrometry

HUANG Xiaoshan, LI Qin, LIU Yanting, CHEN Haibin, CHEN Zaimin *

(Fujian Institute for Food and Drug Quality Control, Fuzhou 350000, China)

Abstract: The 20 Kangguzengsheng tablet samples were taken, removed of the coating and ground finely. An aliquot
(1 g) of powder was taken, and 25 mL of 50% (volume fraction) methanol solution was added. The mixture was ultrasonicated for
30 min at a water temperature not exceeding 60 ℃, shaken well and passed through a 0. 22 μm filter membrane. The filtrate was
determined by ultra-high performance liquid chromatography-tandem mass spectrometry. In chromatographic analysis, a Welch
Ultimate UHPLC XB-C 18 column (100 mm×2. 1 mm, 1. 8 μm) was used as the stationary phase, and a mixture of acetonitrile and
−1
0. 1% (volume fraction) formic acid solution containing 5 mmol · L ammonium acetate at different volume ratios was used as the
mobile phase for gradient elution. In mass spectrometry, positive and negative ion modes of electrospray ion source were used for
ionization, multiple reaction monitoring mode was used for detection, and external standard method was used for quantification.
It was shown that linear relationships between the peak areas of the corresponding quantitative ions and mass concentrations of
41 anti-inflammatory and analgesic compounds were kept in definite ranges, with correlation coefficients greater than 0. 991 0
and detection limits (3S/N) of 0. 1−2 μg · L −1 . Test for recovery was made according to the standard addition method, giving
recoveries in the range of 64. 0%−114%, and RSDs (n=6) of the determined values were less than 11%. The proposed method
was used for the analysis of 57 batches of samples from 33 production enterprises, and aspirin was detected in all samples. The
source of aspirin needed further experimental exploration. Acetaminophen was detected in 3 samples, presumable due to cross
contamination during the production process. The detected levels of aspirin and acetaminophen were much lower than the minimum
daily dose of the corresponding drugs.
Keywords: Kangguzengsheng tablet; ultra-high performance liquid chromatography-tandem mass spectrometry; illegal
addition; anti-inflammatory and analgesic compound

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