中兽药口服液中非法添加化学药物高分辨质谱筛查

Screening of Illegally Added Chemicals in Traditional Chinese Veterinary Medicine Oral Liquid by High Resolution Mass Spectrometry

建立了适用于中兽药口服液中167种非法添加化学药物的超高效液相色谱-四极杆静电场轨道阱质谱高通量筛查方法。样品采用0.5%甲酸乙腈-水进行振荡超声提取,电喷雾电离源(ESI)、正负离子同时扫描方式进行数据采集。通过与自建的167种化合物的基本信息及色谱-质谱信息数据库进行比对,对色谱-质谱条件、提取溶剂的种类和净化条件进行优化。将经前处理后的口服液样品上机测试后,采用Trace Finder筛查软件对数据结果进行分析。结果显示,50 ng/mL非法添加药物(头孢类和内酰胺类药物为100~200 ng/mL)上机时可定性检出。不同药物配方因基质影响,其非法添加药物的检出率略有差异。该方法可基本实现中兽药口服液中非法添加化学药物的高通量快速筛查,具备操作简便、快速高效的特点,为其他兽药剂型中非法添加药物的筛查奠定了基础。

A high-throughput screening method for 167 illegally added chemical drugs in traditional Chinese veterinary medicine oral liquid was established by ultra-high performance liquid chromatography-quadrupole electrostatic field orbit trap mass spectrometry. The samples were extracted with 0. 5% formic acid acetonitrile-water by oscillation ultrasonic extraction,and the data were collected with electrospray ionization source(ESI) in positive and negative ion scanning mode.By comparing the self-built the basic information and MS information database of 167 compounds,the chromatographic conditions, MS conditions, extraction solvent types and purification conditions were optimized,and the test results were analyzed.The results showed that the oral liquid samples after pretreatment were tested on the machine,and the data results were analyzed by Trace Finder screening software.It was found that the concentrations of illegally added drugs could be qualitatively detected when their concentrations were 50 ng/mL(cephalosporin and lactam drugs were 100-200 ng/mL).The detection rates for illegally added drugs were slightly different due to the influence of matrixes.With the characteristics of simple operation,rapidness and efficiency,this method could basically achieve the purpose of high-throughput rapid screening of illegally added chemical drugs in traditional Chinese veterinary medicine oral liquid,and it lays a foundation for the screening of illegally added chemical drugs in other veterinary drug formulations.