HS-SPME-GC/MS法测定生活饮用水中环氧氯丙烷

李国威; 甘平胜; 李晓晶; 杨荣; 刘苗; 曾涛; 林静佳

doi:10.13421/j.cnki.hjwsxzz.2024.08.013

HS-SPME-GC/MS法测定生活饮用水中环氧氯丙烷

Determination of epichlorohydrin in drinking water by headspace solid-phase microextraction coupled with gas chromatography/mass spectrometry

摘要

摘要:
目的建立自动顶空固相微萃取-气相色谱质谱法测定生活饮用水中环氧氯丙烷。
方法采用80 μm DVB/Carbon WR/PDMS固相微萃取头, 在250 r/min振摇条件下, 35 ℃平衡15 min、顶空萃取15 min, 250 ℃解析5 min, 经DB-624色谱柱分离, 质谱仪检测, 外标法定量。
结果环氧氯丙烷在0.2~2.0 μg/L范围内线性良好(r=0.999 2), 方法检出限为0.03 μg/L, 定量限为0.09 μg/L, 相对标准偏差为2.2%~4.6%, 加标回收率为95.3%~102.8%。
结论本法操作简便, 可用于生活饮用水中环氧氯丙烷的测定。

Abstract:
Objective To establish a method of automatic headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography/mass spectrometry (GC/MS) for the determination of epichlorohydrin in drinking water.
Methods The 80 μm DVB/Carbon WR/PDMS was used as SPME fiber, with the condition of 250 r/min shaking, an equilibration time of 15 minutes at 35 ℃, a headspace extraction time of 15 minutes, and desorption at 250℃ for 5 minutes, and then the compound was separated by a DB-624 chromatographic column, detected by a mass spectrometer, and quantified by the external standard method.
Results Epichlorohydrin had good linearity in the range of 0.2-2.0 μg/L (r=0.999 2). This method had a detection limit of 0.03 μg/L, a quantification limit of 0.09 μg/L, a relative standard deviation of 2.2%-4.6%, and a recovery rate of 95.3%-102.8%.
Conclusion The method is simple and convenient and can be used for the determination of epichlorohydrin in drinking water.

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