固相萃取-气相色谱-质谱联用测定土壤中4种拟除虫菊酯农药残留

Determination four Kinds of Pyrethroid Pesticides Residues in Soil with the Combined Use of Solid Phase Extraction-Gas Chromatography-mass Spectrometry

建立了固相萃取-气相色谱-质谱联用快速测定土壤中4种菊酯残留的方法。土壤试样经超声提取、弗洛里硅土柱净化,进气相色谱-质谱联用（GC-MS）检测。实验优化了超声时间、提取溶剂和超声功率对提取率的影响,当超声时间20min,提取溶剂石油醚：丙酮（1：2）,超声功率因数为90%时,菊酯的提取率最好。经过色谱条件优化,4种菊酯得到分离,在0.5-5 mg/L范围内呈现良好的线性,检出限低于3μg/L,回收率介于76.2-96.8%之间。建立的方法准确度好,灵敏度高,可用于土壤中菊酯残留的测定。

Asolid phase extraction-gas chromatography-mass spectrometry（SPE-GC-MS）-method was established for the determination four kinds of pyrethroid pesticides residues in soil. The samples were extracted by ultrasonic assisted extraction and purified by Florisil silica column,and were detected with gas chromatography-mass spectrometry（GC-MS）. Ultrasonic time,extraction solvent rate and ultrasonic power were optimized on the extraction rate. When the ultrasonic time was 20 min,extraction solvent petroleum ether ： acetone was（1： 2）,ultrasonic power was 90%,the extraction rate of pyrethroid was the best. The results showed that the method had good linearity in the range of 0. 5 - 5 mg/l,the detetion limits could reach less than 3 μg/l,and the recovery rate was between 76. 2 - 89. 8%. The established method was of good accuracy,high sensitivity,and could be used for the determination of pyrethroid residue in soil.