食品中二十二碳六烯酸和花生四烯酸检测方法优化  

Optimization of the Detection Method for Docosahexaenoic Acid and Arachidonic Acid in Food

作　　者：李飘然 罗黎明 杨子忠 谢萌 李亚军 冯雪萍 LI Piaoran;LUO Liming;YANG Zizhong;XIE Meng;LI Yajun;FENG Xueping(Hubei Provincial Key Laboratory of Yeast Function,Yichang Hubei 443003,China;Angel Nutritech Co.,Ltd.,Yichang Hubei 443003,China)

机构地区：[1]酵母功能湖北省重点实验室,湖北宜昌443003 [2]安琪纽特股份有限公司,湖北宜昌443003

出　　处：《食品与发酵科技》2023年第5期130-134,151,共6页Food and Fermentation Science & Technology

摘　　要：优化食品中测定二十二碳六烯酸和花生四烯酸含量的气相色谱分析方法。将样品用乙醇-水(1∶2,v/v)溶解,加入2%氢氧化钠-甲醇溶液,水浴1.5h。采用气相色谱法进行测定,以HP-88(100m×0.25mm,0.2μm)色谱柱作为分析柱,流速1.0mL/min,进样口温度270℃,检测器温度280℃,初始柱温140℃保持3min,以5℃/min升温至200℃保持6min,以2℃/min升温至240℃保持10min,并采用内标法进行定量分析。结果表明,经前处理优化甲酯化过程和调节升温程序,二十二碳六烯酸和花生四烯酸峰在50min内可完全有效分离,样品中二十二碳六烯酸和花生四烯酸的含量分别为13.3%和26.6%,其含量稳定性较好,加标回收率分别为94.9%~95.9%和96.3%~97.1%,精密度实验中二十二碳六烯酸和花生四烯酸含量的RSD分别为0.5%和0.3%,说明其重复性及准确性较好,与国家标准方法相比,其检测结果基本一致,在保证准确性好、精密度高的同时,处理过程及检测分析时间缩短近5h,有效解决了实验室前处理及色谱分析时间过长的问题。此方法操作简单,节约时间成本且准确性好、精密度高,适用于食品中二十二碳六烯酸和花生四烯酸含量测定。To optimize the gas chromatography method for determination of docosahexaenoic acid and arachidonic acid in food.The sample was dissolved in ethanol-water(1∶2,v/v),and added to 2%sodium hydroxide-methanol solution and water reflux 1.5 h.The analytical column was HP-88(100 m×0.25 mm,0.2μm)column with a flow rate of 1.0 mL/min by gas chromatography.The injection port temperature was 270℃,detector temperature was 280℃,and the column temperature was 140℃for 3 minutes,raise the temperature to 200℃at 5℃/min for 6 minutes,and raise the temperature to 240℃at 2℃/min for 10 minutes,and the internal standard method was used for quantitative analysis.The results showed that the docosahexaenoic acid and arachidonic acid peaks could be separated effectively within 50 minutes by optimizing the methyl esterification process and adjusting the temperature-rising process,the contents of docosahexaenoic acid and arachidonic acid in the samples were 13.3%and 26.6%,respectively.Its content stability is good,with recovery rates of 94.9%~95.9%and 96.3%~97.1%,respectively.The RSD of the docosahexaenoic acid and arachidonic acid contents in the precision test were 0.5%and 0.3%,respectively,indicating that the accuracy and repeatability were good,compared with the national standard method,its detection results are basically the same.While ensuring good accuracy and high precision,shorten processing and detection analysis time by nearly 5 hours,which effectively solves the problem of long laboratory pretreatment and chromatographic analysis time.The method is simple,time-saving,cost-effective and accurate,and is suitable for the determination of docosahexaenoic acid and arachidonic acid in food.

关 键 词：二十二碳六烯酸 花生四烯酸 甲酯化 食品 检测 

分 类 号：TS207.3[轻工技术与工程—食品科学]