Wei Xiao, Zhang Ya-ying, Zhang Dong, Wang Xia, Sheng Ying-jie, Zhang Jing, Guo Shuai, Zheng Wei-wei, Chen Xin, Qu Wei-dong
Key Laboratory of Public Health and Safety, Ministry of Education, School of Public Health, Fudan University, Shanghai 200032, China.
Zhonghua Yu Fang Yi Xue Za Zhi. 2010 Jul;44(7):591-5.
To modify and optimize gas chromatographic conditions, qualitative and quantitative method on the base of the actual national standard detection method for drinking water on testing iodide with gas chromatography, and detect iodide in drinking water of Shanghai.
Iodobutane derivative was identified by gas chromatography/mass spectrometry, then two capillary columns coupled to electron capture detector were made by qualitative and quantitative analysis. Finally, 100 ml water samples were collected respectively from raw water and finished water of three plants in which water sources were Yangtse river, Huangpu river, and inner river respectively and detected by this developed method.
The results of mass spectrometry showed that iodide would form iodobutane which could generate 1-iodo-2-butanone and 3-iodo-2-butanone isomers by derivatization. The data of qualitative analysis by two capillary columns revealed that iodobutane was separated completely and the total time of chromatogram separation was 19.33 min.3-iodo-2-butanone with the high response value was selected to quantitatively analyse. The linear range was 1 - 100 µg/L, and the coefficient of determination (r(2)) was 0.9997. The limit of detection was 13 ng/L. Recoveries were between 97.68% and 104.37%, and relative standard deviations were between 2.14% and 4.41%. The results of iodide detected by this method in raw water and finished water in three plants in Shanghai showed that the ranking of iodide's concentration in raw water was Huangpu river (15.14 µg/L) > inner river (6.97 µg/L) > Yangtse river (3.55 µg/L). The level of iodide in finished water of plant 1 (3.55 µg/L and 5.92 µg/L for raw and finished water respectively) and 3 (6.97 µg/L and 9.62 µg/L for raw and finished water respectively) increased slightly except for plant 2 (15.14 µg/L and 1.81 µg/L for raw and finished water respectively). The relative standard deviations of all water samples measured in duplicate were less than 9.73%.
The improved method possesses higher degree of sensitivity and accuracy of qualitative and quantitative analysis than actual national standard detection method, and it is fit for trace analysis of iodide in water.
在现行国家标准饮用水中碘化物气相色谱检测方法的基础上,对气相色谱条件、定性和定量方法进行改进和优化,并检测上海市饮用水中的碘化物。
采用气相色谱/质谱联用仪对碘丁烷衍生物进行鉴定,然后通过两根与电子捕获检测器联用的毛细管柱进行定性和定量分析。最后,分别采集了以长江、黄浦江和内河为水源的三家水厂的原水和出厂水各100 ml水样,并用该改进方法进行检测。
质谱分析结果表明,碘化物经衍生化后会形成碘丁烷,碘丁烷可生成1-碘-2-丁酮和3-碘-2-丁酮异构体。两根毛细管柱的定性分析数据显示,碘丁烷分离完全,色谱分离总时间为19.33 min。选择响应值高的3-碘-2-丁酮进行定量分析。线性范围为1 - 100 μg/L,测定系数(r(2))为0.9997。检测限为13 ng/L。回收率在97.68%至104.37%之间,相对标准偏差在2.14%至4.41%之间。该方法对上海市三家水厂原水和出厂水中碘化物的检测结果表明,原水中碘化物浓度排序为黄浦江(15.14 μg/L)>内河(6.97 μg/L)>长江(3.55 μg/L)。除水厂2(原水和出厂水分别为15.14 μg/L和1.81 μg/L)外,水厂1(原水和出厂水分别为3.55 μg/L和5.92 μg/L)和水厂3(原水和出厂水分别为6.97 μg/L和9.62 μg/L)出厂水中碘化物含量略有增加。所有平行测定水样的相对标准偏差均小于9.73%。
改进后的方法比现行国家标准检测方法具有更高的灵敏度和定性、定量分析准确性,适用于水中碘化物的痕量分析。