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%.
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
所属栏目 工作简报
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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
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【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.
【7】YOUNG M S,EARLY M F,MALLET C R,et al.Application of a mixed-mode solid-phase extraction and cleanup procedure for LC/MS determination of thiabendazole and carbendazim in apple juice[J].Journal of AOAC International,2001,84(5):1615-1676.
【8】ATTILIO V,GIOVANNI V,SWIZLY A.Determination of carbendazim,thiabendazole and thiophanate-methyl in banana (Musa acuminata) samples imported to Italy[J].Food Chemistry,2004,87(3):383-386.
【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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