色谱

色谱 ›› 2014, Vol. 32 ›› Issue (3): 263-267.DOI: 10.3724/SP.J.1123.2013.11034

• 研究论文 • 上一篇    下一篇

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

贾妍艳1,2, 谭建华1,2,3, 徐晨1,2, 汤嘉骏1,2, 王赢利1,2, 解启来1,2   

  1. 1. 华南农业大学资源环境学院, 广东 广州 510642;
    2. 土壤环境与废物资源农业利用广东高校重点实验室, 广东 广州 510642;
    3. 广州市质量监督检测研究院, 广东 广州 510110
  • 收稿日期:2013-11-18 修回日期:2014-01-03 出版日期:2014-03-08 发布日期:2014-03-04
  • 通讯作者: 解启来

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

JIA Yanyan1,2, TAN Jianhua1,2,3, XU Chen1,2, TANG Jiajun1,2, WANG Yingli1,2, XIE Qilai1,2   

  1. 1. College of Natural Resources and Environment of Source China Agricultural University, Guangzhou 510642, China;
    2. Key Laboratory of Soil Environment and Waste Reuse in Agriculture of Guangdong Higher Education Institutes, Guangzhou 510642, China;
    3. Guangzhou Quality Supervision and Testing Institute, Guangzhou 510110, China
  • Received:2013-11-18 Revised:2014-01-03 Online:2014-03-08 Published:2014-03-04

PDF

302

被引次数

20

摘要：

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0.03~0.30 μg/L，定量限为0.15~1.50 μg/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0.176~0.998 μg/L。结果表明该方法操作简便，灵敏可靠。

关键词: 固相萃取, 气相色谱-质谱联用, 水样, 衍生化, 药品及个人护理用品

Abstract:

An analytical method has been developed and validated for the simultaneous determination of nine pharmaceuticals and personal care products (PPCPs) in water samples, including salicylic acid, naproxen, ibuprofen, paracetamol, clofibric acid, triclosan, diclofenac, ketoprofen, bisphenol A. The qualification and quantification of the target compounds were performed 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 derivatization) 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 analytical method is sensitive, reliable and acceptable.

Key words: derivatization, gas chromatography-mass spectrometry (GC-MS), pharmaceuticals and personal care products (PPCPs), solid phase extraction (SPE), waters

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