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食用菌中多菌灵残留的分散固相萃取/高效液相色谱法测定 被引量:17

Determination of Carbendazim Residue in Edible Fungus by HPLC Method with Dispersive Solid Phase Extraction
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摘要 建立了食用菌中多菌灵残留量的测定方法。采用乙腈提取样品,提取液经十八烷基硅烷(ODS)和乙二胺-N-丙基硅烷(PSA)吸附净化后,采用反相高效液相色谱-紫外可见检测器进行测定,外标法定量。色谱条件:色谱柱为Agilent Eclipse XDB C18柱(4.6 mm×150 mm,5μm,i.d.),流动相为甲醇-0.02 mol/L磷酸盐缓冲溶液(pH7.4)(体积比25∶75),流速1 mL/min,柱温30℃,检测波长282 nm。结果表明,多菌灵在0.05-10 mg/L质量浓度范围内线性良好,相关系数为0.999 9;方法的相对标准偏差(RSD)不大于3.4%,添加回收率为81%-98%;多菌灵在食用菌中的检出限(LOD)和定量下限(LOQ)分别为0.03、0.10mg/kg。该方法操作简单快速、准确度高,能够满足多菌灵残留限量标准的检测要求。 A method was developed for the determination of carbendazim residue in edible fungus by high performance liquid chromatography coupled with dispersive solid phase extraction.The sample was extracted with acetonitrile,and cleaned up by dispersive solid phase extraction using octadecylsilyl derivatized silica(ODS) and primary secondary amine(PSA) as the sorbent.Carbendazim was separated on an Agilent Eclipse XDB C18 column(150 mm×4.6 mm,5 μm,i.d.)at 30 ℃ by using methyl alcohol-0.02 mol/L phosphate buffered saline(pH 7.4)(25∶75,by volume) as mobile phase at a rate of 1 mL/min.The detection wavelength was set at 282 nm and the external standard method was used for quantitative analysis.The results showed that the linear range for carbendazim was in the range of 0.05-10 mg/L with a correlation coefficient of 0.999 9.The relative standard deviations were below 3.4%,and the recoveries of carbendazim in even mushroom and lentinus edodes were in the range of 81%-98%.The limit of detection(LOD) and limit of quantitation(LOQ) of carbendazim in edible fungus were 0.03 mg/kg and 0.10 mg/kg,respectively.The developed method was simple and rapid,and could meet the requirement for the determination of carbendazim residue in edible fungus.
出处 《分析测试学报》 CAS CSCD 北大核心 2010年第6期573-577,共5页 Journal of Instrumental Analysis
关键词 多菌灵 分散固相萃取 高效液相色谱 食用菌 carbendazim dispersive solid phase extraction HPLC edible fungus
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