目的 建立一种超声波辅助萃取-固相微萃取-气相色谱(UAE-SPME-GC)快速检测金银花等13种贵州苗药中有机氯农药残留。方法 以金银花作为优化对象,样品经有机溶剂超声提取,直接固相微萃取富集, 气相色谱-电子捕获检测器进样检测。结果 在优化条件下, 8种有机氯农药在12.5~500 ng·g-1内线性关系良好,方法回收率在70.4%~119.8%之间,方法精密度在8.9%~14.1%之间,定性检测限在1.03~3.45 ng·g-1内。结论 实验表明超声波辅助萃取-固相微萃取-气相色谱法通过直接富集与进样,无需进行进一步的净化处理,大大减少了传统中药样品前处理的繁琐步骤。该方法是一种简便、环保、快速的分析中药材中有机氯农药残留的新方法。
Abstract
OBJECTIVE To establish a new gas chromatography method coupled with ultrasound-assisted extraction and solid-phase microextraction for rapid analysis of organochlorine pesticide residues (OCPs) in 13 Miao medicines in Guizhou. METHODS Flos Lonicerae Japonicae was used as an optimization object. Before being analyzed by GC, the sample was extracted by organic solvent and ultrasound, then enriched by SPME. RESULTS Under the optimized conditions, the linearities of eight kinds of OCPs ranged from 12.5 to 500 ng·g-1, all with good correlation coefficients. The spiked recoveries ranged from 70.4% to 119.8% and relative standard deviations (RSDs) ranged from 8.9% to 14.1%. The detection limits were 1.03-3.45 ng·g-1. CONCLUSION UAE-SPME-GC method simplifies the preparation steps for traditional Chinese medicines by direct sample enrichment and analysis thus sparing further purification. It is a convenient, environmentally-friendly and rapid method.
关键词
固相微萃取-气相色谱法 /
超声波 /
有机氯农药 /
苗药
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Key words
SPME-GC /
ultrasound-assisted extraction /
organochlorine pesticide /
Miao medicines
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中图分类号：
R284
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参考文献
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脚注
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基金
贵州省科学技术基金资助项目(黔科合J字[2013]2033号);贵州省中医药管理局基金资助项目(QZYY2013-90)
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