固相萃取-气相色谱法定量分析橄榄油中饱和烃矿物油和芳香烃矿物油  

Off-line Solid Phase Extraction Combined with Gas Chromatography-Flame Ionization Detection Method for Determination of Mineral oil Saturated and Aromatic Hydrocarbons in Olive Oils

作　　者：柯润辉[1] 杨春艳[1] 胡雪 谢瑞龙 尹建军[1] 宋全厚[1] KE Run-Hui;YANG Chun-Yan;HU Xue;XIE Rui-Long;YIN Jian-Jun;SONG Quan-Hou(China National Research Institute of Food&Fermentation Industries,National Food Quality Supervision and Inspection Center,Beijing 100015,China;Inner Mongolia Yili Industrial Group Co.,Ltd.,Hohhot 010080,China)

机构地区：[1]中国食品发酵工业研究院,国家食品质量监督检验中心,北京100015 [2]内蒙古伊利实业集团股份有限公司,呼和浩特010080

出　　处：《分析化学》2018年第10期1677-1684,共8页Chinese Journal of Analytical Chemistry

摘　　要：建立了固相萃取(SPE)净化、程序升温进样结合气相色谱-氢火焰离子化检测器(PTV-GC-FID)定量分析橄榄油中饱和烃矿物油(MOSH)和芳香烃矿物油(MOAH)污染残留的方法。样品经正己烷溶解后,利用环氧化反应结合自制的分子筛SPE柱和0.3%AgNO_3硅胶SPE柱交替净化方式,消除了样品中脂质、蜡酯、烯烃、天然烷烃等干扰,并实现MOSH和MOAH的有效分离,氮吹浓缩后,经程序升温进样口大体积进样注入GC-FID分析,外标法定量。优化了环氧化试剂用量、环氧化反应时间、固相萃取洗脱体积等实验参数。结果表明,矿物油标准参考物Gravex 913润滑油在2.0~500.0 mg/L范围内呈良好线性关系,MOSH和MOAH的检出限分别为1.0和0.3 mg/kg,定量限分别为3.0和1.0 mg/kg,加标回收率分别为93.2%~103.7%和78.5%~81.3%,相对标准偏差分别为2.7%~5.0%和2.9%~4.0%。本方法净化效果好、试剂用量少、操作简单、检出限低,能有效分离植物油中MOSH和MOAH,适用于橄榄油中矿物油的定量检测。A method for quantitative analysis of mineral oil saturated hydrocarbons(MOSH)and aromatic hydrocarbons(MOAH)in olive oils by solid phase extraction(SPE)combined with programmed temperature vaporizer-gas chromatography-flame ionization detection(PTV-GC-FID)was established.The samples were dissolved in hexane,purified by the means of epoxidation combined with self-made molecular sieve SPE column and 0.3%silver nitrate silica SPE column alternating purification mode,in which way the interfering substances of lipids,wax esters,olefins and natural alkenes were removed,and the MOSH and MOAH fractions were effectively separated.The fractions were then concentrated by nitrogen,analyzed by the GC with large volume injection,separated by the capillary columns of DB-1,determined by a flame ionization detector,and quantified by external standard method.In addition,the key experimental parameters were optimized,including the amount of epoxidation reagent(mCPBA),epoxidation reaction time and elution volume.Under the optimized experimental conditions,Gravex913 lubricating oil showed good linearity as a standard reference of mineral oil in the ranges of 2.0-500.0 mg/L,the limits of detection(LOD)of MOSH and MOAH fractions were 0.3 mg/kg and 1.0 mg/kg,the limits of quantification(LOQ)were 1.0 mg/kg and 3.0 mg/kg,respectively.The spiked recoveries of MOSH and MOAH fractions were in the range of 93.2%-103.7%and 78.5%-81.3%at three spiked levels with the relative standard deviations(RSDs)of 2.7%-5.0%and 2.9%-4.0%(n=6).The established method has many advantages such as good purification effect,low reagent consumption and low detection limit,and is suitable for the separation and quantification of MOSH and MOAH in olive oils.

关 键 词：橄榄油 饱和烃矿物油 芳香烃矿物油 环氧化反应 固相萃取 程序升温大体积进样 

分 类 号：O657.71[理学—分析化学]