改良QuEChERS法与LC-MS/MS联用测定水产品中13种农药残留
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国家自然科学基金青年科学基金项目(31501398);国家农产品质量安全风险评估项目(GJFP2016009);广东省省级财政专项资金项目


Determination of 13 Pesticide Residues in Aquatic Products by Modified QuEChERs Method Coupled with LC-MS/MS Quantification
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    摘要:

    采用改良的QuEChERS方法提取与净化水产样品,建立氯嘧磺隆、异丙草胺、嘧菌酯等13种农药残留同时测定的液相色谱-串联质谱(LC-MS/MS)检测方法。样品用含1%乙酸的乙腈溶液提取,提取液用聚苯乙烯-二乙烯基苯(PS-DVB)和乙二胺-N-丙基硅烷(PSA)分散固相萃取净化,将目标物在电喷雾正离子(ESI+)电离,多反应监测(MRM)模式下测定,基质外标法定量。在优化的试验条件下,13种目标物在1~100 μg/L范围内线性关系良好,相关系数均大于0.99,方法检出限为0.15~0.75 μg/kg。分别对空白罗非和空白对虾按5,20 μg/kg和50 μg/kg等3个水平添加13种农药,目标物的平均回收率为75%~120%,相对标准偏差(RSD,n=5)均小于15%。采用该方法测定12份鱼样和18份虾样,在2份虾样中检出嘧菌酯,含量分别为 58.4 μg/kg和38.6 μg/kg。试验结果表明,PS-DVB作为QuEChERS分散固相吸附剂净化效果好、灵敏度高,且价格低廉,适用于水产品中农药多残留的检测。

    Abstract:

    An improved QuEChERs pretreatment method of 13 pesticide residues in aquatic products by liquid chromatography/tandem mass spectrometry (LC-MS/MS) was developed. The sample was extracted by 1%acidic acetonitrile and purified by polystyrene-divinylbenzene(PS-DVB) and primary secondary amine(PSA). The analyte was ionized in the positive-ion electrospray ionization (ESI+) under multiple reaction monitoring (MRM) mode. Under optimized conditions, good linear relationship (R>0.99) was obtained in a concentration ranged from 1 to 100 μg/L by external standard method, and the limits of detection were range from 0.15 to 0.75 μg/kg. The recoveries of spiked aquatic product samples were found to be 75%-120% with RSDs under 15%(n=5). The method was successfully applied in 12 fish and 18 shrimp, and the azoxystrobin was found in shrimps, the contents were 58.4 μg/kg and 38.6 μg/kg. The results indicated that the rapid cost-effective accurate method was proved successful in the determination of pesticide residues in aquatic samples. Furthermore, the method is more commercial than other QuEChERS methods with advantage of low cost of PS-DVB.

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尹 怡;赵 城;余 权;李丽春;刘书贵;单 奇;马丽莎;郑光明.改良QuEChERS法与LC-MS/MS联用测定水产品中13种农药残留[J].中国食品学报,2019,19(11):255-260

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  • 在线发布日期: 2019-12-02
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