液相色谱-串联质谱法测定蜂产品中吡虫啉及其3种代谢物

发布时间：2018-02-04 11:12

  本文关键词： 液相色谱-串联质谱 蜂蜜 蜂花粉 吡虫啉 吡虫啉烯烃 吡虫啉脲 -氯烟酸 增强型脂类去除材料　出处：《分析化学》2017年04期 　论文类型：期刊论文

【摘要】：建立了蜂蜜和蜂花粉中吡虫啉及其代谢物吡虫啉烯烃、吡虫啉脲、6-氯烟酸的液相色谱-串联质谱(LC-MS/MS)检测方法。在Qu ECh ERS方法基础上,针对目标物化学性质和样品杂质情况,对提取溶液的p H值、提取次数、净化材料等参数进行了优化。最终以5%甲酸-乙腈溶液提取两次,无水Mg SO_4、NaCl盐析分层,提取液经增强型脂类去除材料(EMR)净化,以LC-MS/MS进行测定,基质外标法进行定量分析。结果表明,蜂蜜和蜂花粉中吡虫啉、吡虫啉烯烃、吡虫啉脲、6-氯烟酸的平均加标回收率为86.0%~111.5%,相对标准偏差在1.7%~9.6%之间,检出限分别为0.20、3.50、0.40和14.00μg/kg,定量限分别为0.60、11.64、1.20和45.00μg/kg。本方法分析速度快、灵敏度高、重现性好,适用于蜂蜜和蜂花粉中吡虫啉及其3种代谢物的快速测定。
[Abstract]:Imidacloprid and its metabolite imidacloprid olefin and imidacloprid urea in honey and bee pollen were established. Determination of 6-Chlorotinic Acid by liquid Chromatography-tandem Mass Spectrometry (LC-MS / MS). Based on the qu ECh ERS method, the chemical properties of the target and the impurity of the sample were studied. The pH value of extraction solution, extraction times and purification materials were optimized. Finally, 5% formic acid-acetonitrile solution was used to extract twice, and anhydrous mg so _ 4 + NaCl salting out was stratified. The extract was purified by enhanced lipids removal material (EMR), determined by LC-MS/MS and quantitatively analyzed by matrix external standard method. The results showed that imidacloprid and imidacloprid olefins were found in honey and bee pollen. The average recovery of imidacloprid 6-chlorniacin was 86.0 and 111.5, the relative standard deviation was between 1.7 and 9.6%, and the detection limit was 0.20 ~ 3.50. The quantitative limits of 0.40 渭 g / kg and 14.00 渭 g / kg were 0.60 渭 g / kg and 45.00 渭 g / kg, respectively. It is suitable for rapid determination of imidacloprid and its three metabolites in honey and bee pollen.
【作者单位】： 省部共建国家重点实验室培育基地"浙江省植物有害生物防控重点实验室"农业部农药残留检测重点实验室浙江省农业科学院农产品质量标准研究所;南京农业大学植物保护学院;中国农业大学理学院;中国农业科学院蜜蜂研究所;
【基金】：浙江省自然基金项目(No.LQ14B070004) 特色农产品全产业链安全风险管控项目(No.ZJNY2016001) 蜂产品全产业链安全风险管控项目(No.ZJNY2016001-02)资助
【分类号】：S896.8;O657.63
【正文快照】： 1引言新烟碱类杀虫剂为昆虫乙酰胆碱受体激动剂,是继有机磷类、氨基甲酸酯类和拟除虫菊酯类等杀虫剂之后的第四大类杀虫剂[1]。吡虫啉是其代表性药剂,主要用于防治水稻、小麦、棉田中的蚜虫、叶蝉、飞虱等30多种刺吸式口器害虫、地下害虫[2]。吡虫啉对哺乳动物低毒,但对蜜蜂具，

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