固相萃取-气相色谱-质谱法同时测定水中9种药品及个人护理用品

Simultaneous determination of nine pharmaceuticals and personal care products in waters bysolid phase extraction-gas chromatography-mass spectrometry

采用固相萃取-气相色谱-质谱联用技术，建立了水体中9种药品及个人护理用品（水杨酸、萘普生、布洛芬、对乙酰氨基酚、降固醇酸、三氯生、双氯酚酸、酮洛芬和双酚 A）的定量分析方法。水样品经稀盐酸调节至 pH =3后，采用 Oasis HLB 固相萃取小柱进行富集净化；选用三甲基氢氧化硫（ TMSH）为衍生化试剂，在常温条件下对目标物进行快速甲基化；以气相色谱-质谱法选择离子监测模式（GC-MS-SIM）进行检测，由2，4，5-涕丙酸为内标进行定量分析。本实验分别对固相萃取和衍生化等前处理条件进行了系统的研究。在优化的实验条件下，方法的回收率为50.7～115.4％，相对标准偏差均不高于10％，检出限为0.03～0.30μg / L，定量限为0．15～1．50μg / L。利用该方法对东莞市某农田灌溉水进行了分析，4种目标物在样品中有检出，最大质量浓度范围为0.176～0.998μg / L。结果表明该方法操作简便，灵敏可靠。

An analytical method has been developed and validated for the simultaneous deter-mination of nine pharmaceuticals and personal care products（PPCPs）in water samples,inclu-ding salicylic acid,naproxen,ibuprofen,paracetamol,clofibric acid,triclosan,diclofenac, ketoprofen,bisphenol A. The qualification and quantification of the target compounds were per-formed by gas chromatography-mass spectrometry in selected ion monitoring mode（ GC-MS-SIM）. The water samples were concentrated and purified through Oasis HLB cartridges after the pH value of the water was adjusted to 3,then derivatized with trimethyl sulfonium hydroxide （TMSH）at room temperature,and determined by GC-MS-SIM using 2,4,5-fenoprop as internal standard. The conditions for sample pretreatment（ e. g. solid phase extraction and derivatiza-tion）were studied. Under the optimized conditions,the recoveries were ranged from 50. 7% to 115. 4% with the relative standard deviations lower than 10% . The limits of detection were in the range of 0. 03-0. 30 μg / L and the limits of quantification were in the range of 0.15-1.50 μg / L. The method has been successfully applied to monitor the occurrence of the PPCPs residues in agricultural irrigation water in Dongguan,Guangdong Province. The four compounds were detected at maximum mass concentration range of 0. 176-0. 998 μg / L. It proved that this analyt-ical method is sensitive,reliable and acceptable.