摘要
目的 建立超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定止咳平喘保健食品和中成药中25种非法添加的化学成分。方法 样品采用甲醇超声提取,经色谱柱分离,以甲醇(含0.1%甲酸)-0.1%甲酸溶液梯度洗脱,采用电喷雾离子源正负离子模式,多反应监测(MRM)模式检测。结果 25种止咳平喘药物在各自线性范围内与测定值线性关系良好,相关系数均≥0.9990;检测限为1.5~37.2 ng·g^(-1),平均回收率72.0%~109.8%,RSD为0.10%~8.7%。应用该方法对10批样品进行筛查,共有2批中成药胶囊剂中检出标识外成分,其中1批检出茶碱,另1批检出那可丁和盐酸麻黄碱。结论 该方法操作简便,具有良好的选择性、灵敏度及准确度,能够用于止咳平喘类保健食品和中成药中非法添加药物的测定。
Objective To establish an ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method to simultaneously determine 25 illegally added chemical components in anti-cough and anti-asthmatic health food and traditional Chinese medicine.Methods The samples were extracted by methanol ultrasonic extraction,the separation was executed on an column with mobile phase consisting of methanol(containing 0.1%formic acid)-0.1%formic acid solution,and detected by electrospray ionization source in positive and negative ion mode with multiple reaction monitoring(MRM)mode.Results The 25 anti-cough and anti-asthmatic drugs had good linearity with the correlation coefficients no less than 0.9990.The limits of detection ranged 1.5~37.2 ng·g^(-1),the average recoveries ranged 72.0%~109.8%,and the RSD ranged 0.10%~8.7%.The method was applied to screen 10 batches of samples,two batches of unlabeled components were detected in two traditional Chinese medicine capsules,among which theophylline was detected in 1 batch and noscapine and ephedrine hydrochloride were detected in 1 batch.Conclusion The method is easy to operate,has good selectivity,sensitivity and accuracy,and can be used for the determination of illegally added drugs of anti-cough and anti-asthmatic components in health food and traditional Chinese medicine.
作者
张珊珊
贾昌平
郑佳新
ZHANG Shan-shan;JIA Chang-ping;ZHENG Jia-xin(Suzhou Institute for Drug Control,Suzhou Jiangsu 215000)
出处
《中南药学》
CAS
2023年第12期3293-3298,共6页
Central South Pharmacy
