【摘要】 建立了超高效液相色谱-电喷雾串联质谱(UPLC-ESI MS/MS)分析生活饮用水中54种药物的方法。采用HLB固相萃取柱对水样中的目标化合物进行富集净化,以5 mL甲醇洗脱;洗脱液用氮气吹至近干,用0.4 mL0.1%甲酸水溶液定容,上机分析;ACQUITY UPLCTMBEH C18柱用作色谱分离,以0.1%甲酸水溶液-甲醇为流动相进行梯度洗脱;多反应监测(MRM)模式进行检测;目标药物使用基质外标法定量。54种药物在自备井水、市政末梢水和地表水中的加标回收率分别为58.7%~104.4%、53.1%~109.5%和50.7%~118.8%,相对标准偏差(n=6)分别为0.3%~12.8%、1.0%~15.5%和0.4%~19.3%;方法定量限为0.002~5.000 ng/L。将建立的方法应用于北京部分自备井水、市政末梢水和地表水样品的分析,结果在自备井水样中检出26种药物。更多还原

【Abstract】 A method for the determination of 54 drugs in drinking water samples was developed by using ultra-high performance liquid chromatography-electrospray ionization tandem mass spectrometry(UPLC-ESI MS / MS). The target drugs in drinking water samples were enriched and cleaned-up by HLB solid-phase extraction(SPE) cartridges and then eluted with 5 mL methanol. The elute was collected,concentrated under a gentle stream of nitrogen gas,diluted with 0. 4 mL 0. 1% formic acid solution,and analyzed by UPLC-ESI MS / MS. The separation of the 54 drugs was performed on an ACQUITY UPLCTMBEH C18 column using mobile phases of0. 1% formic acid and methanol by gradient elution. The multiple reaction monitoring(MRM)mode was employed in mass spectrometry acquisition. The matrix-matched external standard calibration was used for quantitation. The results showed that the average recoveries of the drugs in ground water,tap water and surface water were 58. 7%- 104. 4%,53. 1%- 109. 5%,and 50. 7%-118. 8%,respectively,and the corresponding relative standard deviations(RSD,n= 6)were 0. 3%-12. 8%,1. 0%-15. 5%,and 0. 4%-19. 3%,respectively. The method quantification limits(MQL)for target compounds were in the range of 0. 002-5. 000 ng / L. The developed method was applied to analyze the water samples from Beijing. The results showed that26 drugs were detected in ground water samples.更多还原