棉纺织品中7种残留拟除虫菊酯杀虫剂的检测

建立同时提取和分析棉纺织品中7种拟除虫菊酯类农药残留样品的方法.使用气相色谱-质谱联用仪、弱极性HP-5 MS毛细管色谱柱,选择进样口温度250℃、0.6 mL/min的载气流速(氦气),在梯度升温条件下分离分析出7种拟除虫菊酯杀虫剂及异构体,产生17个色谱峰,分离效果较好.使用V正己烷/V丙酮=4∶1的混合溶剂采用超声提取法提取纺织品中残留农药,7种农药的工作曲线呈较好的线性关系(r0.99),且检测限低,在3个加标水平下进行了回收率和精密度实验,回收率在68.6%~99.8%之间,平行测定相对标准偏差为1.43%~13.20%(n=6).本方法回收率高,重现性好,满足Oeko-Tex Standard 100的要求,可作为生态纺织品中拟除虫菊酯杀虫剂的分离分析方法.

Extraction and Determination of Pyrethroid Pesticides Residues in Cotton Textiles

The analysis and determination of synthetic pyrethroid insecticides in textiles are paid more attention due to their uses in agricuhure and the control of veterinary. Hyphenation of GC and MS was used to determination of residual insecticides with HP-5 MS column at a programmed temperature. When a splitless volume of 1 μL was injected at 250 ℃ , employing helium as the carrier gas in constant flow mode at 0.6 mL/min, the GC-MS （TCI） chromatograms of mixture of seven kinds of pyrethroid insecticides were obtained with seventeen separated peaks. The cotton samples were uhrasonicably extracted with solvent （Vhexane /Vacetone = 4：1 ） , then the extracts were analyzed on GC-MS. Working curves of the seven insecticides were found to have good linearity （r 〉0.99）. The values of recovery measured by standard method were between 68.6% - 99.8% , and the values of RSD＇ s （ n = 6） were in the range of 1.43% - 13.20%. This method is reliable for determination of pyrethroid residues in textile.