液液萃取-超高效液相色谱-三重四级杆质谱测定地表水中19种磺胺类药物残留

建立了液液萃取-超高效液相色谱-三重四级杆质谱技术,测定地表水中19种磺胺类药物。通过乙酸乙酯超声萃取水样中的磺胺类药物,并用0.1%(体积分数)甲酸水溶液-甲醇作为流动相,C18色谱柱分离,在多反应监测(MRM)模式下测定。优化了萃取剂种类和用量、超声时间、流动相的组成等条件。在优化条件下,19种磺胺类药物在0.1~40.0μg/L范围内线性良好且相关系数均大于0.999 0,方法检出限为0.02~0.80ng/L,平均回收率为73.5%~92.8%,相对标准偏差为1.2%~8.7%。该方法操作简单、灵敏度高、所需样品及有机溶剂少,适用于实际的分析检验工作。

Determination of 19 sulfonamides residues in surface water by liquid-liquid extraction with UPLC-MS/MS

A liquid-liquid extraction/UPLC-MS/MS technique was established for the determination of 19 sulfonamides in surface water.The target compounds in water samples were extracted by ethyl acetate and separated on a C18 column,using 0.1%(volume fraction)formic acid aqueous solution and methanol as mobile phase.The data were collected by UPLC-MS/MS under multiple reactions monitoring(MRM)mode.The solvent type and dosage,ultrasonic time and mobile phase composition were optimized.Under optimal conditions,the calibration curves of 19 sulfonamides were linear in the range of 0.1-40.0μg/L and the correlation coefficients were greater than 0.999 0.The detection limits of the method were in the range of 0.02-0.80 ng/L.The average recoveries were in the range of73.5%-92.8%,and the corresponding relative standard deviations were in the range of 1.2%-8.7%.The method was simple,sensitive and required less sample and organic solvent.It was suitable for practical analysis and inspection.