分散微固相萃取-高效液相色谱-串联质谱法测定水样中3种氯霉素类和11种激素类药物残留

Dispersive Micro-Solid Phase Extraction Combined with High Performance Liquid Chromatography-Tandem Mass Spectrometry for Determination of 3 Chloramphenicols and 11 Hormones Residue in Water Samples

基于官能化聚苯乙烯/二乙烯苯填料(PEP),采用分散微固相萃取(DMSPE)前处理技术,结合高效液相色谱-串联质谱法(HPLC-MS/MS),建立了同时测定水样中3种氯霉素类和11种激素类药物残留的分析方法。通过对DMSPE中PEP用量、吸附时间、样品溶液pH、洗脱溶剂的种类和体积等参数进行优化,实现了对水样中3种氯霉素类和11种激素类药物残留的有效提取和净化。分析物经C 18色谱柱分离,以水-甲醇为流动相,梯度洗脱,质谱采用电喷雾电离多反应监测(MRM)模式检测。3种氯霉素类和11种激素类药物在各自线性范围内的线性关系良好,相关系数均大于0.994;方法检出限为0.1~3.1 ng/L,定量限为0.2~10.4 ng/L、2、10、100 ng/L;4个加标水平的回收率在53.6%~90.4%范围,日内精密度为5.2%~16.9%。该方法快速、简便、灵敏,适用于水样中上述两类药物残留量的检测。

A novel method for the simultaneous determination of 3 chloramphenicols and 11 hormones residue in river and tap water was developed using dispersive micro-solid phase extraction(DMSPE)-high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)based on a functionalized polystyrene/divinylbenzene adsorbent(PEP).For DMSPE pretreatment method,the parameters that affected the extraction efficiency of 3 chloramphenicols and 11 hormones,such as the amount of PEP,the adsorption time,the pH of samples,the type and volume of eluent were studied.The analytes were separated on C 18 column by gradient elution with water-methanol as the mobile phases,and determined by multiple reaction monitoring mode using positive and negative ion switching electrospray mode(ESI^+,ESI^-).The analytes showed good linearity relationships in their concentration ranges.The limits of detection(S/N≥3)were in the range of 0.1-3.1 ng/L.The limits of quantification(S/N≥10)were in the range of 0.2-10.4 ng/L.The recoveries were from 53.6% to 90.4% at 4 spiked levels,and the intra-day relative standard deviations from 5.2% to 16.9%.The method is rapid,simple and sensitive,and provides the basis for the determination of chloramphenicols and hormonesdes residue in river and tap water.