气相色谱-三重四级杆串联质谱法检测广州市饮用水中3种酚类污染物含量  

Determination of the concentrations of 3 phenols in drinking water from Guangzhou city with gas chromatography-tandem mass spectrometry

作　　者：刘苗[1] 朱惠扬[1] 甘平胜[1] 彭荣飞[1] 杨荣[1] 

机构地区：[1]广州市疾病预防控制中心,广东广州510440

出　　处：《中国卫生检验杂志》2017年第2期163-165,173,共4页Chinese Journal of Health Laboratory Technology

基　　金：广州市医药卫生科技项目(20151A010079);广东省医学科学技术研究基金项目(A2015425)

摘　　要：目的检测和评价广州市饮用水中3种常见酚类(双酚A、4-辛基酚、4-壬基酚)的污染水平。方法水样经全自动固相萃取仪——OASIS HLB萃取小柱富集净化,二氯甲烷洗脱,氮吹浓缩后加入衍生剂双(三甲基硅烷基)三氟乙酰胺(BSTFA),在水浴中进行衍生化反应。采用气相色谱-三重四级杆串联质谱的多反应监测模式进行检测,内标法定量。结果 3种酚类物质在线性范围内线性关系良好,相关系数r均>0.99,回收率达77.3%~105%,方法检出限为0.40 ng/L^1.7 ng/L。在部分出厂水中检测出酚类物质,双酚A浓度为5.25μg/L^98.2μg/L,4-辛基酚浓度为1.05μg/L^5.20μg/L,4-壬基酚的浓度为1.84μg/L。桶装水和瓶装水中未检出上述3种酚类。结论运用全自动固相萃取仪进行前处理快速简便,节约了大量时间。该方法检出限低,可以应用于水样中痕量酚类物质的定量分析,具有较大的应用价值。Objective To determine and evaluate the contaminative level of 3 common phenols,including bisphenol A,4- n-Octylphenol and 4- n- Nonylphenol in drinking water from Guangzhou. Methods The water samples were concentrated and cleaned up by HLB extraction cartridge with automatic solid- phase extraction,and eluted with dichloromethane. The solvent was dried by nitrogen blow and then derivatized with BSTFA[Bis（ trimethylsilyl） trifluoroacetamide]in water bath. The collected solution was analyzed by triple quadrupole gas chromatography- tandem mass spectrometry using multiple reaction monitoring（ MRM） and quantified with internal standard method. Results Three phenols had good linearity in the correlation ranges,with the correlation coefficients（ r） all above 0. 99. The average recoveries of 3 phenols were within 77. 3%- 105%,and the limits of detection（ LOD） were within 0. 40 ng / L- 1. 7 ng / L. 3 phenolic compounds were detected in some of drinking water samples. The concentrations of bisphenol A,4- n- Octylphenol,4- n- Nonylphenol were respectively within 5. 25 μg / L- 98. 2 μg / L,1. 05 μg / L- 5. 20 μg / L,1. 84 μg / L. No phenols were detected in barreled water and bottled water. Conclusion The use of automatic solid- phase extraction instrument makes pretreatment quick and easy,saving a lot of time. The method has low detection limit and could be applied to quantitative analysis of trace phenols in water samples,and has great value in practical applications.

关 键 词：气相色谱串联质谱 饮用水 酚类 

分 类 号：O657.63[理学—分析化学]