气相色谱法检测乳制品中二十二碳六烯酸方法的改进  

Improvement of gas chromatography method for determination of docosahexaenoic acid in dairy products

作　　者：韩荣 赵清华 张琳 张鹏飞 图雅 方向斌 周慧 许桂秋 HAN Rong;ZHAO Qinghua;ZHANG Lin;ZHANG Pengfei;TU Ya;FANG Xiangbin;ZHOU Hui;XU Guiqiu(Mengniu Dairy Industry(Dengkou Bayan gol)LIimited Liability Company,Bayannur Inner Mongolia,015200,China;Inner Mongolia Mengniu High-Tech Dairy Co.,Ltd.)

机构地区：[1]蒙牛乳业磴口巴彦高勒有限责任公司,内蒙古巴彦淖尔015200 [2]内蒙古蒙牛高科乳业有限公司

出　　处：《质量安全与检验检测》2024年第5期26-30,共5页QUALITY SAFETY INSPECTION AND TESTING

摘　　要：对GB 5009.168—2016《食品安全国家标准食品中脂肪酸的测定》第一法内标法的操作细节进行改进,建立检测乳制品中二十二碳六烯酸(docosahexaenoic acid,DHA)项目的分析方法。改进的方法采用在毛氏抽脂瓶中进行脂肪的水解、提取,减少了传统加热回流装置以及分液漏斗的使用。并且将仪器条件中氮气、氢气、空气的流量调整为25、30、400 mL/min,升温程序中初始温度调整为100℃,并调节加热速率。结果显示,DHA标准溶液在10~2000μg/mL浓度内呈良好的线性关系,相关系数R2为0.9994,方法的检出限为0.03 mg/100 g,定量限为1.3 mg/100 g。样品分别加入低、中、高3个浓度水平的DHA标准,检测加标回收率在87.3%~105.9%范围内,相对标准偏差(RSD)在3.65%~4.80%范围内。对婴幼儿配方乳粉质控样中的DHA进行测定,测定结果均在其标识范围内。改进后的方法简便、快速、准确性高,适用于乳制品中DHA的大批量检测。The operation details of the first internal standard method of GB 5009.168-2016"Determination of Fatty Acids in Food under the National Standard for Food Safety"were improved,and the analytical method for the detection of docosahexaenoicacid(DHA)in dairy products was established.The improved method is to hydrolyze and extract the fat in the Maurer bottle,which reduces the use of traditional heating reflux device and liquid separation funnel.In addition,the flow rate of nitrogen,hydrogen and air in the instrument conditions is adjusted to 25,30 and 400 mL/min,the initial temperature is adjusted to 100℃in the heating program,and the heating rate is adjusted.The results showed that DHA standard solution showed a good linear relationship in the concentration of 10-2000μg/mL,the correlation coefficient R2 was 0.9994,the detection limit of the method was 0.03 mg/100 g,and the quantification was 1.3 mg/100 g.The samples were added with low,medium and high concentrations of DHA.The recoveries were in the range of 87.3%-105.9%,and the relative standard deviations(RSD)were in the range of 3.65%-4.80%.DHA in the quality control sample of infant formula milk powder was determined,and the results were all within the labeled range.The improved method is simple,rapid and accurate,and is suitable for the detection of DHA in dairy products in large quantities.

关 键 词：脂肪酸 二十二碳六稀酸 乳制品 气相色谱法 

分 类 号：O657.7[理学—分析化学]