高效液相色谱-串联质谱法同时检测水体中26种药物及个人护理品

通过优化固相萃取条件和高效液相色谱-串联质谱参数,建立了可以同时检测地表水和地下水中26种典型药物及个人护理品(pharmaceuticals and personal care products,PPCPs),包括磺胺类、大环内酯类、喹诺酮类、酰胺醇类、精神类、消炎止痛类以及个人护理品的检测方法.通过将水样pH值调节至7,利用HLB固相萃取柱对水样中PPCPs进行富集,以甲醇和含0.005%甲酸的水溶液作为正离子模式流动相,甲醇和含0.5 mmol·L^-1乙酸铵的水溶液作为负离子模式流动相进行梯度洗脱,采用多反应监测的质谱扫描模式(MRM)分析测定.26种PPCPs的检出限为0.007—1.78 ng·L^-1,定量限为0.02—5.68 ng·L^-1,回收率为52.28%—115.24%.利用该方法检测北京潮白河地表水和地下水中PPCPs的浓度,结果表明,地表水中PPCPs的含量普遍高于地下水,磺胺甲恶唑、舒必利、咖啡因、卡马西平和布洛芬在地表水和地下水中的含量相对较高,检测浓度分别高达147.83、52.48、78.35、166.58、30.63 ng·L^-1.

Simultaneous determination of 26 pharmaceuticals and personal care products(PPCPs)in water using solid-phase extraction and liquid chromatography-tandem mass spectrometry

An analytical method was developed for the determination of 26 pharmaceuticals and personal care products(PPCPs)by solid-phase extraction(SPE)followed liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Water samples were concentrated with HLB cartridge at pH=7.Gradient elution was performed using methanol and 0.005%formic acid water in positive mode,and methanol and 0.5 mmol·L^-1 ammonium acetate in negative mode.The mass spectrometric acquisition was carried out by multiple reaction monitoring(MRM)mode.The limits of detection(LOD)and quantitation(LOQ)for the 26 PPCPs were 0.007—1.78 ng·L^-1 and 0.02—5.68 ng·L^-1.The recoveries for the 26 PPCPs were in the range of 52.28%—115.24%.The method was successfully applied to investigate occurrences of persistent PPCPs in surface water and groundwater of the Chaobai River.The result revealed that the concentration of PPCPs in the surface water was higher than those in the groundwater.Moreover,the concentration of sulfamethoxazole(147.83 ng·L^-1),sulpiride(52.48 ng·L^-1),caffeine(78.35 ng·L-1),carbamazepine(166.58 ng·L^-1)and ibuprofen(30.63 ng·L^-1)were higher than other PPCPs.