摘要
目的优化顶空-固相微萃取-气相色谱法测定中草药中拟除虫菊酯类农药残留的条件。方法样品经丙酮超声提取,顶空固相微萃取净化、富集后,采用气相色谱-电子捕获检测器检测;对影响顶空-固相微萃取的主要因素如萃取涂层类型、萃取温度及时间等进行条件试验。结果选择聚二甲基硅氧烷(PDMS 100μm)固相微萃取萃取头,萃取溶剂为丙酮-水(1∶4),加入0.5 g氯化钠,95℃顶空萃取40 min;色谱柱为DB-608。结论前处理方法简便、快速,几乎不使用有机溶剂,适用于中草药中拟除虫菊酯类农药残留检测。
Objective exploring detection pyrethroids in traditional chineses medicine by using headspace solid - phase microextracton （HS- SPME）. Method After acetone extraction assisted with ultrasonic, then analyzed by gas chromatograph（C,C） equipped with an dec- tron capture detector（ECD） ; the main influential dements, like the type of PDMS＇ s fiber -coating, extraction time and temperature, and some other elements were investigated. Results The optimal conditions for HS - SPME is a 100 - μm PDMS - coated fiber and the aetone - aqua（0. 5 -2） solvent combine with 0. 5 g sodium chloride, the extraction time and sample temperature established were 40 min and 95 ℃, repectively; select DB -608 as GC column, the column temperature was hdd at 160℃ for 1 min, then programmed at 10℃/min to 260℃ and held for 34 min finally. Conclusion this preprocess method is simple and fast,low solvent consumption, being the method of pesticide resi- dues in Chinese medicinal herb has a broad application prospect.
出处
《湖北中医药大学学报》
2012年第3期35-37,共3页
Journal of Hubei University of Chinese Medicine
基金
湖北省教育厅科研基金资助重点项目(D20716004)
国家中医药行业科研专项(201007012)
