直接进样/液相色谱—串联质谱法同时测定地表水中22种典型抗生素

建立了直接进样/高效液相色谱—三重四级杆串联质谱法同时测定地表水中22种抗生素的检测方法,水样经0.22μm亲水性PTFE微孔滤膜过滤后直接进样,以流动相乙腈和0.1%甲酸水溶液梯度洗脱,采用高效液相色谱经Proshell 120 EC-C18色谱柱分离,三重四极杆串联质谱仪检测。结果显示,6类22种抗生素在0.001~2.00 ng/mL,线性良好,平均加标回收率为80.4%~113.0%。采用该方法对辽河流域多条河流进行检测,共检出17种抗生素,含量为1.0~493.0 ng/L,其中大环内酯类中的罗红霉素检出浓度最高,最高浓度为493 ng/L,其次是氯霉素类氟苯尼考、磺胺类磺胺甲噁唑。该方法操作简单、灵敏度高,排除了前处理过程对于不同抗生素回收率的影响,可用于地表水中多种类抗生素的准确、快速检测分析。

A direct injection/high performance liquid chromatography-triple quadrupole tandem mass spectrometry(HPLC-MS/MS)method was developed for the simultaneous determination of 22 kinds of antibiotics in surface water.The water samples were filtered by 0.22μm hydrophilic PTFE membrane and then directly injected.The mobile phase consisted of 0.1%formic acid aqueous solution and acetonitrile for gradient elution,separated by high performance liquid chromatography on Proshell 120 EC-C18 column,detected by three quadrupole tandem mass spectrometry.The results showed that 22 antibiotics had good linear relationship at the level of 0.001-2.00 ng/mL,and the average recoveries were 80.4%-113.0%.This method was used to detect the water quality of many rivers in Liaohe River Basin,17 kinds of antibiotics were detected with the content of 1.0-493.0 ng/L.Among them,macrolide roxithromycin had the highest detection concentration,with the highest concentration of 493 ng/L,followed by chloramphenicol,florfenicol and sulfamethoxazole.The method is simple,sensitive and can be used for the rapid and accurate determination of antibiotics in surface water.