固相萃取柱净化-气相色谱法定量测定食用植物油中饱和烃类矿物油

目的以自制硫酸硅胶和10%硝酸银硅胶填料分层装填的复合固相萃取柱为净化手段,建立一种测定食用植物油中饱和烃类矿物油的分析方法。方法样品经正己烷提取,固相萃取柱净化,氮吹浓缩,然后经DB-1石英毛细管色谱柱分离,采用气相色谱-火焰离子化检测器检测,外标法定量。结果考察了填料类型、填料用量、洗脱体积等因素对提取效率的影响。在优化的条件下,饱和烃类矿物油检测的线性范围为5.0～500.0mg/L,相关系数r～2=0.9991,方法检出限为3.0 mg/kg,定量限为10.0 mg/kg。样品在10.0、20.0、50.0 mg/kg 3个水平下的加标回收率为93.2%～103.7%,相对标准偏差为3...

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Published in食品安全质量检测学报 Vol. 8; no. 3; pp. 1041 - 1046
Main Author 杨春艳 郑涛 柯润辉 安红梅 田菲菲 尹建军 宋全厚
Format Journal Article
LanguageChinese
Published 中国食品发酵工业研究院,北京,100015%中钢设备有限公司,北京,100080%岛津(中国)有限公司,北京,100020 2017
Subjects
固相萃取
气相色谱
食用植物油
饱和烃类矿物油
食用植物油
饱和烃类矿物油
气相色谱
mineral oil saturated hydrocarbons
edible vegetable oil
solid phase extraction
固相萃取
gas chromatography
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ISSN2095-0381

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Summary:目的以自制硫酸硅胶和10%硝酸银硅胶填料分层装填的复合固相萃取柱为净化手段,建立一种测定食用植物油中饱和烃类矿物油的分析方法。方法样品经正己烷提取,固相萃取柱净化,氮吹浓缩,然后经DB-1石英毛细管色谱柱分离,采用气相色谱-火焰离子化检测器检测,外标法定量。结果考察了填料类型、填料用量、洗脱体积等因素对提取效率的影响。在优化的条件下,饱和烃类矿物油检测的线性范围为5.0～500.0mg/L,相关系数r～2=0.9991,方法检出限为3.0 mg/kg,定量限为10.0 mg/kg。样品在10.0、20.0、50.0 mg/kg 3个水平下的加标回收率为93.2%～103.7%,相对标准偏差为3.97%～5.33%（n=6）。结论该法操作简单、快速、准确度高,检出限能满足对食用植物油中饱和烃类矿物油残留的检测要求,且使用常规分析仪器、分析成本低,值得推广应用。
Bibliography:edible vegetable oil; mineral oil saturated hydrocarbons; solid phase extraction; gas chromatography
YANG Chun-Yan1, ZHENG Tao2, KE Run-Hui1 , AN Hong-Mei1, TIAN Fei-Fei3, YIN Jian-Jun1, SONG Quan-Hou1 （1. China National Research Institute of Food ＆ Fermentation Industries, Beijing 100015, China; 2. Sinosteel Engineering ＆ Technology Co., Ltd., Beijing 100080, China; 3. SHIMADZU （China） Co., Ltd., Beijing 100020, China）
11-5956/TS
Objective To establish a gas chromatographic method for the simultaneous determination of mineral oil saturated hydrocarbons in edible vegetable oils by packing sulfuric acid silica gel and 10% silver nitrate-silica gel separately,a homemade double solid phase extraction purification column.Methods The samples were extracted by hexane,purified with solid phase extraction column,then concentrated by nitrogen,separated by the capillary columns of DB-1,determined by a flame photometric detector and quantified by external standard method.Results The effects of influencing factors on extrac
ISSN:2095-0381