气相色谱-质谱法测定新鲜贝类中丙烯腈的残留量

目的建立新鲜贝类中丙烯腈残留量检测的气相色谱-质谱分析方法。方法样品经N,N-二甲基甲酰胺（DMF）超声提取,高速离心后,过0.45μm.有机相滤膜,气相色谱-质谱测定。选择VOCOL石英毛细管柱（60m×0.32 mm,1.8μm）分离,电子轰击离子源（EI）离子化,选择监测离子为m/z 53,m/z 52,m/z 51（其中定量离子为m/z 53）,外标法定量。结果丙烯腈在10-200 ng/m L浓度范围内呈良好的线性关系,相关系数r^2=0.9999;回收率为87.2%-96.1%,相对偏差RSD为4.4%-7.3%（n=6）;方法检出限为0.02 mg/kg,定量限为0.05 mg/...

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Bibliographic Details
Published in食品安全质量检测学报 Vol. 7; no. 6; pp. 2516 - 2522
Main Author 李玉玉 宋桂雪 赵永彪 宋薇
Format Journal Article
LanguageChinese
Published 谱尼测试集团股份有限公司,北京,100080 2016
Subjects
丙烯腈
气相色谱-质谱法
贝类
丙烯腈
shellfish
gas chromatography-mass spectrometry
气相色谱-质谱法
acrylonitrile
贝类
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ISSN2095-0381

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Summary:目的建立新鲜贝类中丙烯腈残留量检测的气相色谱-质谱分析方法。方法样品经N,N-二甲基甲酰胺（DMF）超声提取,高速离心后,过0.45μm.有机相滤膜,气相色谱-质谱测定。选择VOCOL石英毛细管柱（60m×0.32 mm,1.8μm）分离,电子轰击离子源（EI）离子化,选择监测离子为m/z 53,m/z 52,m/z 51（其中定量离子为m/z 53）,外标法定量。结果丙烯腈在10-200 ng/m L浓度范围内呈良好的线性关系,相关系数r^2=0.9999;回收率为87.2%-96.1%,相对偏差RSD为4.4%-7.3%（n=6）;方法检出限为0.02 mg/kg,定量限为0.05 mg/kg。结论本方法前处理简单,准确度及精密度高,在保证分析结果可靠的基础上大大的节省了检测时间及成本,可快速,准确地对新鲜贝类中丙烯腈的残留量进行分析。
Bibliography:LI Yu-Yu, SONG Gui-Xue, ZHAO Yong-Biao, SONG Wei （Pony Testing International Group Co., Ltd., Beijing 100080, China）
Objective To establish a method for determination of acrylonitrile residue in fresh shellfish by gas chromatography–mass spectrometry（GC-MS）. Methods Samples were determined by GC-MS after extraction by N,N- dimethyl formamide（DMF） combined with ultrasonic, high speed centrifugation and filtration by 0.45 μm organic phase membrane. Compounds were separated by VOCOL quartz capillary column（60 m×0.32 mm, 1.8 μm） and ionized by electron impact ionization source（EI）, selected ion monitoring（SIM） was used and the selected ions were m/z 53, m/z 52, m/z 51（m/z 53 was the quantitative ion）, with external standard method for quantitation. Results The acrylonitrile had a good linear relationship in the range of 10 -200 ng/m L, with the correlation coefficient r^2=0.9999. The recoveries were 87.2%-96.1%, relative standard deviations（RSDs） were 4.4%-7.3%（n=6）, the limit of detection of the method was 0.02 m
ISSN:2095-0381