GC Determination of Residual Fenbutatin Oxide in Vegetable
摘 要
提出了气相色谱法、用火焰光度检测器测定蔬菜中苯丁锡的残留量.样品在酸性条件下经丙酮-乙酸(99+1)溶液和正己烷提取,提取物用乙基溴化镁乙醚溶液衍生,采用硅胶固相萃取柱净化,正己烷-二氯甲烷(4+1)混合液洗脱,氮气吹干后用正己烷定容至1 mL,用气相色谱测定,外标法定量.苯丁锡的质量浓度在0.2~2.0 mg·L-1范围内与其峰面积呈线性关系,检出限(3S/N)为0.1 mg·kg-1.以蔬菜阴性样品为基底,做加标回收试验,回收率为 76.9%~88.8%,相对标准偏差(n=6)为 3.46%~9.34%.
Abstract
Residual amount of fenbutatin oxide in vegetable sample was determined by GC with flame photometric detector (FPD).The sample was extracted by acetone-acetic acid (1+1) solution and n-hexane,and derivatized with ethyl magnesium bromide-diethyl ether solution.The derivatized product was purified and concentrated on silica column with n-hexane-dichloromethane mixture (4+1) as eluant.The eluate from column was evaporated by N2-blowing and made up to 1 mL,with n-hexane,which was used for GC analysis.External standard calibration was adopted in the determination.Linear relationship between values of peak area and mass concentration of fenbutatin oxide were obtained in the range of 0.2-2.0 mg·L-1,with detection limit (3S/N) of 0.1 mg·kg-1.Test for recovery was made by standard addition method,giving results in the range of 76.9%-88.8%.Values of RSD′s (n=6) found were in the range of 3.46%-9.34%.
中图分类号 O657.7
所属栏目 工作简报
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收稿日期 2009/4/17
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备注李德良(1966-),男,江西丰城人,实验师,学士,主要从事实验室设备管理及应用.
引用该论文: LI De-liang. GC Determination of Residual Fenbutatin Oxide in Vegetable[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(5): 518~520
李德良. 气相色谱法测定蔬菜中苯丁锡残留量[J]. 理化检验-化学分册, 2010, 46(5): 518~520
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