气相色谱-氢火焰离子化测定脂肪酸甲酯的响应机理与定量规律  

Determination of Fatty Acid Methyl Esters by Gas Chromatography-Flame Ionization Detection:Response Mechanism and Quantitative Pattern

作　　者：崔华玲 杨慧 孙丽华 叶倩 丁晨红 王威利 季天荣 马蕾 曾坤宏 殷秋妙 CUI Hualing;YANG Hui;SUN Lihua;YE Qian;DING Chenhong;WANG Weili;JI Tianrong;MA Lei;ZENG Kunhong;YIN Qiumiao(Institute of Quality Standard and Monitoring Technology for Agro-products of Guangdong Academy of Agricultural Sciences,Key Laboratory for Quality and Safety Testing and Evaluation of Agricultural Products,Ministry of Agriculture and Rural Affairs,Guangzhou 510640,China;Guangdong Provincial Planting Industry Standardization Technical Committee,Guangzhou 510640,China;Guangdong Association for Agricultural Standardization,Guangzhou 510640,China;Guangzhou UBT S&T Co.Ltd.,Guangzhou 511370,China)

机构地区：[1]广东省农业科学院农业质量标准与监测技术研究所,农业农村部农产品质量安全检测与评价重点实验室,广东广州510640 [2]广东省种植业标准化技术委员会,广东广州510640 [3]广东省农业标准化协会,广东广州510640 [4]广州优百特科技有限公司,广东广州511370

出　　处：《食品科学》2024年第13期49-57,共9页Food Science

基　　金：广东省企业科技特派员项目(GDKTP2020064600);广东省农产品质量安全风险评估重点实验室项目(2019B121203009)。

摘　　要：针对国内外现行标准中气相色谱-氢火焰离子化检测器(gas chromatography-flame ionization detector,GCFID)测定脂肪酸甲酯(fatty acid methyl esters,FAME)定量方法的不足,本实验通过理论推导和实验验证,从仪器、色谱柱、分流比、标准物质方面系统研究利用GC-FID分析37种FAME的响应规律、理论模型及实验干扰因素,提出“质量系数”和“关联因子”概念,揭示实验关联因子(experimental relevance factors,FF_(E))和理论关联因子(theoretical relevance factors,FF_(T))的函数关系和等值性条件,并经多个实验证实了关联因子的稳定性,发现当脂肪酸碳数大于10时,可充分利用理论质量系数(theoretical quality coefficient,QC_(T))和FFT对FAME进行相对或绝对定量;当脂肪酸碳数小于10时,可以通过现配FAME标准物质等方法精确测定实验质量系数(experimental quality coefficient,QC_(E))和实验关联因子FFE,并用此校正FAME的量进行定量,不仅能够提高定量结果的准确性,而且能够增加标准物质的使用时效以及节省标准物质的使用量。In light of the shortcomings of the quantitative methods for the determination of fatty acid methyl esters(FAME)using gas chromatography-flame ionization detection(GC-FID)specified by the current Chinese and international standards,this work systematically studied the response pattern,theoretical model,and experimental interfering factors in the GC-FID method for the determination of 37 FAME through theoretical derivation and laboratory validation from the perspectives of instruments,chromatographic columns,split ratio,and standard substances.Then,the concepts of“quality coefficient”and“correlation factor”were proposed to reveal the functional relationship and equivalence conditions between experimental relevance factors(FF_(E))and theoretical relevance factors(FF_(T)).Through multiple experiments,the stability of the correlation factors was confirmed.It was found that the theoretical quality coefficient(QC_(T))and the FFT could be fully utilized for relative or absolute quantification of FAME with more than 10 carbon atoms.The experimental quality coefficient(QC_(E))and FFE for FAME with less than 10 carbon atoms could be accurately measured through methods such as freshly preparing FAME reference materials and be used to correct the amount of FAME for quantitative analysis.This not only improved the accuracy of quantitative results,but also increased the timeliness of the use of reference materials and reduced the amount of reference materials used.

关 键 词：脂肪酸甲酯 甲酯化 气相色谱-氢火焰离子化检测 质量系数 关联因子 

分 类 号：TS207.3[轻工技术与工程—食品科学]