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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。
A liquid chromatography-tandem mass spectrometry (LC-MS / MS) method was developed for the determination of imidacloprid and its metabolites imidacloprid, imidacloprid and 6-chloronicotinic acid in honey and bee pollen. Based on the Qu ECh ERS method, the p H value, extraction times and purification materials of the extraction solution were optimized according to the chemical properties of the target and the sample impurities. The solution was finally extracted twice with 5% formic acid-acetonitrile solution, and then was separated by MgSO4 and NaCl. The extracts were purified by enhanced lipid removal (EMR) and determined by LC-MS / MS. Quantitative analysis. The results showed that the average recoveries of imidacloprid, imidacloprid, imidacloprid and 6-chloronicotinic acid in honey and bee pollen were 86.0% ~ 111.5% with RSDs between 1.7% ~ 9.6% 0.20, 3.50, 0.40 and 14.00 μg / kg, respectively, and the limits of quantitation were 0.60, 11.64, 1.20 and 45.00 μg / kg, respectively. The method has the advantages of fast analysis, high sensitivity and good reproducibility, and is suitable for the rapid determination of imidacloprid and three metabolites in honey and bee pollen.