微囊型脂肪粉油脂的常规甲酯化方法优化OA北大核心CSTPCD
Optimization on conventional methyl-esterification method of oils in microencapsulated fat powders
试验旨在优化微囊型脂肪粉油脂的甲酯化方法.采用酸解法和石油醚萃取法从试样中提取油脂,取50 mg油脂于耐压瓶中,加入2 mL 0.2 mol/L氢氧化钠-甲醇溶液在65 ℃条件下超声水浴,皂化完成后以酚酞指示,利用1 mol/L硫酸-甲醇溶液中和至酚酞无色,加入300 μL硫酸-甲醇溶液,70℃超声水浴5 min,加饱和氯化钠水溶液分离,利用异辛烷萃取脂肪酸甲酯无水硫酸钠除水,采用气相色谱-火焰离子化检测器(GC-FID)测定,考察方法的精密度、准确度、检测限和定量限.结果显示,优化后方法测定大豆油标准物质GBW(E)100120的各种脂肪酸结果与标准值一致,精密度相对标准偏差(RSD)为1.25%.实验室间的比对结果显示:该方法甲酯化率达95%,重复性误差限RSD为2.71%,再现性误差限RSD为4.86%;反式油酸/反式亚油酸的检测限和定量限分别为0.004%、0.011%.研究表明,试验所用方法具有高效、精准和环保的优点,可为油脂产业的发展和今后的标准修订提供参考.
The purpose of this experiment is to optimize the methyl-esterification method of microencapsulated fat powder oil.The oil extracted from the samples using acid hydrolysis and petroleum ether.Take 50 mg of the oil and place it in a pressure-resistant vial,then add 2 mL 0.2 mol/L sodium hydroxide-methanol solution and sonicate in a water bath at 65℃.After the saponification was complete,as indicated by phenolphthalein,neutralized with 1 mol/L sulfuric acid-methanol solution until the phenolphthalein is colorless.Then add another 300 μL of sulfuric acid-methanol solution and sonicate again in a water bath at 70 ℃ for 5 minutes.Add a saturated sodium chloride into aqueous solution to assist with phase separation,and extract with isooctane after a desiccating with anhydrous sodium sulfate.Determine the content using Gas Chromatography-Flame Ionization Detector(GC-FID),and evaluate the precision,accuracy,detection limit,and quantitation limit of the method.The results showed that the optimized method of fatty acids in soybean oil standard substance GBW(E)100120 determined by the optimized method were consistent with the standard values,and the precision RSD was 1.25%.The comparison results between laboratories showed that the methyl-esterification rate of this method was more than 95%,the repeatability error limit RSD was 2.71%,and the reproducibility error limit RSD was 4.86%.The limit of detection and limit of quantitation of trans-oleic acid/trans-linoleic acid were 0.004%and 0.011%,respectively.The study indicates that the methods used in the experiment are efficient,accurate,and environmentally friendly,which can provide references for the development of the oil industry and the revision of future standards.
孙丽华;王勇;丁为国;韩冬月;谭淑君;殷秋妙
广州优百特科技有限公司,广东广州 511370广东省农业科学院农业质量标准与监测技术研究所,广东广州 510640||农业农村部农产品质量安全检测与评价重点实验室(广州),广东广州 510640
畜牧业
微囊型脂肪粉脂肪酸甲酯化气相色谱-火焰离子化检测器
microencapsulated fat powderfatty acidmethyl-esterificationGC-FID
《饲料研究》 2024 (017)
133-137 / 5
广东省企业科技特派员项目(项目编号:GDKTP2020064600);广东省农产品质量安全风险评估重点实验室项目(项目编号:2019B121203009)
评论