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    气相色谱-质谱法同时测定菠菜中4种二缩甲酰亚胺类杀菌剂的残留量

    Simultaneous GC Determination of Residual Amounts of 4 Diformylimide Bactericides in Spinach

    • 摘要: 提出了气相色谱-质谱法同时测定菠菜中乙烯菌核利、乙菌利、腐霉利和异菌脲等4种二缩甲酰亚胺类杀菌剂残留量的方法。样品用丙酮-正己烷(1+4)混合溶剂提取,所得提取液用凝胶色谱进行净化。采用气相色谱分离后,选择离子监测模式下质谱法进行测定。乙烯菌核利、乙菌利、腐霉利和异菌脲的检出限(3S/N)分别为0.01,0.01,0.01,0.02 mg·kg-1。取菠菜空白样品在3个浓度水平上加入4种杀菌剂混合标准溶液后,按试验方法进行测定,所得回收率在78.1%~94.9%之间,相对标准偏差(n=6)在4.9%~12%之间。

       

      Abstract: A method for determination of residual amounts of 4 diformylimide bactericides, i.e. vinclozolin, chlorzolinate, procymidone and iprodione, in spinach by GC-MS was proposed. Samples were extracted with mixed solvent of ethyl acetate and n-hexane (1+4). The extract obtained was purified by gel permeation chromatography, and the eluates were taken for separation by GC and the contents of the 4 bactericides were determined by MS under select ion monitoring (SIM) mode. Values of detection limit (3S/N) found were 0.01 mg·kg-1 for vinclozolin, 0.01 mg·kg-1 for chlorzolinate, 0.01 mg·kg-1 for procymidone, and 0.02 mg·kg-1 for iprodione. Tests for recovery were made by addition of mixed standards to a blank spinach sample at 3 different concentration levels, values of recovery found were in the range of 78.1%-94.9%, with values of RSD′s (n=6) in the range of 4.9%-12%.

       

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