摘要
目的:建立检测中药和保健食品中16种非法掺加的抗炎类和抗组胺类化学药品的专属性方法。方法:样品经甲醇提取,采用液相色谱-离子阱质谱联用法测定。色谱条件:Agilent ZORBAX SB-C_(18)(2.1 mm×150 mm,5μm),流速0.3 mL·min^(-1),柱温30℃,16种化合物分为3个液相系统,分别以不同比例的0.5%甲酸溶液-乙腈进行梯度洗脱;质谱条件:离子源ESI,雾化气压力2.07×10~5Pa,干燥气流速8 L·min^(-1)。,干燥气温度350℃,自动扫描模式。通过与标准谱库中保留时间和多级质谱图的双重对比,对样品中非法掺加的化学药品进行定性鉴别。结果:在20批供试品中,分别检测到曲安缩松和氯苯那敏。结论:该方法准确、快速、灵敏度高,为国内首次报道的检测种类最多的液相质谱方法。
Objective：To establish a specific method for the identification of 16 anti - inflammatory and anti - his- tamine chemical drugs added illegally into traditional Chinese medicines and health food. Methods：The liquid chro- matography - ion trap mass spectrometry method was used to detect the samples extracted with methanol. The HPLC chromatographic determinations were run on an Agilent 1100 HPLC/MSD trap using Agilent ZORBAX SB -C18 （2. 1 mm × 150 mm,5 μm）column. The column temperature was 30 ℃. The 16 compounds were designed into 3 teams. The mobile phase were grading of 0. 5 % formic acid solution and acetonitrile at a flow rate of 0. 3 mL · min-1. The mass spectrometer condition were as follows：The ionization mode was ESI, the pressure of nebulizer gas was 2.07 ×10^5 Pa,the flow rate of drying gas was 8 L · min -1,the temperature of drying gas was 350℃,the mode was autoscan. Comparing with retention time and spectra of references in library set up by ourselves, the target com- pounds in sample are screened and identified. Results：Triamcinolone and chlorpheniramine were detected respectively. Conclusions ：The method is accurate, fast and sensitive. It is the first time in China to report the LC/MS method for detection of so many chemical drugs.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2008年第12期2065-2068,共4页
Chinese Journal of Pharmaceutical Analysis
关键词
抗炎类
抗组胺类
中药和保健食品
非法掺加
液相色谱-离子阱质谱联用
anti - inflammatory and anti - histamine
traditional Chinese medicines and health food
illegal
liquid chromatography- ion trap mass spectrometry
