超高效液相色谱-四极杆-飞行时间质谱组合化学计量学方法快速筛查肉中109种药物残留

目的 建立109种药物的超高效液相色谱-四极杆-飞行时间质谱（Ultra performance liquid chromatography-quadrupole-time-of-flight mass spectrometry，UPLC-Q-TOF-MS）数据库以及结合化学计量学主成分分析（principal component analysis，PCA）和正交偏最小二乘判别分析（orthogonal partial least squares discriminant analysis，OPLS-DA）构建肉中药物残留的快速筛查方法，并应用于阳性样本分析。方法 样本经提取、快速柱净化、色谱柱分离后，电喷雾电离源正离子模式电离，全信息串联质谱模式检测。设置对照组和实验组，研究药物添加数量、添加浓度及基质种类对PCA和OPLS-DA模型的影响，同时，以小鼠阳性样本为研究对象，运用模型进行差异目标物识别，并利用数据库进行验证。结果 建立了包含药物名称、分子式、CAS号、精确质量数等信息的109种药物数据库，PCA和OPLS-DA模型对不同样品中差异组分的辨析能力不受药物数量、药物浓度、基质种类的影响。同时，阳性小鼠样本中的未知药物多菌灵被精准识别。结论 UPLC-Q-TOF-MS组合化学计量学方法是一种简便的用于未知样品中差异组分快速筛选的方法，可实现肉中多药物残留组分的高通量筛查。

Rapid screening of 109 kinds of drug residues in meat by ultra performance liquid chromatography-quadrupole-time of flight-mass spectrometry combined with chemometrics

Objective To establish the ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) database of 109 drugs, and to develop a rapid screening and analysis method for the drug residues in meat by combining UPLC-Q-TOF-MS with chemometrics principal component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA). The method was applied to the analysis of positive samples. Methods After extraction, purification with rapid column and clean-up with chromatographic column, the samples were analyzed in positive ion mode and full information tandem mass spectrometry mode. The control group and experimental group were set up to study the influences of drug quantity, concentration and matrix on PCA and OPLS-DA. Taken mice as the research object, the different markers were identified by PCA and OPLS-DA, and verified by the established drug databases. Results 109 drug databases which including drug name, molecular formula, CAS number, accurate mass and other information was established. The ability of PCA and OPLS-DA to discriminate different components in different samples was not affected by drug quantity, concentration and matrix. Carbendazim, an unknown drug in positive mouse samples, was accurately identified. Conclusion UPLC-Q-TOF-MS combined with chemometrics is a simple approach for rapid screening of differential components in unknown samples, which can simultaneously identify and realize high-throughput screening of multi drug residues in meat.