渔业水质中15种头孢菌素固相萃取-超高效液相色谱串联质谱测定方法的建立

Determination of 15 cephalosporins in fishery water by solid-phase extraction and ultrahigh performance liquid chromatography-mass spectrometry

本研究采用固相萃取技术进行前处理,利用超高效液相色谱串联质谱法建立渔业水质中15种头孢菌素的测定方法。500 mL水样经0.45μm滤膜过滤,经Oasis HLB固相萃取柱净化,洗脱收集后,进行液相色谱-串联质谱分析。采用Agilent SB-C_(18)色谱柱,以0.1%甲酸水溶液-乙腈体系作为流动相进行梯度洗脱,ESI源正离子模式电离,多反应离子监测模式(MRM)检测,内标法定量。结果表明,15种头孢菌素在1~50μg/L浓度范围线性关系良好,相关系数(r^(2))大于0.99,检出限为0.03~0.30μg/L,定量限为0.1~0.9μg/L;空白水样中的加标回收率在82.6%~116.3%,相对标准偏差(RSD)在1.51%~8.94%(n=6)。该方法检测耗时短、稳定性好、准确度高,适用于渔业水质中头孢菌素的测定。

This study established the detection method for 15 cephalosporins in fishery water by ultra high performance liquid chromatography-mass spectrometry,combined with solid-phase extraction for preparation.The water samples of 500 mL were filtered by 0.45μm membrane,and then purified through oasis HLB solid phase extraction column.After elution and collection,the obtained samples were analyzed by liquid chromatography tandem mass spectrometry.The samples were separated on an Agilent SB-C_(18) column under gradient elution with the mobile phase of acetonitrile containing 0.1%formic acid..The analysis was carried out by a positive electrospray ion source in the multiple reaction monitoring mode.The matrix-matched external internal standard method was applied for quantitative analysis.Good linear relationships were obtained for 15 cephalosporins in concentration ranges of 1~50μg/L,and the correlation coefficients were more than 0.99.The detection limits and quantification limits were 0.03~0.30μg/L and 0.1~0.9μg/L,respectively.The recoveries in blank samples were in the range of 82.6%~116.3%,along with relative standard deviations(RSD)of 1.51%~8.94%(n=6).This method is characterized with short analysis time,good stability and high accuracy,which is suitable for the determination of cephalosporins in different fishery water.