纺织学报 ›› 2013, Vol. 34 ›› Issue (5): 1-6.

• 纤维材料 •    下一篇

基于气相色谱法的含脂羊毛中4种拟除虫菊酯药物残留测定

牛春娥1,2,3,熊琳1,2,杨博辉1,2,郭天芬1,2,李维红1,2,王宏博1,杜天庆1,2   

    1. 中国农业科学院兰州畜牧与兽药研究所
    2. 农业部动物毛皮及制品质量监督检验测试中心
    3. 中国农业科学院兰州畜产品质量安全风险评估研究中心
  • 收稿日期:2012-05-22 修回日期:2012-12-12 出版日期:2013-05-15 发布日期:2013-05-09
  • 通讯作者: 牛春娥 E-mail:chuneniu@163.com
  • 基金资助:

    国家绒毛用羊产业技术体系分子育种科学家岗位项目;国家标准制定项目

 Determination of 4 pyrethroid pesticide residues in greasy wool based on gas chromatography

  • Received:2012-05-22 Revised:2012-12-12 Online:2013-05-15 Published:2013-05-09
  • Contact: chun-e NIU E-mail:chuneniu@163.com

摘要: 为了研究建立气相色谱-电子捕获检测器测定含脂羊毛中4种拟除虫菊酯杀虫剂残留的国家标准方法。在空白含脂毛中分别添加4个浓度水平(0.06 μg/g、0.30 μg/g、2.00 μg/g、5.00 μg/g)的4种拟除虫菊酯农药混标,以正己烷+乙醚(体积比2:1)为提取溶剂,中性氧化铝固相萃取柱和弗罗里硅土柱净化,以4 ml正己烷+乙酸乙酯(体积比95:5)进行洗脱,气相色谱-电子捕获检测器测定,外标法定量。结果显示:4种农药的最小检出量分别为0.020 μg/g、0.060 μg/g、0.024 μg/g和0.030 μg/g,平均回收率79.4%~101.2%,相对标准偏差1.20%~3.08%,分离良好,干扰峰少,结果准确,且操作简便、快捷,溶剂使用量小、符合环保要求。

关键词: 气相色谱, 含脂羊毛, 拟除虫菊酯农药, 残留

Abstract: n order to study and establish the national standard method of 4 kinds of pyrethroid pesticide residues in greasy wool by a gas chromatography - ECD method, the greasy wool?were added 4 levels mixed?standard reagent (0.06?μg/g,?0.30?μg/g,?2.00?μg/g,?5.00?μg/g),?which contains?4 kinds of pyrethroids, then the sample was extracted by n-hexane and aether(Volume ratio2:1), and then purified by a neutral alumina column and an florisil column and eluted by 4ml of n-hexane and ethyl acetate(Volume ratio95:5), finally detected by gas chromatography -ECD, the quantitative results were obtained based on external standard method. The result shows that the limits of detection of 4 kinds of pesticides were 0.020 μg/g, 0.060 μg/g, 0.024 μg/g and 0.030 μg/g respectively, the recoveries range were from 79.4% to 101.2%, the relative standard deviations were between 1.20% and 3.08%.So the method is an favorable separation effect, less disturbance, accurate, easy, quick, less use of solvent and environmental friendly.

Key words: gas chromatography, greasy wool, pyrethroid pesticide, residue

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