气相色谱-三重四极杆质谱法测定稻米中27种持久性有机污染物

Determination of 27 kinds of persistent organic pollutants in rice by gas chromatography-triple quadrupole mass spectrometry

中文关键词:  持久性有机污染物  多氯联苯  有机氯农药  多溴联苯醚  气相色谱-三重四极杆质谱法  稻米

英文关键词:persistent organic pollutants  polychlorinated biphenyl  organochlorine pesticides  polybrominated biphenyl ether  gas chromatography-triple quadrupole mass spectrometry  rice

中文摘要:

      目的 建立气相色谱-三重四极杆质谱法测定稻米样品中多氯联苯、有机氯农药和多溴联苯醚等27种持久性有机污染物的分析方法。方法 糙米粉样品经水化后, 采用乙酸乙酯进行2次直接提取, 采用5 g酸性硅胶(44%, m:m)固相净化柱进行净化后采用气相色谱-三重四极杆质谱在动态多反应离子监测模式进行分析, 内标法定量。结果 27种持久性有机污染物中, 4-溴联苯醚的回收率较低, 其他7种多氯联苯、7种有机氯农药和12种多溴联苯醚具有较好定量范围, 其中高取代溴联苯醚呈二次曲线, 回归系数均大于0.996; 方法检出限为0.002~1.543 ng/g之间, 高取代溴联苯醚的检测灵敏度略差; 方法回收率为59.3%~132.7%, 相对标准偏差为0.7%~10.8% (n=6)。结论 本方法样品前处理操作简单, 具有较好的灵敏度、准确度和精密度, 适用于稻米中极低含量持久性有机污染物的检测分析。

英文摘要:

      Objective To establish a method for the determination of 27 kinds of persistent organic pollutants in rice samples, including polychlorinated biphenyls, organochlorine pesticides and polybrominated diphenyl ethers by gas chromatography-triple quadrupole mass spectrometry. Method After hydration, brown rice flour samples were directly extracted twice with ethyl acetate, purified with 5 g acid silica gel (44%, m:m) solid phase purification column, and then analyzed by gas chromatography-triple quadrupole mass spectrometry in dynamic multi reaction ion detection mode, and quantified by internal standard method. Results Among the 27 kinds of persistent organic pollutants, the recovery rate of 4-bromodiphenyl ether was lower and other 7 kinds of polychlorinated biphenyls, 7 kinds of organochlorines and 12 kinds of polybrominated diphenyl ethers had good linear ranges, among which highly substituted brominated diphenyl ethers showed a quadratic curve, and the regression coefficients were greater than 0.996; the limits of detection were 0.002?1.543 ng/g, and the sensitivity of highly substituted bromodiphenyl ether was slightly poor; the recoveries were 59.3%?132.7%, and the relative standard deviations were 0.7%?10.8% (n=6). Conclusion This method has the advantages of simple sample pretreatment, good sensitivity, accuracy and precision, which is suitable for the detection and analysis of trace persistent organic pollutants in rice.