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[同位素稀释气相色谱-质谱法测定饮用水中的环氧氯丙烷]

[Determination of epichlorohydrin in drinking water by isotope dilution gas chromatography-mass spectrometry].

作者信息

Huang Ying-yu, Xie Wei-ping, Chen Lin-gang

机构信息

Quanzhou Center for Disease Control and Prevention, Quanzhou, China.

出版信息

Zhonghua Yu Fang Yi Xue Za Zhi. 2013 May;47(5):455-8.

PMID:23958132
Abstract

OBJECTIVE

To establish a method for determination of the epichlorohydrin in drinking water by isotope dilution gas chromatography-mass spectrometry (GC-MS).

METHODS

The internal standard solution D5-epichlorohydrin was added in drinking water sample. The epichlorohydrin was firstly collected by active carbon, and the adsorbent was then centrifuged at 2739 × g for 10 min to remove water. Finally, the epichlorohydrin was desorbed by dipping the active carbon in 1.0 ml acetone for 1 h. The desorbed solution was tested by GC-MS and quantified with isotopic internal standards. The detection limit, precision and accuracy of the assay were evaluated. This method was adopted to detect the epichlorohydrin in drinking water for 25 batches in a city.

RESULTS

The determination method of epichlorohydrin represented a good linear relationship in the range of 0.0645-3.8700 µg/L, the linear regression equation was Y = 2.828X + 4.91 × 10(-2) (r > 0.999). When the epichlorohydrin concentration were 0.0806, 0.3230 and 3.2300 µg/L, the relative standard deviations (RSD) were 7.9%, 4.7% and 3.1%, respectively. The average recoveries were from 95.7% to 98.7%. The limit of detection (LOD) was 0.015 µg/L, limit of quantification (LOQ) was 0.052 µg/L. The content of epichlorohydrin in the 25 cases of drinking water was under the limit of detection.

CONCLUSION

The method is more simple than the national standard method, with high sensitivity, accuracy and good reproducibility, which is suitable for detection of the trace amounts of epichlorohydrin in drinking water.

摘要

目的

建立同位素稀释气相色谱 - 质谱联用法(GC-MS)测定饮用水中环氧氯丙烷的方法。

方法

向饮用水样品中加入内标溶液D5-环氧氯丙烷。环氧氯丙烷先用活性炭采集,然后将吸附剂在2739×g下离心10分钟以除去水分。最后,将活性炭浸入1.0 ml丙酮中1小时进行环氧氯丙烷解吸。解吸液用GC-MS检测并用同位素内标定量。评估该方法的检测限、精密度和准确度。采用该方法对某城市25批次饮用水中的环氧氯丙烷进行检测。

结果

环氧氯丙烷测定方法在0.0645 - 3.8700 μg/L范围内呈良好线性关系,线性回归方程为Y = 2.828X + 4.91×10(-2)(r > 0.999)。当环氧氯丙烷浓度为0.0806、0.3230和3.2300 μg/L时,相对标准偏差(RSD)分别为7.9%、4.7%和3.1%。平均回收率为95.7%至98.7%。检测限(LOD)为0.015 μg/L,定量限(LOQ)为0.052 μg/L。25份饮用水中环氧氯丙烷含量均低于检测限。

结论

该方法比国家标准方法更简便,具有高灵敏度、准确度和良好的重现性,适用于饮用水中痕量环氧氯丙烷的检测。

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