固相萃取-高效液相色谱-串联质谱测定九龙江流域水中药品和个人护理用品

Determination of Pharmaceuticals and Personal Care Products in Jiulong River by Solid Phase Extraction and High Performance Liquid Chromatography-Tandem Mass Spectrometry

针对6大类共15种药品和个人护理用品(pharmaceuticals and personal care products,PPCPs)建立了固相萃取(SPE)-高效液相色谱-串联质谱检测(HPLC-MS/MS)的分析方法,并利用该方法,研究九龙江流域水体中PPCPs的污染现状.通过优化SPE、HPLC和MS的参数,提高了分析方法的灵敏度和准确性,所建立的方法对15种PPCPs的检出限和定量限分别为0.008 20～3.20ng/L和0.028 0～10.5ng/L.九龙江西溪和北溪各8个站位水样中PPCPs的研究结果表明,11种目标PPCPs都有不同程度的检出,其中三氯生和三氯卡班的检出率均为100%,布洛芬、美多心安、四环素、诺氟沙星和环丙沙星的检出率分别为93.8%、93.8%、68.8%、68.8%和50%;值得注意的是,九龙江北溪上游布洛芬和四环素的质量浓度高达65.1和106ng/L.结果表明,九龙江流域PPCPs污染状况需引起进一步关注.

In this study,an analytical method based on solid phase extraction （SPE） and high performance liquid chromatography- tandem mass spectrometry （HPLC-MS/MS） was established and used for the determination of 15 pharmaceuticals and personal care products （PPCPs）. The parameters of MS, HPLC and SPE were systematically optimized to improve the sensitivity and accuracy. The detection limits and quantification limits for 15 PPCPs were 0. 008 20-3.20 ng/L and 0. 028 0-10.5 ng/L, respectively. The proposed method was applied to the determination of PPCPs in 16 stations of Jiulong River. It was experimentally showed that 11 out of the 15 targeted PPCPs were detected, of which, the most frequently detected compounds were triclosan and triclocarban, which were detected in all samples, followed closely by ibuprofen, metoprolol, tetracycline, norfloxacin and ciprofloxacin, which were detected in 93.8%, 93.8 %, 68.8 %, 68.8 %and 50 % of all samples, respectively. The maximum concentration of ibuprofen and tetracycline in upstream of northern Jiulong River were as high as 65.1 ng/L and 106 ng/L, respectively. Further studies are needed for the comprehensive knowledge of PPCPs contaminants in Jiulong River.