中兽药口服液中隐性药物筛查高分辨质谱方法的建立

Establishment of High Resolution Mass Spectrometry Method for Screening Recessive Drugs in Traditional Chinese Veterinary Medical Oral Liquid

建立了测定中兽药口服液中170种隐性药物的超高效液相色谱-四极杆静电场轨道阱质谱(HPLC-Q-Exactive Focus/MS)高通量筛查方法。通过构建药物筛查数据库并与样品中未知物信息进行比对,从而实现快速筛查中兽药口服液中隐性药物的种类和含量。数据库包括磺胺类、喹诺酮类、β-受体激动剂类、硝基咪唑类、苯并咪唑类、蛋白同化激素类、糖皮质激素类、喹噁啉类、四环素类、抗病毒类、酰胺醇类和真菌毒素类等12类170种药物的筛查参数。样品中人为添加化学药物,经1%甲酸乙腈提取,QuEChERs净化,氮气吹干,0.2%甲酸水复溶上机,正负模式扫描,TraceFinder软件筛查定性,当药物添加浓度为400 ng/g时,170种添加药物的检出率约为92.8%,随着药物浓度逐步提高至1μg/g时,所有添加药物均可检出。结果表明,该方法可满足中兽药口服液中隐性药物高通量快速筛查的需要,为打击畜禽养殖投入品中非法使用化学药物的行为提高技术支持和数据支撑。

An ultra performance liquid chromatography-quadrupole electrostatic field orbitrap mass spectrometry(HPLC-Q-Exactive Focus/MS) high-throughput screening method was developed for the determination of 170 recessive drugs in traditional chinese veterinary medical oral liquid. By constructing a drug screening database and comparing with the unknown information in the sample, the type and content of recessive drugs in veterinary oral liquid can be quickly screened. The database includes screening parameters for 170 drugs in 12 classes, including sulfonamides, quinolones, β-agonists, nitroimidazoles, benzimidazoles, protein-assimilating hormones, glucocorticoids, quinoxalines, tetracyclines, antivirals, amide alcohols and mycotoxins. The sample was artificially added with chemical drugs, extracted with 1% formic acid acetonitrile, purified by QuEChERs, dried by nitrogen, reconstituted in 0.2% formic acid water, scanned in positive and negative modes, screened and identified by TraceFinder software. When the drug concentration was 400 ng/g, the detection rate of 170 added drugs was about 92.8%. As the drug concentration gradually increased to 1 μg/g, all added drugs could be detected. The results indicated that this method could meet the needs of high-throughput rapid screening of recessive drugs in traditional chinese veterinary medical oral liquid, It could also improve technical support and data support for combating illegal use of chemical drugs in livestock and poultry products.