摘要
目的建立QuEChERS-超高效液相色谱-串联质谱法(UPLC-MS/MS),测定散装凉茶中6种非法添加的化学药物(对乙酰氨基酚、马来酸氯苯那敏、氢溴酸右美沙芬、安替比林、盐酸苯海拉明和萘普生等)。方法凉茶样品经含0.8%(V/V)甲酸的乙腈提取,C_(18)吸附剂净化,BEH C18超高效液相色谱柱(3.0 mm×150 mm,1.7μm)分离,多重反应监测(MRM)正离子模式扫描,标准曲线外标法定量。结果 6种化学药物的检出限为0.10μg/L^1.0μg/L;定量限为0.4μg/L^4.0μg/L;在线性范围内相关系数为0.998 4~0.999 4。3个不同添加水平下的平均加标回收率为72.3%~107.4%,RSD为1.2%~6.3%(n=6)。应用该方法对广州市售25份不同品牌散装凉茶样品进行测定,1份样品检出对乙酰氨基酚和马来酸氯苯那敏,浓度分别为721 mg/L和4.29 mg/L。结论该方法简便、快速、准确,可用于凉茶中非法添加的6种化学药物的快速筛查。
Objective To develop a method for determination of 6 chemical drugs（ paracetamol,chlorphenamine,dextromethorphan,antipyrine,diphenhydramine and naproxen） illegally added in herbal tea by QuEChERS with ultra-performance liquid chromatography-tandem mass spectrometry（ UPLC-MS/MS）. Methods The samples were extracted by acetonitrile with0. 8% formic acid,purified with C18 adsorbent,separated by BEH C18 ultra high performance liquid chromatography column（ 3. 0 mm × 150 mm,1. 7 μm）. Quantitative analysis was performed by a tandem quadrupole mass spectrometer operated under multiplereaction monitoring（ MRM） mode in positive ion detection mode. Results The detection limits of the 6 chemical drugs were within 0. 10 μg/L-1. 0 μg/L and the limits of quantification were within 0. 40 μg/L-4. 0 μg/L. In the linear range,the correlation coefficient was within 0. 998 4-0. 999 4. The average recoveries of the sample ranged from 72. 3% to 107. 4% under three different additive levels with the RSD ranged from 1. 2% to 6. 3%（ n = 6）. The developed method was used for the determination of 25 samples bought from markets. The results showed that the concentration of paracetamol and chlorphenamine in1 sample was 721 mg/L and 4. 29 mg/L,respectively. Conclusion The method is simple,rapid,accurate and can be used for rapid screening of 6 chemical drugs illegally added in herbal tea.
出处
《中国卫生检验杂志》
CAS
2017年第16期2287-2290,2294,共5页
Chinese Journal of Health Laboratory Technology
基金
广州市医药卫生科技项目(20151A010082)
