色谱

色谱 ›› 2013, Vol. 31 ›› Issue (1): 15-21.DOI: 10.3724/SP.J.1123.2012.09015

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱法同时检测地表水中18种药物与个人护理品的残留量

朱赛嫦1, 王静2, 邵卫伟2, 陈红1*   

  1. 1. 浙江大学环境与资源学院环境工程系, 浙江 杭州 310058; 2. 浙江省环境监测中心, 浙江 杭州 310058
  • 收稿日期:2012-09-10 修回日期:2012-10-16 出版日期:2013-01-28 发布日期:2013-01-21
  • 通讯作者:
  • 基金资助:

    浙江省科技厅公益技术研究社会发展项目(2012C23043).

Simultaneous determination of 18 pharmaceuticals and personal care products in surface water by ultra-high performance liquid chromatography-tandem mass spectrometry

ZHU Saichang1, WANG Jing2, SHAO Weiwei2, CHEN Hong1*   

  1. 1. Department of Environmental Engineering, College of Environmental and Resource Science of Zhejiang University, Hangzhou 310058, China; 2. Zhejiang Environmental Monitoring Center, Hangzhou 310058, China
  • Received:2012-09-10 Revised:2012-10-16 Online:2013-01-28 Published:2013-01-21

PDF

342

被引次数

29

摘要： 采用固相萃取对水样进行预处理,建立了同时检测地表水中包括抗生素、β-阻滞剂、驱蚊剂、抗癫痫药、中枢神经兴奋剂、血脂调节剂、非甾体抗炎药、杀菌消毒剂在内的18种药物与个人护理品的超高效液相色谱-串联质谱分析方法。采用中性条件萃取水样,控制上样流速为2 mL/min,用甲醇-乙腈(1:1, v/v)溶液洗脱。纯水中的平均加标回收率为53.9%～112%,相对标准偏差为2.6%～15.3%(n=6);以地表水样加标100 ng/L为样品,目标分析物平均回收率为45.1%～156.6%,相对标准偏差为2.4%～15.7%(n=6)。结果表明,本方法可同时精确检测地表水样中的18种分析物,方法验证结果表明所建立的方法可靠。用该方法分析杭州余杭塘河水,结果检出9种分析物,其中咖啡因平均质量浓度达550.7 ng/L。结果表明该方法可靠。

关键词: 超高效液相色谱-串联质谱, 地表水, 固相萃取, 药物与个人护理品

Abstract: An analytical method has been developed and validated for the simultaneous determination of 18 pharmaceuticals and personal care products (PPCPs), including antibiotics (trimethoprim, erythromycin•2H2O, norfloxacin, ofloxacin, pencilline G, penicillin V potassium salt, cephalexin and sulfamethoxazole), β-bloker (atenolol), anophelifuge (N,N-diethyl-3-methylbenzoylamide, DEET), antiepileptics (carbamazepine), central nervous system stimulant (caffeine), lipid modifying agent (clofibric acid), non-steroidal anti-inflammatory drugs (ibuprofen, naproxen and diclofenac sodium salt) and antimicrobial agents (triclosan and triclocarban). The detection and qualification of the target compounds were performed by ultra-high performance liquid chromatography-tandem mass spectrometry. The optimized mobile phases were methanol as organic phase, 0.3% (v/v) formic acid-5 mmol/L ammonium acetate for positive electrospray ionization (ESI+) and 5 mmol/L ammonium acetate for ESI- as inorganic phase. Water samples were concentrated by solid phase extraction at 2 mL/min, and all the target PPCPs were efficiently extracted at pH 7. The extracted PPCPs were eluted by the mixture of methanol and acetonitrile (1:1, v/v). The average recoveries of the target compounds in the spiked pure water samples ranged from 53.9%-112%. The average recoveries of the target compounds ranged from 45.1%-156.6% with the relative standard deviations ranged from 2.4%-15.7%, in the surface water samples spiked at 100 ng/L. The surface water samples collected from Yu Hangtang River in Hangzhou were detected. The results showed that nine PPCPs were detected including caffeine that reached a maximum concentration of 550.7 ng/L. It proved that this analytical method is reliable and acceptable.

Key words: pharmaceuticals and personal care products, surface water, solid phase extraction (SPE), ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)