气相色谱-氢火焰离子化检测器测定婴幼儿乳粉中37种脂肪酸含量  

Determination of 37 Kinds of Fatty Acids in Infant Milk Powder by Gas Chromatography-Hydrogen Flame Ionization Detector

作　　者：罗叶丽 李国薇 董梅 赵璧 强鑫 LUO Yeli;LI Guowei;DONG Mei;ZHAO Bi;QIANG Xin(Weinan Inspection and Research Institute,Weinan 714000,China;Fuping County Inspection and Testing Center(Shaanxi Sheep Milk Product Quality Supervision and Inspection Center),Fuping 711700,China)

机构地区：[1]渭南市检验检测研究院,陕西渭南714000 [2]富平县检验检测中心(陕西省羊乳产品质量监督检验中心),陕西富平711700

出　　处：《食品工业科技》2023年第11期245-253,共9页Science and Technology of Food Industry

摘　　要：目的:建立气相色谱-氢火焰离子化检测器测定乳粉中37种脂肪酸含量的分析方法。方法:婴幼儿乳粉样品运用乙酰氯-甲醇法(10%乙酰氯甲醇溶液于80℃±1℃水浴2 h)甲酯化,离心取上清液过0.22μm的有机滤膜后经SP-2560(100 m×250μm×0.2μm)分离,气相色谱法检测,外标法定量。结果:37种脂肪酸甲酯在0.002~0.2 mg/mL浓度范围内线性良好,相关系数均大于0.999,回收率低梯度在85.5%~100.0%之间,中梯度在91.2%~104.2%之间,高梯度在86.8%~103.8%之间,精密度在0.88%~3.81%之间,实际样品测定结果符合相关标准要求。结论:该方法是在国标基础上建立了一种更为快速、分离度更好的脂肪酸检测技术,有很好的实用价值,方法稳定性好,成本低,重现性好,准确度高,适用于婴幼儿乳粉中37种脂肪酸含量的测定。Objective:To establish an analytical method for the determination of 37 kinds of fatty acid in milk powder by gas chromatography-hydrogen flame ionization detector(GC-FID).Methods:Infant milk powder samples were methylated by acetyl chloride-methanol method(10%acetyl chloride methanol solution in water bath at 80℃±1℃for 2 h).The supernatant was collected by centrifugation,passed through a 0.22μm organic filter membrane,and separated through SP-2560(100 m×250μm×0.2μm).Then,the detection was operated by gas chromatography,and the external standard method was used for quantification.Results:The linearity of 37 kinds of fatty acid methyl esters was good in the concentration range of 0.002~0.2 mg/mL,and the correlation coefficients were all greater than 0.999.The recovery rate fell in 85.5%~100.0%for the low gradient,91.2%~104.2%for the medium gradient,and 86.8%~103.8%for the high gradient.The precision was between 0.88%and 3.81%,and the actual sample determination results met the relevant standards.Conclusion:This method is a more rapid and better separation degree of fatty acid detection technology established on the basis of national standard,which has good practical value.The method has good stability,low cost,good reproducibility and high accuracy,and it is suitable for the determination of 37 kinds of fatty acid in infant milk powder.

关 键 词：脂肪酸 乙酰氯-甲醇法 气相色谱法 婴幼儿乳粉 

分 类 号：O657.71[理学—分析化学]