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小麦中多氯联苯、有机氯农药和多溴联苯醚检测方法研究(网络首发、推荐阅读)
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Research on Determination of Polychlorinated Biphenyl, Organochlorine Pesticides and Polybrominated Biphenyl Ether in Wheat(Online First, Recommended Article)
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    摘要:

    建立了基于气相色谱-三重四极杆串联质谱的分析方法,用于小麦中多氯联苯,有机氯农药和多溴联苯醚的同时检测分析。小麦粉样品加水后,使用乙酸乙酯直接提取,采用44%硅胶净化柱进行净化,净化浓缩后的样品使用气相色谱-三重四极杆质谱进行检测,质谱检测器采用动态多反应监测(dMRM)模式。通过内标法定量。多氯联苯、有机氯农药和多溴联苯醚具有较好线性范围,其中七溴代联苯醚、八溴代联苯醚、九溴代联苯醚和十溴代联苯醚的响应与浓度呈二次曲线回归;方法检出限在0.001~1.108 ng/g之间,溴联苯醚随溴原子数量增加而检测灵敏度降低;方法回收率在57.9%~118.6%之间,相对标准偏差在1.6%~10.7%之间。该方法简单、快速、准确、经济,适用于大批量小麦样品中痕量持久性有机污染物的筛查和分析检测。

    Abstract:

    This study is objected to develop a gas chromatographic-tandem mass spectrometric method to determine the contamination level of polychlorinated biphenyls, organochlorine pesticides and polybrominated biphenyl ether in wheat. In this method, the hydrated wheat powder was extracted with ethyl acetate and purified with acidic silica (44%). The gas chromatography-tandem mass spectrometry which operated on a dynamic multiple reaction monitor (dMRM) acquisition mode was using for instrumental analysis. The quantitation was carried out with internal standard method. The results demonstrated that all target analytes have good quantitative linear range with excellent regression factor (R2>0.996), while highly brominated biphenyl ethers were with quadratic regression. The recovery of method was between 57.9% to 118.6% with relative standard deviations of 1.6%~10.7%. The method detection limits were between 0.001 ng/g and 1.108 ng/g as the highly brominated biphenyl ether gave relatively poor detection limits. This method is simple, rapid, accurate and low-cost, especially useful for the high-throughput analysis of trace persistent organic pollutants in wheat.

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张 炜,杨永坛*,王松雪,李 森,李 丽,蔡 娣.小麦中多氯联苯、有机氯农药和多溴联苯醚检测方法研究(网络首发、推荐阅读)[J].粮油食品科技,2022,30(2):148-160.

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  • 在线发布日期: 2022-03-24
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