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 mL 0.1％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。
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 UPLC TM BEH C 18 column using mobile phases of 0. 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 that 26 drugs were detected in ground water samples.
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