文章摘要
母玉敏,叶 玫,吴成业,余 颖,邓武剑.气相色谱法测定南美白对虾中10种拟除虫菊酯残留方法的研究[J].上海海洋大学学报,2011,20(3):399-404
气相色谱法测定南美白对虾中10种拟除虫菊酯残留方法的研究
Determination of 10 pyrethroids residues in Penaeus vannamei by gas chromatography
  
DOI:
中文关键词: 拟除虫菊酯  水产品  气相色谱法
英文关键词: pyrethroids  aquatic product  gas chromatography
基金项目:福建省海洋与渔业厅重点项目(闽海渔合同〔2009〕1-17 号)
作者单位
母玉敏 福建农林大学 食品科学学院 
叶 玫 福建省水产研究所 
吴成业 福建省水产研究所 
余 颖 福建省水产研究所 
邓武剑 福建省水产研究所 
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中文摘要:
      建立了气相-电子捕获检测器(GC-ECD)同时测定南美白对虾(Penaeus Vannamei)中七氟菊酯等10种拟除虫菊酯类药物残留的检测方法。样品经正己烷-乙酸乙酯-丙酮有机溶剂提取后,先采用乙腈饱和的石油醚除脂,再通过Florisil层析柱净化,最后利用GC-ECD同时测定七氟菊酯等10种拟除虫菊酯类药物残留。实验结果表明:该方法在1 ng/mL~100 ng/mL浓度范围内线性良好,相关系数r≥0.999 51;在南美白对虾空白样本中加标浓度为2 μg/kg、10 μg/kg、20 μg/kg 3个水平下(七氟菊酯对应为1 μg/kg、5μg/kg、10 μg/kg)相应的回收率在78.0%~110.0%之间,日内精密度为4.0%~12.0%(n=6 ) ,日间精密度为2.3%~12.0%(n=3);按照10倍信噪比计算,七氟菊酯的检测限为1.0 μg/kg;联苯菊酯、甲氰菊酯、三氟氯氰菊酯、氯氰菊酯、氰戊菊酯、溴氰菊酯、氟胺氰菊酯、氯菊酯、氟氯氰菊酯的检测限为2.0 μg/kg。该方法快速、准确、可靠,适合于测定水产品中拟除虫菊酯类药物的残留。
英文摘要:
      The method for determination of 10 pyrethroids residues such as tefluthrin in Penaeus vannamei by gas chromatography with electron capture detection (GC-ECD) was developed. Pyrethroids were extracted with hexan ethylacetate actone organic solvent and lipids were removed with petroleum ether saturated with acetonitrile. After purification by Florisil column, 10 pyrethroids residues were detected simultaneously by GC-ECD. The results indicated that the working curves were linear (r≥0.999 51) in the range of 1-100 ng/mL for 10 pyrethroids . When spiked with 2 μg/kg, 10 μg/kg and 20 μg/kg of pyrethroids (1 μg/kg, 5 μg/kg and 10 μg/kg for tefluthrin) in Penaeus vannamei blank sample, the average recoveries were 78.0%-110.0% and the intra day RSD (n=6) were 4.0%-12.0% and the inter day RSD (n=3) were 2.3%-12.0%. The detection limit as estimated by 10 times signal to noise method for tefluthrin was 1.0 μg/kg and that for bifenthrin, fenpropanate, cyhalothrin, pemethrin, cyfluthrin, cypermethrin, tau fluvalinate, fenvalate, deltamethrin was 2.0 μg/kg respectively. This method can detect pyrethroids residues in aquatic product quickly and exactly.
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