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[摘要]
目的建立凝胶渗透色谱(GPC)和活性炭固相萃取柱(ENVI-Carb-SPE)结合的方法对样品进行净化处理,采用气相色谱-负化学电离源质谱联用(GC-NCIMS)的方法分析人参根及茎叶中三唑酮及其代谢产物三唑醇A、三唑醇B残留量的方法。方法样品以丙酮为提取溶剂超声提取,并采用凝胶渗透色谱(GPC)和活性炭固相萃取柱(ENVI-Carb-SPE)结合的方法进行样品的净化,DB-5MS毛细管柱程序升温分离,采用气质联用负化学电离源(NCI)SIM方式检测,以空白样品提取液配制对照品溶液,以克服基质效应,外标法测定。结果3种农药在10min内完全分离,根及茎叶样品在3个水平添加回收率在90%~105%,均小于6%(n=6)。三唑酮和三唑醇的检测限分别为0。1和10μg/L,仪器进样精密度均小于2%(n=6)。结论本方法简便、快速、灵敏度高,适用于人参中三唑酮和三唑醇农药残留量测定与安全监控。
[Key word]
[Abstract]
Objective To set up a clean-up method using gel permeation chromatography(GPC)and ENVI-Carb-SPE.The residues of triadimefon and its metablites,triadimenol A and triadimenol B in ginseng were detected by GC-MS with negative chemical ionization(NCI).Methods The sample was extracted with acetone and the extract was cleaned using GPC and ENVI-Carb-SPE.Based on GC-MS(NCI)the pesticides were separated on a DB-5MS column using a temperature program and were detected with a mass selective detector in selective ion monitoring(SIM)mode.The reference solution was prepared by the blank sample extract to overcome the matrix effect,the external reference method was used to detect.Results Three pesticides were separated within 10 min.The average spiked recoveries in three levels were 90%—105% with relative standard deviations(RSD)below 6%(n=6)in roots and stems.The limits of detection(LOD)of triadimefon and triadimenols were 0.1 and 10 μg/L.The precision was below 2%(n=6).Conclusion The method is sensitive for the residue analysis of three pesticides and could be used to the triadimefon and triadimenols detection and security control in ginseng.
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[基金项目]
“十一五”国家科技支撑项目“中药材资源与生产标准规范”(项目号:2006BAI21B07)