摘要
目的建立同时检测痛风类中成药中17种非法添加物的超高效液相色谱-串联质谱方法。方法将痛风类中成药用100%甲醇超声提取,冷却至室温后,再用纯水定容,稀释至适当浓度,过0.22μm有机膜,待测。使用Agilent Eclipse Plus C18色谱柱进行17种非法添加物分离,流动相为乙腈(0.1%乙酸)-水(0.1%乙酸),在优化的洗脱梯度和时间条件下,17种非法添加物在10 min内实现良好分离,串联四级杆质谱仪检测,MRM方式采集并定量。结果17种非法添加物检出限为0.1 mg/L,在线性范围为1.0μg/L^100μg/L,相关性好,线性相关系数r>0.9892,3个添加水平的平均回收率为72.3%-104.7%,相对标准偏差(RSD)为1.7%-9.3%。结论本方法经济、快速、简单、高效,能够满足痛风类中成药中多种非法添加物同时检测要求。
Objective To establish a method for simultaneous detection of 17 illegal additions in gout Chinese patent medicine by using ultra performance liquid chromatography-tandem mass spectrometry. Methods The ultrasonic extraction from gout Chinese patent medicines was conducted with 100% methanol. After cooling to room temperature, the sample’s volume was set with pure water, then diluted to appropriate concentration, and filtered using 0.22 μm organic filtration. All the 17 illegal additions were well separated on Agilent Eclipse Plus C18 column within 10 min under the optimized gradient and time, with acetonitrile(0.1% acetic acid)-water(0.1% acetic acid) as the mobile phase. It was detected by a tandem quadrupole mass spectrometer and collected and quantified by MRM. Results The result showed that the limits of detection(LODs) for the 17 illegal additions were 0.1 mg/L, with linearity of 1.0 μg/L-100 μg/L and the correlation coefficients(r) above 0.989 2. The average recoveries of the 17 illegal additions in matrices were within 72.3%-104.7%, and the relative standard deviation(RSD) was within 1.7%-9.3%. Conclusion This economical, fast, simple and efficient method could be used for simultaneous detection of multi illegal additions in gout Chinese patent medicines.
作者
勇艳华
李鹏
边海涛
董广彬
YONG Yan-hua;LI Peng;BIAN Hai-tao;DONG Guang-bin(Dalian Institute for Food Control,Dalian,Liaoning 116630,China)
出处
《中国卫生检验杂志》
CAS
2019年第22期2711-2714,共4页
Chinese Journal of Health Laboratory Technology
关键词
痛风类中成药
非法添加物
超高效液相色谱-串联质谱法
Gout Chinese patent medicine
Illegal additions
Ultra high performance liquid chromatography-tandem mass
