固相萃取-超高效液相色谱-串联质谱法测定水样中17种磺胺类抗生素

Determination of 17 sulfonamides in water samples by ultra-performanceliquid chromatography -tandem mass spectrometry after solid phase extraction

目的建立固相萃取-超高效液相色谱-串联质谱法测定水样中17种磺胺类抗生素药物(磺胺吡啶、磺胺嘧啶、磺胺甲恶唑、磺胺噻唑、磺胺甲基嘧啶、磺胺二甲恶唑、磺胺二甲异恶唑、磺胺甲噻二唑、磺胺喹恶啉、磺胺苯吡唑、磺胺多辛、磺胺二甲氧嗪、磺胺醋酰、磺胺苯甲酰、磺胺二甲嘧啶、磺胺间甲氧嘧啶和磺胺对甲氧嘧啶)的方法。方法采用HLB固相萃取柱富集纯化水样中磺胺类抗生素,经CSH C18(2.1 mm×100 mm,1.7μm)色谱柱分离,在电喷雾正离子多反应扫描监测模式下进行测定。结果 17种磺胺类抗生素在一定的浓度范围内线性关系良好,相关系数(r)>0.99。方法检出限(LOD)为0.014 ng/L^0.293 ng/L,定量限(LOQ)为0.046 ng/L^0.977 ng/L。在2.0 ng/L、10.0 ng/L、50.0 ng/L 3个添加水平下,其加标回收率为74.8%~108.6%,相对标准偏差为0.14%~8.61%。结论该方法灵敏度高、准确性好,可适用于水样中磺胺类抗生素的检测。

Objective To establish a method for the determination of 17 sulfonamides(sulfapyridine,sulfadiazine,sulfamethoxazole,sulfathiazole,sulfamerazine,sulfamoxole,sulfisoxazole,sulfamethizole,sulfaquinoxaline,sulfaphenazole,sulfadixine,sulfadimethoxine,sulfacetamide,sulfabenzamide,sulfadimidine,sulfamonomethoxine,sulfametoxydiazine)in water samples by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS).Methods The samples were extracted and purified by HLB solid phase extraction column.The analytes were separated on a CSH C18 column(2.1 mm×100 mm,1.7μm)and detected by using electrospray ionization positive ionization mode(ESI+)and multiple reaction monitoring(MRM).Results The method showed a good linearity within a certain concentration ranges with correlative coefficients(r)greater than 0.99.The detection limits were within 0.014 ng/L-0.293 ng/L,and the quantification limits were within 0.046 ng/L-0.977 ng/L.The average recoveries at the spiking levels of 2.0 ng/L,10.0 ng/L and 50.0 ng/L were in the range of 74.8%-108.6%,with the relative standard deviations(RSDs)in the range of 0.14%-8.61%.Conclusion The established method is highly sensitive and accurate,which is suitable for the detection of sulfonamides in water.