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作 者:刘柱 陈万勤 茅佩卿 丁宇琦 朱炳祺 周赛静 罗金文
机构地区:[1]浙江省食品药品检验研究院,浙江杭州310052
出 处:《安徽农业科学》2015年第21期274-276,279,共4页Journal of Anhui Agricultural Sciences
摘 要:[目的]建立同时检测水果、蔬菜中7种常用农药残留的基质分散固相萃取(MSPD)-高效液相色谱法(HPLC)分析方法。[方法]供试样品通过乙腈高速均质提取,经PSA和C18(2∶1)基质分散固相萃取快速净化,以C18柱进行HLPC紫外多波长检测。通过流动相、吸附剂种类和用量的选择,加标回收试验,建立和优化了MSPD-HPLC同时测定7种常用农药残留的方法。[结果]试验表明,7种常用农药在各浓度范围内呈良好的线性关系,且相关系数R均大于0.999;选取苹果、草莓、番茄、黄瓜4种具有代表性水果、蔬菜进行加标回收试验,回收率均大于80%,相对标准偏差(RSD)为5%以内,检出限(LOD,S/N=3)为0.01-0.06 mg/kg。[结论]研究表明,该MSPD-HPLC方法操作简单、快速、准确,可满足多种水果、蔬菜中7种常用农药残留同时检测的实际需要。[ Objective ] A method was developed for the simultaneous determination of seven commonly-used pesticides in fruits and vegetables by using matrix solid phase dispersion(MSPD)-high performance liquid chromatography (HPLC). [ Method] The samples were extracted with acetonitrile, cleaned up by primary secondary amine (PSA) and C18 (2:1 ) adsorbents with MSPD method, separated by C18 column via HPLC, analyzed by different UV wavelengths. Through the selection of mobile phase test, adsorbent selection test, adsorbent dosage test and recovery test, the method of MSPD-HPLC for the determination of seven commonly-used pesticides analysis was established and optimized. [ Result] The result show that the calibration curves of seven commonly-used pesticides were linear in each concentration ranges with correla- tion more than O. 999. The absolute recoveries of seven pesticides analytes from four common representative samples were more than 80%, with RSDs (n = 6) less than 5%. The limit of detection(LODs, SIN = 3 ) were 0. 01 -0. 06 mg/kg. [ Conclusion] The MSPD-HPLC method is simple, rapid, accurate, which can meet the demands of practical used for the simultaneous determination of multi-residue pesticides in fruits and vegetables.
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