DMSPE-HPLC-MS/MS法测定水中19种磺胺类药物

Determination of 19 Sulfonamides Residue in Water with Combination of Dispersive Micro Solid Phase Extraction and High Performance Liquid Chromatography-Tandem Mass Spectrometry

以强阳离子交换填料(PCX)为吸附剂,采用分散微固相萃取前处理(DMSPE)技术,结合高效液相色谱-串联质谱(HPLC-MS/MS)建立了同时测定河水和自来水中19种磺胺类药物残留的分析方法。通过对吸附剂用量、吸附时间、样品溶液的pH值、洗脱溶剂等参数进行优化,实现了DMSPE对水样中磺胺类药物的有效提取和净化。目标分析物经C18色谱柱分离,以0. 1%的甲酸水-乙腈为流动相进行梯度洗脱,在电喷雾正离子模式下进行多重反应监测。19种磺胺类药物在其线性范围内的线性相关系数(r2)均大于0. 993,方法检出限在0. 5~3. 1 ng/L,定量限在1. 7~10. 3 ng/L;3个加标水平下的回收率在55. 1%~102. 4%,相对标准偏差在4. 5%~23. 0%。该方法简便、灵敏、快速,适用于河水和自来水中磺胺类药物残留的监测。

A new method for the simultaneous determination of 19 sulfonamides residue in river and tap water was developed,which used dispersive microsolid phase extraction(DMSPE)-highperformance liquid chromatography-tandem mass spectrometry with strong cation exchange substance(PCX) as adsorbent. For DMSPE pretreatment method,the parameters that affected the extraction efficiency of the 19 sulfonamids,such as the amount of PCX,the adsorption time,the pH of samples,the type and volume of eluent were optimized. The target analyte was separated on C18 column by gradient elution with acetonitrile-0. 1% formic acid in water as the mobile phases,and determined by multiple reaction monitoring mode(MRM) using electrospray positive ion source(ESI+). The 19 sulfonamides showed good linearity relationships in their concentration ranges with correlation coefficients(r2) over 0. 993. The limits of detection were in the range of 0. 5-3. 1 ng/L. The limits of quantification were in the range of 1. 7-10. 3 ng/L. The recoveries were from 55. 1% to 102. 4% at 3 spiked levels,and the relative standard deviation was(RSDs) from 4. 5% to 23. 0%. The method is rapid,simple and sensitive,and is suitable for the determination of sulfonamides residues in river and tap water.