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

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。

Abstract:

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.