中药材农药残留分析中的前处理方法比较  

Study the Pretreatment Method of the China Traditional Medicine in Pesticide Residue Analysis

作　　者：俞芳[1] 贾丽娟[1] 黄薇[1] 林诗云[1] 王红斌[1] 杨敏[1] 

机构地区：[1]云南民族大学化学与生物技术学院民族药资源化学国家民委-教育部重点实验室,昆明650500

出　　处：《农药》2014年第9期666-669,673,共5页Agrochemicals

基　　金：云南民族大学绿色化学与功能材料研究省创新团队项目(2011HC008);云南省高校绿色化学新能源与材料科技创新团队项目(2011UY09);2012年国家级大学生创新创业训练计划项目(201210691001);民族药资源化学国家民委-教育部重点实验室开放基金(MZY1121)

摘　　要：[目的]比较中药萝芙木中17种农药残留的2种前处理技术。[方法]样品经有机溶剂提取后,采用磺化法和固相萃取法进行净化,并采用GC-ECD进行检测,对前处理的提取条件和净化条件进行优化。[结果]石墨炭黑/氨基（CARBON/NH2）复合固相萃取小柱能够较好地去除杂质,磺化法不适用硫丹（含硫丹Ⅰ和硫丹Ⅱ）、狄氏剂和拟除虫菊酯类农药。[结论]采用CARBON/NH2复合固相萃取技术的方法平均回收率为75.11%~113.53%,相对标准偏差为0.34%~4.84%,适合中药萝芙木中17种农药残留的分析。[Aims] The sample preparation technique are compared in determination of 17 organic pesticide residues of Chinese traditional medicine （CTM） rauvolfia. [Methods] The sample was extracted by organic solvent, and purified by sulfonation and solid phase extraction （SPE）, and detected by GC-ECD, the extracting and purifying condition about pretreatment method were optimized. [Results] The Bond Elut Carbon/NH： （CARBON/NH2） mixed-mode SPE could remove impurity efficiently, and sulfonation was inapplicable to detection of pesticides endosulfan （include endosulfan I and endosulfan II ）, octalox, pyrethroids. [Conclusions] When samples were purified by CARBON/NH2, the average recoveries ranged from 75.11 to 113.53%, the relative standard deviations ranged from 0.34 to 4.84%, it could be used for 17 pesticides residues analysis in rauvolfia.

关 键 词：中药 萝芙木 农药残留 磺化法 固相萃取法 

分 类 号：R284.1[医药卫生—中药学] O652[医药卫生—中医学]