自动固相萃取—气相色谱—高分辨质谱法测定地表水中41种持久性有机污染物

陆一夫; 邱天; 胡小键; 丁昌明; 林少彬

doi:10.13421/j.cnki.hjwsxzz.2019.03.015

自动固相萃取—气相色谱—高分辨质谱法测定地表水中41种持久性有机污染物

Determination of 41 Persistent Organic Pollutants in Surface Water by Automatic Solid Phase-extraction Gas-chromatography High Resolution-mass Spectrometry

摘要

摘要:
目的建立同时测定地表水中41种持久性有机污染物的自动固相萃取—气相色谱—高分辨质谱方法（GC-HRMS）。
方法地表水样品采用HLB固相萃取柱富集提取，乙酸乙酯和二氯甲烷联合洗脱，氮吹浓缩进样分析。
结果 41种持久性有机污染物在（0.10~20.0）ng/L范围内线性关系良好，其相关系数均≥0.997，检出限范围（0.002~0.15）ng/L，定量限范围（0.005~0.51）ng/L，回收率范围70.4%~122.4%，精密度（RSD）范围4.2%~19.4%。
结论该方法操作简便，灵敏度高，选择性强，适用于同时测定地表水中41种持久性有机污染物。

Abstract:
Objectives To establish a method for simultaneous determination of 41 persistent organic pollutants in surface water by automatic solid phase extraction-gas chromatography-high resolution mass spectrometry(GC-HRMS).
Methods Water samples were extracted by HLB solid phase extraction, extracted with the mixture of dichloromethane and acetic ether, and the final eluate was then concentrated and detected.
Results The calibration curves of 41 persistent organic pollutants showed a good linearity in the range of (0.10~20.0) ng/L, and the correlation coefficients were more than 0.997. The detection limits(LOD)of method were in the range of (0.002~0.15) ng/L, and the limits of quantification(LOQ)of method were in the range of (0.005~0.51) ng/L. The spiked recoveries ranged from 70.4%~122.4% and the relative standard deviations ranged from 4.2%~19.4%.
Conclusions The method was simple, sensitive, selective and suitable for simultaneous determination of 41 persistent organic pollutants in surface water.

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