超高效液相色谱-质谱联用法同时测定地下水中23种药物残留

建立了一种采用固相萃取、超高效液相色谱-质普联用技术快速并同时测定地下水中23种药物残留的方法.样品经HLB固相萃取富集净化,以反相C18柱为分离柱,甲醇和0.1%的甲酸溶液进行梯度洗脱,结合多时间段多反应监测的质谱扫描方法(mp MRM),可在10 min内同时检测地下水中10种磺胺类药物、7种喹诺酮类药物及6种β-受体激动剂药物.结果发现,该方法在1.0~100.0 ng·m L-1的浓度范围内峰面积与药物浓度呈良好的线性关系,相关系数均大于0.99,回收率在80%~110%,检测限和定量限分别为0.5 ng·m L-1和1.0 ng·m L-1.研究表明,该方法快速灵敏,专属性好,可用于地下水中药物残留的快速检测.

Simultaneous determination of 23 drug residues in groundwater using UPLC-MS/MS

A high ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with HLB solid-phase extraction and multi-period multiple reaction monitoring scan method(mpMRM) has been developed for the simultaneous detection of ten kinds of sulfonamides, seven kinds of quinolones and six kinds of beta-agonists in a single run of ten minutes. The extracts were cleaned up and preconcentrated by an HLB cartridge. Separation was performed on a reverse-phase Cl8 column with gradient elution of methanol (incl. 0.1% formic acid). The developed method showed good precision and accuracy with recoveries of 80%~110% for all the drugs. The linear range was 1.0~100.0 ng·mL^-1, and the correlation coefficient was above 0.99. The testing results showed the detection limit of 0.5 ng·mL^-1 and the quantification limit of 1.0 ng·mL^-1. The result demonstrated that the method is convenient, rapid and exclusive and can be applied in screening drug residues from groundwater.