色谱

色谱

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液相色谱-串联质谱法检测蜂蜜中杀虫脒及其代谢产物残留

伊雄海*, 韩丽, 杨惠琴, 樊祥, 朱坚, 郭德华   

  1. 上海出入境检验检疫局, 上海 200135
  • 收稿日期:2010-03-28 修回日期:2010-05-28 出版日期:2010-07-28 发布日期:1980-03-25
  • 通讯作者: 伊雄海

Determination of chlordimeform and its metabolite residues in honey using liquid chromatography-tandem mass spectrometry

YI Xionghai*, HAN Li, YANG Huiqin, FAN Xiang, ZHU Jian, GUO Dehua   

  1. Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China
  • Received:2010-03-28 Revised:2010-05-28 Online:2010-07-28 Published:1980-03-25
  • Contact: YI Xionghai

PDF

537

被引次数

10

摘要： 建立了液相色谱-串联质谱分析洋槐蜜、荆条蜜、蜂巢蜜、杂花蜜、野蜂蜜中杀虫脒及其代谢产物残留的方法。样品经氢氧化钠水溶液稀释溶解后,采用Waters Oasis HLB固相萃取柱净化。样品提取液经Agilent XDB-C18色谱柱分离,以0.1%甲酸水溶液和乙腈为流动相进行梯度洗脱。以电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测,基质匹配标准溶液外标法定量。杀虫脒及其代谢产物(4-氯邻甲苯胺)在2.5～250 μg/L范围内呈线性相关,相关系数(r)均大于0.999;定量限(S/N＞10)为5 μg/kg,检出限(S/N＞3)为2.5 μg/kg。各种蜂蜜基质样品在5、10和20 μg/kg添加水平时,杀虫脒及其代谢产物的回收率范围分别为75.8%～113.8%和85.6%～114.3%,相对标准偏差(RSD)分别为4.8%～10.2%和4.7%～9.1%,可以满足蜂蜜中杀虫脒及其代谢产物残留量的检测需要。

关键词: 代谢产物, 蜂蜜 , 杀虫脒, 液相色谱-串联质谱

Abstract: A liquid chromatography-tandam mass spectrometry (LC-MS/MS) method was developed for the determination of chlordimeform and its metabolite (4-chloro-o-toluidine) residue in acacia honey, chaste honey, comb honey, multifloral honey and wild honey. The samples were dissolved and diluted with sodium hydroxide solution, and cleaned up by a Waters Oasis HLB solid phase extraction column. The separation was performed on an Agilent XDB-C18 column with gradient elution using 0.1% formic acid solution and acetonitrile. The residues of chlordimeform and its metabolite were determined by electrospray ionization-tandem mass spectrometry, and quantified by the method of matrix-matched external standard. The calibration curves for chlordimeform and its metabolite showed good linearity in the range of 2.5~250 μg/L with the correlation coefficients (r) higher than 0.999. The limit of quantification was 5 μg/kg, and the limit of detection was 2.5 μg/kg. The recoveries of chlordimeform and 4-chloro-o-toluidine in honey at the spiked levels of 5, 10 and 20 μg/kg were in the ranges of 75.8%~113.8% and 85.6%~114.3%, respectively. The relative standard deviations were 4.8%~10.2% and 4.7%~9.1%, respectively. The method can meet the requirements for the determination of chlordimeform and 4-chloro-o-toluidine in honey for import and export inspection.

Key words: chlordimeform, honey , metabolite, liquid chromatography-tandem mass spectrometry (LC-MS/MS)