三重四级杆气质联用仪多反应监测模式测定莜面中脂肪酸含量  

Determination of Fatty Acids in Oat Flour by MRM of GC/MS/MS

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作  者:张春萍 郭舒岗[1] 张蕤 熊慧霞 薛红波 杜兴 ZHANG Chun-ping;GUO Shu-gang;ZHANG Rui;XIONG Hui-xia;XUE Hong-bo;DU Xing(Shanxi Center for Disease Control and Prevention,Taiyuan,Shanxi 030000,China)

机构地区:[1]山西省疾病预防控制中心,山西太原030000

出  处:《粮油食品科技》2024年第3期170-178,共9页Science and Technology of Cereals,Oils and Foods

基  金:国家卫生健康委员会食物成分监测项目。

摘  要:采用三重四级杆气质联用仪(GC/MS/MS)多反应监测模式(multiple reaction monitoring,MRM)建立莜面中脂肪酸含量的分析方法。莜面样品和脂肪酸标准品经过氢氧化钾-甲醇和三氟化硼-甲醇溶液甲酯化15 min生成对应的脂肪酸甲酯。经DB-FastFAME(90 m×0.25 mm×0.25μm)色谱柱在电子轰击电离(EI)源下采用多反应监测模式进行扫描,外标法定量分析。40种脂肪酸甲酯在38 min内达到完全分离,脂肪酸甲酯化标准品在0.4~40μg/mL浓度范围内有良好的线性关系,相关系数R均达到0.9997。C20:2等6种脂肪酸定量限为0.003 g/100 g,其余34种脂肪酸定量限为0.0006 g/100 g。脂肪酸在3个浓度添加水平下的加标回收率为86.8%~107.3%,精密度在0.9%~5.2%之间。此法操作简便,选择性高,准确度、精密度、灵敏度好,适用于莜面中脂肪酸含量的快速、准确测定。Fatty acids in oat flour have been analyzed by using multiple reaction monitoring mode of gas chromatograph-mass spectrometer.The samples and fatty acid standards were methylated by potassium hydroxide-methanol and boron trifluoride-methanol solutions for 15 min to produce the corresponding fatty acid methyl ester.Then,the products would be separated through DB-FastFAME(90 m×0.25 mm×0.25μm)capillary column.Multiple reaction monitoring mode(MRM)was performed under electron bombardment ionization(EI)source,and the external standard method was carried out for quantitative analysis.40 kinds of fatty acid methyl esters could be completely separated within 38 min.A good linear relationship was achieved in the concentration range of 0.4~40μg/mL.The correlation coefficients of standard curve were all greater than 0.9997.The limit of quantification of 6 fatty acids such as C20:2 was 0.003 g/100 g,and the remaining 34 fatty acids was 0.0006 g/100 g.The standard recoveries of fatty acids were 86.6%~107.3%,and the precision was between 0.9%and 5.2%.It is a method for simple operate and high selectivity,which has a good accurate,precise and sensitive.The method is suitable for the rapid and accurate determination of fatty acids in oat flour.

关 键 词:莜面 三重四级杆气质联用仪 脂肪酸 多反应监测模式 

分 类 号:TS207.3[轻工技术与工程—食品科学] O657.63[轻工技术与工程—食品科学与工程]

 

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