基质固相分散-气相色谱法测定桃中3种残留杀真菌剂
GC Determination of 3 Residual Fungicides in Peach with Matrix Solid Phase Dispersion of Sample
摘 要
采用基质固相分散进行样品前处理,并用n-己烷及二氯甲烷作淋洗液,从桃中提取五氯苯胺、甲基五氯苯基硫醚和腐霉利3种杀真菌剂,所得淋出液蒸发至近干,残渣溶于1 mL丙酮中供气相色谱分析,用毛细管色谱柱及电子捕获检测器进行测定.基质匹配标准校正方法补偿基质效应.添加0.01,0.05,0.10 mg·L-1杀真菌剂混合标准的回收率为82.6%~109.7%,相对标准偏差为3.3%~9.6%,检出限(3S/N)为0.1~0.4 μg·kg-1.
气相色谱
残留的杀真菌剂
桃
Matrix solid phase dispersion
Gas chromatography
Residual fungicides
Peach
Abstract
Three residual fungicides i.e.,pentachloroaniline,methyl pentachlorophenyl sulfide and procymidone,were separated from the peach sample by pretreatment with matrix solid phase dispersion,packing into a glass column and eluting with mixed solvent of n-hexane and dichloromethane.The eluate was evaporated to near dryness,and residue dissolved in 1 mL of acetone and used for GC-analysis.Capillary chromatographic column and electron capture detector were used in the GC-determination.Matrix matching method was used in preparation of calibration curve.Test for recovery was made at concentration levels of 0.01,0.05 and 0.10 mg·L-1 of the mixed standard solution of the fungicides,and values of recovery in the range of 82.6%-109.7% were obtained,with values of RSD′s (n=8) in the range of 3.3%-9.6%.Detection limits (3S/N) found were range from 0.1 to 0.4 μg·kg-1 for the 3 fungicides.
中图分类号 O657.7
所属栏目 工作简报
基金项目
收稿日期 2007/11/12
修改稿日期
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备注朱学良(1982-),男,河南鹿邑人,硕士研究生,主要从事食品安全、食品分析与食品化学、天然产物化学等方面的研究.
引用该论文: ZHU Xue-liang,QI Xiang-yang,LIU Chuan-ju,LI Hui-hui,LIU He-sheng,CAO Pin-bao,WANG Jing. GC Determination of 3 Residual Fungicides in Peach with Matrix Solid Phase Dispersion of Sample[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(1): 46～48
朱学良,戚向阳,刘传菊,李蕙蕙,刘合生,曹品豹,王静. 基质固相分散-气相色谱法测定桃中3种残留杀真菌剂[J]. 理化检验－化学分册, 2009, 45(1): 46～48
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参考文献
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【14】Zhu X L,Qi X Y,Wang J,et al.Determination of procymidone,pentachloroaniline and methyl-pentachloro-phenylsulfide residues in wine by MSPD-GC-ECD[J].Chromatographia,2007,65:625-628．
【15】黄宝勇.果蔬中农药多残留的气相色谱-质谱方法与基质效应的研究[D].北京:中国农业大学,2005．
【2】Jalbert J,Gilbert R,Tetreault P,et al.Matrix effects affecting the indirect calibration of the static headspace gas chromatographic method used for dissolved gas analysis in dielectric liquids[J].Anal Chem,2003,75(19):5230-5239．
【3】Hajslova J,Zrostlikowi J.Matrix efects in (ultra)trace analysis of pesticide residues in food and biotic matrices[J].J Chromatogr A,2003,1000(1):181-197．
【4】Egea G F J,Hernndez T M E,Almansa L E,et al.Matrix-effects of vegetable commodities in electron capture detection applied to pesticide multiresidue analysis[J].J Chromatogr A,2002,966(1):155-165．
【5】Martínez J L,Vidal F J,Arrebola A,et al.Validation of a gas chromatographic tandem mass spectrometric method for analysis of pesticide residues in six food commodities:Selection of a reference matrix for calibration[J].Chromatographia,2004,59:321-327．
【6】Schenck F J,Lehotay S J.Does further clean up reduce the matrix enhancement effect in gas chromatographic analysis of pesticide residues in food[J].J Chromatogr A,2000,868(1):51-61．
【7】Zrostlikova J,Hajslova J,Godula M,et al.Performance of programmed temperature vaporizer,pulsed splitless and on column injection techniques in analysis of pesticide residues in plant matrices[J].J Chromatogr A ,2001,937(1):73-86．
【8】Gonzalez C F,Otero R R,Grande B C,et al.Determination of fungicide residues in white grapes for winemaking by gas chromatography with mass spectrometric detection and assessment of matrix effects[J].J AOAC Int,2003,86(5):1008-1014．
【9】Albero B,Sanchez-brunete C,Tadeo J L.Analysis of pesticides in honey by solid phase extraction and gas chromatography mass spectrometry[J].J Agric Food Chem,2004,52(19):5828-5835．
【10】Anastassiades M,Mastovska K,Lehotay S J.Evaluation of analyte protectants to improve gas chromatographic analysis of pesticides[J].J Chromatogr A,2003,1015(1):163-184．
【11】Luis C R,Ana M G C,Eva A L,et al.Correction function on biased results due to matrix effects Application to the routine analysis of pesticide residues[J].Anal Chim Acta,2003,478:281-301．
【12】黄宝勇,潘灿,张微,等.应用分析保护剂补偿基质效应与气相色谱-质谱快速检测果蔬中农药多残留[J].分析测试学报,2006,25(3):11-16．
【13】朱学良,戚向阳,岳晶念,等.基质固相分散气相色谱电子捕获检测器测定葡萄酒中5种农药残留[J].分析化学,2007,35(2):259-263．
【14】Zhu X L,Qi X Y,Wang J,et al.Determination of procymidone,pentachloroaniline and methyl-pentachloro-phenylsulfide residues in wine by MSPD-GC-ECD[J].Chromatographia,2007,65:625-628．
【15】黄宝勇.果蔬中农药多残留的气相色谱-质谱方法与基质效应的研究[D].北京:中国农业大学,2005．
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