绞股蓝中毒死蜱残留量SFE-GC/MS检测方法研究  

Determination of chlorpyrifos in Gynostemmna pentaphullum by supercritical fluid extraction and gas chromatography/mass spectrometry

作　　者：张璟[1] 唐光辉[1,2] 冯俊涛[1] 马志卿[1] 姚树萍 耿义良 张兴[1] 

机构地区：[1]西北农林科技大学无公害农药研究服务中心/陕西省生物农药工程技术研究中心,陕西杨凌712100 [2]西北农林科技大学林学院,陕西杨凌712100 [3]陕西省农药管理检定所,陕西西安710003 [4]陕西省山阳县林业局,陕西山阳726400

出　　处：《西北农林科技大学学报（自然科学版）》2009年第6期171-176,共6页Journal of Northwest A&F University(Natural Science Edition)

基　　金：国家"十五"科技攻关项目(2002BA516A04);西北农林科技大学人才基金项目

摘　　要：【目的】建立快速测定绞股蓝中毒死蜱残留量的超临界CO2萃取（SFE）和气相色谱-质谱结合的检测方法（SFE-GC/MS）。【方法】选择萃取压力、萃取温度、动态萃取CO2体积为影响萃取效果的主要因素,设计L16（43）正交试验,确定超临界CO2萃取绞股蓝中毒死蜱的最佳萃取条件,采用气相色谱-质谱选择离子检测模式对绞股蓝中残留的毒死蜱进行检测,并对毒死蜱在绞股蓝中的残留降解动态进行研究。【结果】超临界CO2萃取绞股蓝中毒死蜱的适宜条件为：采用先静态后动态的萃取方式,静态萃取时间为20 min,动态萃取条件为：压力41.370 MPa、温度50℃、CO2体积30 mL。毒死蜱超临界CO2萃取方法的添加回收率为88.87%-112.32%,相对标准偏差（RSD）为6.58%-13.78%,符合农药残留分析要求。在推荐用量（75 mL/hm^2）和加倍用量（150 mL/hm^2）条件下,毒死蜱在绞股蓝上的动态残留半衰期分别为2.36和2.21 d,喷药30 d后,已检测不到其在绞股蓝上的残留量。【结论】建立的毒死蜱SFE-GC/MS检测方法具有萃取效率高、无污染、经济等优点,适合于绞股蓝中毒死蜱残留量的检测。【Objective】In the present thesis,with the sample extraction by CO2 Supercritical Fluid Extraction（SFE） technology,fast detection protocols on chlorpyrifos residue in Gynostemmna pentaphullum were established using Gas Chromatography/Mass Spectrometry.【Method】The insecticide chlorpyrifos was extracted from Gynostemmna pentaphullum tissue by supercritical fluid extraction（SFE） and detected by Gas Chromatography/Mass Spectrometry（GC/MS）.The degradation dynamic of chlorpyrifos residue in Gynostemmna pentaphullum was investigated.【Result】The extraction conditions were optimized,including temperature,pressure and dynamic extraction.Gas Chromatography/Mass Spectrometry was used to examine the extracts.The suitable technology conditions were obtained as：firstly 20 min static extracting then turn to dynamic doing;the best dynamic extraction conditions was 41.370 MPa,50 ℃,dynamic extraction with 30 mL of CO2.Recoveries ranged from 88.87%-112.32%,and a method precision of 6.58%-13.78% was obtained for spiking levels of 0.1-2 mg/kg.Based on the recommended methods of one-dose and double-dose application,the half life ofchlorpyrifos residue degeneration period in Gynostemmna pentaphullum was 2.36 d and 2.21 d.【Conclusion】Compared to the general method SFE technique is simple and convenient,efficient,economical,and pollution-free.This method can be applied to detect chlorpyrifos residue in Gynostemmna pentaphullum.

关 键 词：超临界CO2萃取 残留动态 毒死蜱 绞股蓝 

分 类 号：S482.23[农业科学—农药学]