摘要
考察了固相萃取-程序升温-气相色谱法(SPE-PTV-GC)与大容量固相萃取-气相色谱法(LS-SPE-GC)测定食用油脂中饱和烃矿物油(MOSH)污染物的差异。从前处理程序、仪器方法、方法学考察与实际样品测定几个方面比较了两种分析方法。结果表明:不同容量的SPE柱对样品净化程序不存在显著性差异(P>0.05);PTV-GC与普通GC在C12~C40碳数分布不存在显著性差异,PTV-GC在2.5~200 mg/kg范围内线性良好(R^2=0.9991),GC在12.5~500 mg/kg范围内线性良好(R^2=0.9994);两种方法测定6种食用油脂中MOSH的结果没有显著性差异,其回收率和RSD值均可以满足检测要求。其中SPE-PTV-GC灵敏度更高,适合低含量污染物的分析。
The investigation focused on direct comparison of two off-line mineral oil saturated hydrocarbons（MOSH） analytical methods： the solid phase extraction-programmed temperature vaporizer-gas chromatography（SPE-PTV-GC） and large scale solid phase extraction-ordinary gas chromatography（LS-SPE-GC）.In this work,the sample preparation procedures,instrumental analysis methods,method validation and determination of mineral oil saturated hydrocarbons（MOSH） in edible oils and fats samples were compared between the two analytical methods.Results： there was no significant difference（P 〉0.05） between the different scale SPE columns,and either no significant difference in the alkane distribution of the C12～ C40 range between the two methods.The PTV-GC instrument was linear in the concentration range of 2.5 ～ 200 mg/kg（R2= 0.9991）,and the common GC instrument was linear in the concentration range of 12.5 ～ 500 mg/kg（R^2= 0.9994）.There was no significant difference in actual samples detections between the two methods,and therecovery and RSD of the two methods could meet the detection requirements.SPE-PTV-GC method has a higher sensitivity and is more suitable for low-level contaminant analysis.
作者
李冰宁
刘玲玲
武彦文
LI Bing-ning;LIU Ling-ling;WU Yan-wen(Beijing Academy of Science and Technology, Beijing Center for Physical and Chemical Analysis, Beijing Food Safety Analysis and Testing Engineering Research Center, Key Laboratory of Analysis and Testing, Beijing Academy of Science and Technology, Beijing 100089)
出处
《分析试验室》
CAS
CSCD
北大核心
2018年第6期701-705,共5页
Chinese Journal of Analysis Laboratory
基金
北京市科技计划课题(Z161100000616005)
北京市科学技术研究院财政专项(PXM2018_178305_000005)
北京市科学技术研究院青年骨干计划(YC201805)项目资助
关键词
食用油脂
饱和烃矿物油(MOSH)
气相色谱
程序升温进样
固相萃取
Edible oil and fats
Mineral oil saturated hydrocarbons （MOSH）
Gas chromatography （GC）
Programmed temperature vaporizer（PTV）
Solid phase extraction（SPE）
