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1、高效液相色譜法測(cè)定蔬菜中8種氨基甲酸酯類農(nóng)藥殘留現(xiàn)代食品科技ModernFoodScienceandTechnology2011,Vo1.27,No.7高效液相色譜法測(cè)定蔬菜中8種氨基甲酸酯類農(nóng)藥殘留邵金良,黎其萬,劉宏程,佴注,蘭珊珊,梅文泉,杜麗娟,樊建麟(云南省農(nóng)業(yè)科學(xué)院質(zhì)量標(biāo)準(zhǔn)與檢測(cè)技術(shù)研究所,云南昆明650223)摘要:建立了固相萃取.高效液相色譜柱后衍生熒光檢測(cè)蔬菜中涕滅威亞砜,涕滅威砜,滅多威,三羥基克百威,涕滅威,克百威,甲萘威及異丙威等8種氨基甲酸脂類農(nóng)藥殘留的分析方法.本文對(duì)測(cè)定氨基甲酸酯農(nóng)藥
2、殘留的分離條件,提取溶劑,洗脫溶劑,凈化材料和基質(zhì)效應(yīng)進(jìn)行了優(yōu)化試驗(yàn).結(jié)果顯示,8種氨基甲酸脂類農(nóng)藥在0.1—1.0mg,L的濃度范圍內(nèi)線性良好,線性相關(guān)系數(shù)為0.99943--4).99992,檢出限為0.008~0.01mg/kg之間.樣品經(jīng)乙腈提取,氨基小柱凈化,采用基質(zhì)加標(biāo),在0.1mgg添加水平的平均回收率為79.4119.0%,相對(duì)標(biāo)準(zhǔn)偏差2.5%～l1.5%;0.2mg/kg添加水平的平均回收率為81.2%～115.5%,相對(duì)標(biāo)準(zhǔn)偏差為2.8%8.1%.此方法可適用于大白菜,辣椒,茄子,番茄,菠菜,
3、苦瓜,結(jié)球甘藍(lán)和豇豆等樣品的氨基甲酸酯類農(nóng)藥殘留的分析測(cè)定.關(guān)鍵詞:高效液相色譜法;柱后衍生;氨基甲酸酯類農(nóng)藥;蔬菜文章篇號(hào):1673.9078(2011)7.856.860Determination0fEightCarbamatePesticidesinVegetablesbyHighPLiquidChromatographyertormanceLiquitl11romato~rap11rSHAOJin-Liang,LIQi-Wan,LIUHong-cheng,ER-Zhu,LANShan-shanMEIWen
4、-quan,DULi-juan,FANJian-lin(InstituteofAgricultureQualitystandards&TestingTechnique,YunnanAcademyofAgriculturalScience,Kunming,Yunnan650223,China)Abstract:AnewmethodforthesimultaneousdeterminationofeightcarbamatepesticidesinChinesecabbage,pepper,egg-plant
5、,tomato,Chinesespinach,bittergourd,cabbageandcowpeabyhighperformanceliquidchromatographywasdeveloped.Eightcarbamatepesticideswasextractedfromthesamplesbyacetonitrile,salted,purifiedwithLC—NH2columnanddeterminedbyhighperformanceliquidchmmat0graphyusingpost-col
6、umnderivatizationwithfluorescencedetector.TheproposedmethodsshowedagoodlinearitybetweenanalyticalsignalintherangeofO.1～1.0mg,Lwiththelinearcorrelationcoefficientsof0.99943~0.99992andlimitsofdetectionof0.008-0.01mg/kg.Theaveragerecoveriesobtainedfromsamplesspi
7、kedwi幽standardsatconcentrationlevel0.1megkgand0.2mg/kgwereintherangeof79.4%-119.O%and81.2%一l15.5%,respectively,withrelativestandarddeviationsof2.5%～l1.5%and2.8%～8.1%,respectively.Themethodwasaccurate,reliable,andCanbeusedfordeterminationcarbamatepesticidesinv
8、egetables.Keywords:highperformanceliquidchromatography;post—columnderivatization;carbamatepesticides;vegetables氨基甲酸酯是一種具有良好殺蟲效果,在我國(guó)使用量較大的廣譜性農(nóng)藥【I】.該類農(nóng)藥是以甲酸酯為前體化合物發(fā)展而來的農(nóng)藥,具有分解快,殘留期短,低毒,高效和選
