摘要
文章对气相色谱法检测原生DHA牛乳中二十二碳六烯酸(Docosahexaenoic acid,DHA)方法进行优化。对GB 5009.168—2016《食品安全国家标准食品中脂肪酸的测定》内标法中脂肪抽提次数、旋转蒸发次数、检测药品等分别进行优化验证,并检测原生DHA牛乳中DHA含量。结果表明,经检测方法优化后,DHA可有效分离。样品分别加入2个浓度水平DHA后,加标回收率均在90.6%~104.9%之间,精密度试验中DHA含量的CV值均在0.9%~4.8%间,表明其重复性及准确性好。用氢氧化钾和正己烷代替三氟化硼、氢氧化钠、正庚烷、无水硫酸钠、氯化钠,加快反应过程,减少水浴时间,且避免有毒药品三氟化硼使用。该方法与国标法相比,检测结果基本一致,在准确性与精密度均得到保证的同时,样品前处理所用时间大幅度缩短,同时仪器检测分析时间缩短近15 min,有效解决了检测分析时间过长问题。优化后方法检测流程简单、快速、节约时间和成本,且准确性与精密度得到保证,适用于原生DHA牛乳中DHA含量大批量检测。
The method of detecting docosahexaenoic acid(DHA)in native DHA milk by gas chromatography was optimized.The times of fat extraction,times of rotary evaporation,detection drugs in GB 5009.168—2016 internal standard method were optimized and verified respectively,and the DHA content in native DHA milk was detected.The results demonstrated that after the optimization of detection method,DHA could be effectively separated.After the samples were added with two concentrations of DHA,the recovery rates were all between 90%and 110%,and the CV values of DHA content in precision experiments were all between 0.9%and 4.8%,which showed that the repeatability and accuracy were good.Potassium hydroxide and n-hexane were used instead of boron trifluoride,sodium hydroxide,n-heptane,anhydrous sodium sulfate and sodium chloride to speed up the reaction process,reduce water bath time and avoid the use of toxic drugs of boron trifluoride.The detection results of this method were basically consistent with the national standard method.At the same time,the accuracy and precision were guaranteed,the time of sample pretreatment was greatly shortened,and the time of instrument detection and analysis was shortened by nearly 15 min,which effectively solved the problem of long detection and analysis time.The optimized method is simple,rapid,time-saving and cost-saving,and its accuracy and precision are guaranteed.It is suitable for large-scale detection of DHA content in native DHA milk.
作者
李慧
王俊燕
胡娅洁
姚国新
孙学通
孟克达来
张鹏飞
张昊
LI Hui;WANG Junyan;HU Yajie;YAO Guoxin;SUN Xuetong;MENG Kedalai;ZHANG Pengfei;ZHANG Hao(Inner Mongolia Mengniu Dairy(Group)Co.Ltd.,Hohhot 011500,China;Inner Mongolia Mengniu High-Tech Dairy,Co.Ltd.,Hohhot 011500,China)
出处
《中国乳品工业》
北大核心
2025年第8期65-71,共7页
China Dairy Industry
基金
国家重点研发计划项目(2022YFD1301005)。
关键词
气相色谱法
内标法
二十二碳六烯酸
牛乳
检测
分析
gas chromatography
internal standard method
docosahexaenoic acid
milk detection
analyse
作者简介
李慧(1981年—),女,高级工程师,研究方向为食品加工及检验自动化。E-mail:lihui2@mengniu.cn。
