摘要：

建立了顶空固相微萃取-气相色谱-质谱法（HS-SPME-GC-MS）测定水中六氯环戊二烯的分析方法，采用顶空固相微萃取进样，DB-1色谱柱分离，气相色谱/质谱检测器检测，系统考察了不同涂层固相萃取针、进样口温度、固相萃取条件、盐效应等对测定结果的影响，并在最优实验条件下对方法进行了验证。结果表明，六氯环戊二烯在质量浓度为0.1~10 µg/L范围内与色谱峰面积线性良好，相关性系数为0.997，方法检出限为0.03 µg/L。对实际地表水和废水样品进行测定，废水样品监测结果为0.5 µg/L，地表水样品监测结果为未检出，对实际样品分别加标0.5 µg/L和1.0 µg/L测定，加标回收率为70%~87%，相对标准偏差为4.14%~13.9%（n=6）。该方法操作简单，不使用有机溶剂萃取，精密度好，准确度高，可用于快速测定工业废水和地表水中六氯环戊二烯。

关键词: 顶空固相微萃取, 气相色谱-质谱法, 水, 六氯环戊二烯

Abstract:

A headspace solid-phase microextraction gas chromatography-mass spectrometry(HS-SPME-GC-MS) method was established for the determination of hexachlorocyclopentadiene in water, with using headspace solid-phase microextraction injection, DB-1 chromatographic column separation, and gas chromatography/mass spectrometry detector detection. The effects of coating solid-phase extraction needles, inlet temperatures, solid-phase extraction conditions, salt effects on the determination were systematically investigated, and the method was validated under the optimal experimental conditions. The results showed that hexachlorocyclopentadiene exhibited good linearity with chromatographic peak area within the mass concentration range of 0.1-10 µg/L, with a correlation coefficient of 0.997 and a detection limit of 0.03 µg/L. The actual surface water and wastewater samples were measured, and the monitoring result of wastewater sample was 0.5 µg/L, while the monitoring result of surface water sample was not detected. The actual samples were spiked with 0.5 µg/L and 1.0 µg/L, respectively. The recovery rate was 70%-87%, and the relative standard deviation was 4.14%-13.9%(n=6). This method was simple to operate, did not use organic solvents for extraction, had good precision and high accuracy, which could be used for rapid determination of hexachlorocyclopentadiene in industrial wastewater and surface water.

Key words: headspace solid-phase microextraction, gas chromatography-mass spectrometry, water sample, hexachlorocyclopentadiene

中图分类号: 

• O657.7

• O657.63