水中10种抗生素的全自动固相萃取-超高效液相色谱-串联质谱测定法

Determination of 10 antibiotics in drinking water by automatic solid-phase extraction-ultra high performance liquid chromatography tandem mass spectrometry

目的建立生活饮用水及水源水中10种抗生素的全自动固相萃取-超高效液相色谱串联质谱(UPLC-MS/MS)测定法。方法在1 000 ml水样加入Na_2EDTA充分溶解过滤后经全自动固相萃取装置浓缩净化,利用Waters ACQUITY UPLC HSS T3柱进行色谱分离,以乙腈-甲醇(V∶V=1∶1)和0.2%甲酸溶液为流动相,正离子模式扫描,多反应监测(MRM)模式检测。结果该方法线性范围为10~500μg/L,相关系数均大于0.99。10种抗生素的检出限为0.01~0.03μg/L,回收率为62.4~119%,RSD均小于10%。结论该方法准确、灵敏、快速,适用于水中抗生素的检测。

Objective To establish the method for determination of 10 antibiotics in drinking water by automatic solid-phase extraction-ultra high performance liquid chromatography tandem mass spectrometry （UPLC-MS/MS）. Methods 1 000 ml water sample added by Na2EDTA was filtered,then purified and concentrated by automatic solid-phase extraction, seperated by Waters ACQUITY UPLC HSS T3 column, eluted by mobile phase composed of acetonitrile-methanol （V/V=1：1） and 0.2% formic acid solution, multiple reaction monitoring （MRM） mode under positive ion scanning was used for mass spectrometry determination. Results The linear range was 10-500μg/L with r〉0.99.The detection limit was 0.01-0.03μg/L. The recovery rates were 62.4%-119%.The RSDs were 〈10%. Conclusion This method is accurate, sensitive, rapid and suitable for the detection of antibiotics in water.