超高效液相色谱串联质谱法同时检测小儿止咳平喘类中成药中28种非法添加化学成分OA
Determination of 28 Chemical Compounds Illegally Added in Pediatric Chinese Patent Medicines for Relieving Cough and Asthma by UPLC-MS/MS
目的 建立同时测定小儿止咳平喘类中成药中 28 种非法添加化学成分的超高效液相色谱串联质谱(UPLC-MS/MS)法.方法 色谱柱为 Waters UPLC BEH C18 柱(100 mm×2.1 mm,1.7 µm),流动相为乙腈-含 0.1%甲酸的 5 mmol/L 甲酸铵(梯度洗脱),流速为 0.3 mL/min,柱温为 40℃,进样量为2 µL;电离方式为电喷雾电离正离子模式(ESI+),采用多反应监测(MRM)模式进行定量分析.结果 28 种化学成分在各自质量浓度范围内与离子对峰面积的线性关系良好(R2＞0.995,n=11);检测限为 0.005～0.010 µg,定量限为 0.015～0.050 µg;精密度、稳定性、重复性试验结果的 RSD 均小于 8.0%(n=6);平均回收率为 80.23%～114.02%,RSD 为 0.82%～7.71%(n=6).4 个品种 12 批儿童用中成药样品(小儿止咳糖浆 3 批,小儿咳喘灵口服液 3 批,小儿咳喘灵颗粒 3批,小儿清肺化痰颗粒3批)中,有2批小儿咳喘灵颗粒样品检出咖啡因,其含量分别为2.75,2.98 mg/kg,其余27种成分均未被检出,综合检出率为16.67%.结论 所建立的方法灵敏、准确、快速,可用于小儿止咳平喘类中成药中多种非法添加化学成分的定量分析.
Objective To establish an ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the simultaneous determination of 28 chemical components illegally added in pediatric Chinese patent medicines for relieving cough and asthma.Methods The chromatographic column was Waters UPLC BEH C18 column(100 mm×2.1 mm,1.7 µm),the mobile phase was acetonitrile-5 mmol/L ammonium formate containing 0.1%formic acid(gradient elution),the flow rate was 0.3 mL/min,the column temperature was 40℃,and the injection volume was 2 µL.The ionization mode was the electrospray ionization positive ion mode(ESI+),and the quantitative analysis was carried out by the multi-reaction monitoring(MRM)mode.Results The 28 chemical components showed a good linear relationship with the peak area of ion pairs within their respective mass concentration ranges(R2＞0.995,n=11).The limit of detection was in the range of 0.005-0.010 µg,and the limit of quantification was in the range of 0.015-0.050 µg.The RSDs of precision,stability,and repeatability test results were all lower than 8.0%(n=6).The average recovery rates of 28 chemical components ranged from 80.23%to 114.02%,and the RSDs ranged from 0.82%to 7.71%(n=6).Among the twelve batches of four varieties of pediatric Chinese patent medicines(three batches of Xiao'er Cough Syrup,three batches of Xiao'er Kechuanling Oral Liquid,three batches of Xiao'er Kechuanling Granules,and three batches of Xiao'er Qingfei Huatan Granules),caffeine was detected in two batches of Xiao'er Kechuanling Granules samples,with the contents of 2.75 mg/kg and 2.98 mg/kg,respectively,while the other 27 components were not detected in samples,with a comprehensive detection rate of 16.67%.Conclusion The established method is sensitive,accurate,and rapid,which can be used for the quantitative analysis of multiple illegally added chemical components in pediatric Chinese patent medicines for relieving cough and asthma.
高萌;崔佳惠;撖志明;贺凯;张家萌
宁夏回族自治区药品检验研究院·宁夏药品质量控制与评价重点实验室,宁夏 银川 750004宁夏回族自治区药品检验研究院·宁夏药品质量控制与评价重点实验室,宁夏 银川 750004宁夏回族自治区药品检验研究院·宁夏药品质量控制与评价重点实验室,宁夏 银川 750004宁夏回族自治区药品检验研究院·宁夏药品质量控制与评价重点实验室,宁夏 银川 750004宁夏回族自治区药品检验研究院·宁夏药品质量控制与评价重点实验室,宁夏 银川 750004
医药卫生
超高效液相色谱串联质谱法止咳平喘儿童中成药非法添加化学成分
UPLC-MS/MSrelieving cough and asthmachildrenChinese patent medicinesillegal addition of chemical components
《中国药业》 2026 (11)
93-97,5
宁夏药品质量控制与评价重点实验室科研课题(2024年).
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