Carb/NH_2-SPE-GC-MS法快速监测飞龙掌血中4大类农药残留  

Rapid Determination of Four Categories of Pesticide Residues in Toddaliae asiaticae(L.) Lam. by Carb /NH_2-SPE-GC-MS

作　　者：梁金良 林野[2] 刘利亚[2] 周威[1] 何茂秋[1] 郝小燕[1] 

机构地区：[1]贵州医科大学药学院,贵阳550025 [2]贵州省疾病预防控制中心,贵阳550004

出　　处：《中国药学杂志》2015年第5期435-441,共7页Chinese Pharmaceutical Journal

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[2013]2033号);中组部"西部之光"访问学者基金(2014~2015)

摘　　要：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·m L-1内线性关系良好（r〉0.998 2）,检测限LODs均在2.5 ng·m L-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。OBJECTIVE To establish a Carb/NH2-SPE-GC-MS method for rapid monitoring of 40 kinds of pesticides of four cate- gories in Toddaliae asiaticae （L.） Lain.. 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 pes- ticide 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·mL-1 （r 〉0. 998 2）, the limits of detections （LODs） were around 2. 5 ng· mL-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.） Lain..

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 

分 类 号：R917[医药卫生—药物分析学]