分散固相萃取-三重四极杆气相色谱质谱联用法测定糙米、小麦和玉米中2,4-滴丁酯残留  

Determination of 2,4-D Butylate Residue in Husked Rice,Wheat and Maize by Dispersive Solid Phase Extraction-Triple Quadrupole Gas Chromatograph Mass Spectrometer

作　　者：王枭鹏 许诗尧 WANG Xiaopeng;XU Shiyao(Hubei Cereals Oils and Food Stuffs Quality Supervision and Inspection Center,Wuhan 430000,China)

机构地区：[1]湖北省粮油食品质量监督检测中心,湖北武汉430000

出　　处：《食品安全导刊》2024年第14期96-100,105,共6页China Food Safety Magazine

摘　　要：建立了分散固相萃取-三重四极杆气相色谱质谱联用法测定糙米、小麦和玉米中2,4-滴丁酯残留的分析方法。试样经水和酸化乙腈提取后,经C_(18)、乙二胺-N-丙基甲硅烷(Primary Secondary Amine,PSA)和硫酸镁净化,吹干后用乙酸乙酯定容,用三重四极杆气相色谱质谱联用仪以多反应监测(Multiple Reaction Monitoring,MRM)模式分析,采用基质匹配标准曲线,内标法定量。经过对质谱参数、提取净化条件和基质效应的优化,2,4-滴丁酯在0.001~0.500 mg·L^(-1)浓度范围内线性关系良好,R^(2)大于0.999,方法检出限为0.001 mg·kg^(-1),定量限为0.005 mg·kg^(-1),在0.005 mg·kg^(-1)、0.050 mg·kg^(-1)和0.500 mg·kg^(-1)加标水平下的平均回收率为91.9%~108.0%,相对标准偏差(Relative Standard Deviation,RSD)在2.59%~6.35%(n=6)。本方法易于操作,灵敏度高,可有效测定糙米、小麦和玉米中2,4-滴丁酯残留。A method for the analysis of 2,4-D butylate residues in husked rice,wheat and maize was established by dispersive solid phase extraction-triple quadrupole gas chromatograph mass spectrometer.The samples were soaked in water,extracted with acidified acetonitrile,purified by C18,primary secondary amine and magnesium sulfate,dried by nitrogen and filled to specified volume with ethyl acetate,analyzed by triple quadrupole gas chromatograph mass spectrometer and multiple reaction monitoring mode,with matrix matched standard curve,and quantified by internal standard method.After optimizing the mass spectrometry parameters,extraction and purification conditions,and matrix effects,the linear relationship of 2,4-D butylate was good in the range of 0.001 mg·L^(-1) to 0.500 mg·L^(-1),and the R2 was greater than 0.999,the limit of detection of the method was 0.001 mg·kg^(-1),and the quantification limit was 0.005 mg·kg^(-1),the average recovery rate under the three spiked gradients of 0.005 mg·kg^(-1),0.050 mg·kg^(-1) and 0.500 mg·kg^(-1) was between 91.9%and 108.0%,and the relative standard deviation was between 2.59%and 6.35%(n=6).This method is simple and easy to perform and is highly sensitive,can effectively determine the 2,4-D butylate residues in husked rice,wheat and maize.

关 键 词：2 4-滴丁酯 分散固相萃取 三重四极杆气相色谱质谱联用仪 粮谷 

分 类 号：O657.63[理学—分析化学] TS210.7[理学—化学]