气相色谱微池电子捕获检测器测定蜂蜡中6种杀螨剂药物残留

doi:10.7506/spkx1002-6630-201018056

食品科学 ›› 2010, Vol. 31 ›› Issue (18): 244-247.doi: 10.7506/spkx1002-6630-201018056

气相色谱微池电子捕获检测器测定蜂蜡中6种杀螨剂药物残留

陈芳¹，李丹²，张金振¹，黄京平¹，赵静¹，吴黎明^1,*

1.中国农业科学院蜜蜂研究所，国家农产品加工中心蜂业分中心
2.北京城市学院生物医药系

收稿日期:2010-02-23 出版日期:2010-09-25 发布日期:2010-12-29
通讯作者: 吴黎明 E-mail:apiswu@126.com
基金资助:
国家现代农业(蜂)产业技术体系建设专项(NYCYTX-43)

Determination of Six Acaricide Residues in Beeswax by Gas Chromatography Coupled with a Micro-electron Capture Detector

CHEN Fang1，LI Dan2，ZHANG Jin-zhen1，HUANG Jing-ping1，ZHAO Jing1，WU Li-ming1,*

1. Apiculture Sub-Centers, National Agricultural Products Processing Center, Bee Research Institute, Chinese Academy of Agricultural
Sciences, Beijing 100093, China；2. Biological Medicine Department, Beijing City University, Beijing 100083, China

Received:2010-02-23 Online:2010-09-25 Published:2010-12-29
Contact: WU Li-ming1,* E-mail:apiswu@126.com

摘要/Abstract

摘要：

建立一种准确、快速、简便的蜂蜡中杀螨剂类药物多残留检测技术。样品经恒温水浴液- 液萃取、低温冷冻离心净化后用气相色谱微池电子捕获检测器测定。对提取溶剂的种类、体积及提取次数进行研究。结果表明：30.0mL 乙腈- 正己烷(V/V，2:1)是最佳提取溶剂。经两次冷冻及高速离心能将大部分的脂类基质去除。该方法的线性范围为0.01～4mg/L，相关系数均大于0.9878。检出限为0.96～4.69μg/kg，定量限为2.56～13.12μg/kg。该方法在3 个不同浓度水平的添加均有很好的回收率(83.8%～110.4%)，相对标准偏差为1.70%～6.60%。

关键词: 杀螨剂, 蜂蜡, 气相色谱微池电子辅获检测器

Abstract:

An accurate, fast and convenient method for simultaneous determination of 6 acaricide residues in beeswax by gas chromatography coupled with a micro-electron capture detector (GC-MECD) was established. The sample was saturated with hexane and acetonitrile in water bath with constant temperature. After frozen and centrifugation at 10000 r/min, the extract was analyzed by GC-MECD. Effects of extraction solvent, solvent volume and extraction times on extraction efficiency were explored. The best extraction solvent was 30.0 mL of acetonitrile-hexane (V:V, 2:1). Twice freezing and high speed centrifugation could remove the interference of lipid matrix. This method exhibited an excellent linear relationship over the range of 0.01 to 4.0 mg/L with a correlation coefficient of larger than 0.9878. The limits of detection (LOD) for the 6 acaricides varied from 0.96 to 4.69 μg/kg. The average recovery rates of these analytes spiked at three different levels ranged from 83.8% to110.4%, and the relative standard deviations (RSD) from 1.70% to 6.60%.

Key words: acaricide, beeswax, gas chromatography coupled with a micro-electron capture detector (GC-MECD)

中图分类号:

TS207.53

陈芳1，李丹2，张金振1，黄京平1，赵静1，吴黎明1,*. 气相色谱微池电子捕获检测器测定蜂蜡中6种杀螨剂药物残留[J]. 食品科学, 2010, 31(18): 244-247.

CHEN Fang1，LI Dan2，ZHANG Jin-zhen1，HUANG Jing-ping1，ZHAO Jing1，WU Li-ming1,*. Determination of Six Acaricide Residues in Beeswax by Gas Chromatography Coupled with a Micro-electron Capture Detector[J]. FOOD SCIENCE, 2010, 31(18): 244-247.

气相色谱微池电子捕获检测器测定蜂蜡中6种杀螨剂药物残留

Determination of Six Acaricide Residues in Beeswax by Gas Chromatography Coupled with a Micro-electron Capture Detector

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