饮用水中35种抗生素的超高效液相色谱-串联质谱测定法

发布时间：2018-04-20 20:42

本文选题：固相萃取 + 超高效液相色谱-串联质谱　；参考：《环境与健康杂志》2017年08期

【摘要】：目的建立饮用水中35种抗生素类药物的超高效液相色谱-串联质谱(UPLC-MS-MS)测定方法。方法水样经0.45μm膜过滤,采用HLB固相萃取柱对水样中的目标物进行富集净化,用12 ml甲醇洗脱,洗脱液氮气环境下吹至近干,5%甲醇水溶液定容至1 ml,上机分析。选择ACQUITY UPLC HSS T3色谱柱(2.1 mm×100 mm,1.8μm)用作色谱分离,0.1%甲酸水溶液-甲醇为流动相进行梯度洗脱,质谱采用正离子扫描多反应监测(MRM)模式。结果在0.1~100μg/L的范围内,所得35种目标分析物的回归方程均具有良好的线性关系。方法的检出限为0.02~1.40 ng/L,定量下限为0.08~4.46 ng/L,加标回收率为63.0%~127.1%,RSD为0.6%~20.3%。结论该方法操作简单、快速,准确度和精密度均较高,适用于饮用水中35种抗生素的同时检测。
[Abstract]:Objective to establish a high performance liquid chromatography-tandem mass spectrometry (UPLC-MS) method for the determination of 35 antibiotics in drinking water. Methods the water sample was filtrated by 0.45 渭 m membrane and purified by HLB solid phase extraction column. The sample was eluted with 12 ml methanol. ACQUITY UPLC HSS T3 column (2.1 mm 脳 100mm ~ 1.8 渭 m) was used as mobile phase to separate 0.1% formic acid aqueous solution and methanol as mobile phase for gradient elution. Results in the range of 0.1 渭 g / L of 0.1 渭 g / L, the regression equations of the 35 target analytes have good linear relationship. The detection limit of the method was 0.02 ~ 1.40 ng / L, the lower limit of quantification was 0.08 ~ 4.46 ng / L, the recovery rate was 63.0% and 127.1% RSD was 0.6 ~ 20.3%. Conclusion the method is simple, rapid, accurate and accurate. It is suitable for simultaneous detection of 35 antibiotics in drinking water.
【作者单位】：中国疾病预防控制中心环境与健康相关产品安全所;
【基金】：国家卫生计生委委托研究项目
【分类号】：O657.63;R123.1

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