目的 建立一种Carb/NH2-SPE-GC-MS方法快速监测飞龙掌血根皮中4大类40种农药残留。方法 采用Carb/NH2固相萃取小柱同时处理4类农药样品,采用气相色谱-质谱联用法(GC-MS)进行40种农药残留痕量测定。结果 Carb/NH2-SPE-GC-MS法与《中国药典》收录的农药残留前处理方法比较,都不具有统计学差异(P>0.05),在处理飞龙掌血多种农药残留时更为简便可行。4大类40种农药在10～200 ng·mL-1内线性关系良好(r>0.998 2),检测限LODs均在2.5 ng·mL-1左右,40种农药的精密度、稳定性和加样回收率基本满足方法学考察要求。结论 本实验建立的Carb/NH2-SPE-GC-MS方法操作简单、快速、灵敏度高,能够对飞龙掌血药材中多组分农药残留进行准确的定性和定量分析。
Abstract
OBJECTIVE To establish a Carb/NH2-SPE-GC-MS method for rapid monitoring of 40 kinds of pesticides of four categories in Toddaliae asiaticae(L.) Lam. . METHODS The samples were pretreated with Carb/NH2 solid phase extraction (SPE) subpost, and a GC-MS method was used for the determination of the trace pesticide residues. RESULTS In comparison with the pesticide residue pretreatment METHODS included in the Chinese Pharmacopoeia, the Carb/NH2-SPE-GC-MS method showed no significant differences (P>0.05) and was simpler and more feasible in handling a variety of pesticide residues in Toddaliae asiaticae(L.) Lam. Good linearity was obtained for the calibration curves for the 40 kinds of pesticides in the concentration range of 10 to 200 ng穖L-1(r>0.998 2), the limits of detections (LODs) were around 2.5 ng穖L-1, and the precisions, stabilities and recoveries basically met the methodological requirements. CONCLUSION Carb/NH2-SPE-GC-MS method established in this paper is simple, rapid, highly sensitive, and accurate for the qualitative and quantitative analysis of multi-component pesticide residues in Toddaliae asiaticae(L.) Lam. .
关键词
固相萃取 /
气相色谱质谱联用方法 /
样品前处理 /
农药残留 /
飞龙掌血
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Key words
solid phase extraction (SPE) /
GC-MS /
sample pretreatment /
pesticide residue /
Toddaliae asiaticae(L.) Lam.
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中图分类号：
R917
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参考文献
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脚注
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基金
国家自然科学基金资助项目(81360681); 贵州省科学技术基金(黔科合J字2033号); 中组部“西部之光”访问学者基金(2014~2015)
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