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固相萃取-高效液相色谱法同时测定食用菌中多菌灵和噻菌灵残留量
          
Simultaneous Determination of Residual Amounts of Thiabendazole and Carbendazim in Edible Fungus by HPLC with Solid Phase Extraction

摘    要
食用菌样品经乙酸乙酯提取、氮气吹干,0.05 mol·L-1盐酸溶解后,经固相萃取小柱净化用液相色谱法测定.测定中采用Waters Symmetry C18色谱柱为固定相以及磷酸盐缓冲溶液和乙腈(75+25)混合溶液作为流动相.用二极管阵列紫外检测器于288 nm波长处进行紫外检测,外标法定量.方法的检出限(3S/N)和测定下限(10S/N)依次为0.010 mg·L-1和0.025 mg·L-1.在4个不同的浓度水平对方法的回收率进行了试验,测得结果在72.0%~86.0%之间.测定值的相对标准偏差(n=6)均小于8.5%.
标    签 高效液相色谱法   固相萃取   多菌灵   噻菌灵   食用菌   HPLC   Solid phase extraction   Carbendazim   Thiabendazole   Edible fungus  
 
Abstract
Residual amounts of thiabendazole (TBD) and carbendazim (CBD) were extracted ulltrasonically with ethylacetate from samples of edible fungus.The extract was evaporated to dryness by N2-blowing and the residue was dissolved in 0.05 mol·L-1 HCl.TBD and CBD in dil.HCl solution was then purified by SPE.The Waters Symmetry C18 column was used as stationary phase and a mixture of phosphate buffer solution and acetonitrile (mixed in the ratio of 75+25 by volume) was used as mobile phase.UV-detection was made using diode array detector at the wavelength of 288 nm,and external standard were used for quantification.Limit of detection (3S/N) and lower limit of determination (10S/N) of the methd were found to be 0.010 mg·L-1 and 0.025 mg·L-1 respectively for both bactericides.Tests for recovery and precision were made at 4 different concentration levels,and values of recovery found were in the range of 72.0%-86.0% with values of RSD′s (n=6) less than 8.5%.

中图分类号 O657.32

 
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收稿日期 2008/4/9

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备注陈练洪(1980-),女,福建漳州人,硕士研究生,主要从事进出口食品农产品检验.

引用该论文: CHEN Lian-hong,WANG Deng-fei,YOU Jun,HUANG Zhi-hui,ZHENG Jun-chao,WANG Rui-long. Simultaneous Determination of Residual Amounts of Thiabendazole and Carbendazim in Edible Fungus by HPLC with Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(8): 982~984
陈练洪,王登飞,游俊,黄智辉,郑俊超,王瑞龙. 固相萃取-高效液相色谱法同时测定食用菌中多菌灵和噻菌灵残留量[J]. 理化检验-化学分册, 2009, 45(8): 982~984


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参考文献
【1】唐月新.现行有效国内外食品中农兽药残留限量标准实用手册[M].北京:中国科学技术出版社,2005.
 
【2】SN/T 1753-2006进出口浓缩果汁中噻菌灵、多菌灵残留量检测方法 高效液相色谱法[S].
 
【3】SN 0220-1993出口水果中多菌灵残留量检验方法[S].
 
【4】SN 0606-1996出口乳及乳制品中噻菌灵残留量检验方法 荧光分光光度法[S].
 
【5】刘晓松,童张法,郑玲,等.浓缩刺梨汁中噻菌灵和多菌灵残留量的高效液相色谱法测定[J].分析测试技术与仪器,2006,12(3):131-135.
 
【6】胡彦学,杨秀敏,王志,等.固相微萃取-高效液相色谱-荧光检测法测定番茄中的多菌灵和噻菌灵[J].色谱,2005,23(6):581-584.
 
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【9】KONSTANTINOS P,DIMITRIS P,ALEXANDRA S,et al.Determination of carbendazim,thiabendazole,and o-phenylphenol residues in lemons by HPLC following sample clean-up by ion-pairing[J].Analytical and Bioanalytical Chemistry,2004,379(3):458-463.
 
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