| 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/hm2)和加倍用量(150 mL/hm2)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. |
| 关键词: 超临界CO2萃取 残留动态 毒死蜱 绞股蓝 |
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| 基金项目: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 |
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| Determination of chlorpyrifos in Gynostemmna pentaphullum by supercritical fluid extraction and gas chromatography/ mass spectrometry |
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| Abstract: |
| 【Objective】 In the present thesis，with the sample extraction by CO2 Supercritical Fluid Extraction (SFE) technology,fast detection protocols on chlorpyrifos residue in Gynostemmna pentaphullumwere 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 inGynostemmna 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 pentaphullumwas 2.36d and 2.21d.【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. |
| Key words: supercritical CO2 extraction residual dynamic chlorpyrifos Gynostemmna pentaphullum |
