液相色谱-串联质谱法测定饮用水中6类12种药品和个人护理品

Determination of 12 pharmaceuticals and personal care products in drinking water by liquid chromatography-tandem mass spectrometry

建立了同时检测饮用水中6大类共12种典型药品和个人护理品(Pharmaceuticals and personal care products,PPCPs)的自动固相萃取-液相色谱-电喷雾三重四极杆串联质谱(ASPE-HPLC--ESI-MS/MS)方法.样品经ASPE(自动固相萃取)富集提取后,40℃氮吹至近干,用甲醇-水溶液(20∶80,V/V)定容至1 mL后测定.采用正离子和负离子多反应监测离子模式(MRM)定性分析,针对不同扫描模式优化流动相条件,两次进样分析.在低、中、高的3个添加水平下,12种PPCPs的方法回收率为60.8%—110%,相对标准偏差为2.0%—14.0%;检出限(LOD)为0.02—1.5 ng·L-1,定量限(LOQ)为0.06—5 ng·L-1.应用该方法调查了北京市饮用水中PPCPs污染状况,结果表明,9种PPCPs(氧氟沙星、脱水红霉素、磺胺甲恶唑、卡马西平、舒必利、普萘洛尔、萘普生、苯扎贝特和双酚A)在不同饮用水水样中被检出,最高浓度为苯扎贝特34.47 ng·L-1.该方法操作简单、灵敏度高、选择性强,符合饮用水样品中痕量污染物检测要求.

An analytical method was developed to determine 12 pharmaceuticals and personal care products（ PPCPs） in drinking water by automated solid phase extraction-high performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry（ ASPE-HPLC-ESIMS /MS）. The ASPE extracts were evaporated to near dryness at 40 ℃ under a stream of nitrogen,and were redissolved in 1 mL of methanol ∶water（ 20∶80,V /V） for further HPLC analysis. The mass spectrometric acquisition was carried out by means of multiple reaction monitoring（ MRM） in either positive or negative ionization mode. The detection limits（ LOD） and quantitation limits（ LOQ） of the 12 PPCPs were 0. 02—1. 5 ng·L-1and 0. 06—5 ng·L-1. The mean recoveries of the targeted 12PPCPs（ spiked at three concentration levels） were in the range of 60. 8% —110%,with relative standard deviations（ RSDs） of 2. 0% —14. 0%. The proposed method was used to determine the 12 PPCPs in drinking water in Beijing. It showed that ofloxacin,erythromycin-H2O,sulfamethoxazole,carbamazepine,sulpiride,propranolol,naproxen,bezafibrate and bisphenol A were detected,with the highest level of 34. 47 ng·L-1for bezafibrate. The method for the 12 representative PPCPs is simple,sensitive, specific, and complies with the regulations for the determination of tracecontaminant residues in drinking water.