基于模拟实验建立改进的乙酰氯甲醇法测定特殊医学用途婴儿配方食品中的脂肪酸

doi:10.7506/spkx1002-6630-20230715-179

食品科学 ›› 2024, Vol. 45 ›› Issue (10): 194-200.doi: 10.7506/spkx1002-6630-20230715-179

基于模拟实验建立改进的乙酰氯甲醇法测定特殊医学用途婴儿配方食品中的脂肪酸

李洁，田其燕，刘艳明，王艳丽，李海霞，张卉，梁秀清，李芳芳，鞠香，王骏，胡梅

（山东省食品药品检验研究院，国家市场监管重点实验室（肉及肉制品监管技术），山东省特殊医学用途配方食品质量控制工程技术研究中心，产业技术基础公共服务平台，山东济南 250101）

出版日期:2024-05-25 发布日期:2024-06-08
基金资助:
山东省食品药品检验研究院发展类课题（SDIFDC-KY-4-2022002）

Establishment of an Improved Acetyl Chloride-Methanol Method for the Determination of Fatty Acids in Infant Foods for Special Medical Purpose Based on Simulation Experiments

LI Jie, TIAN Qiyan, LIU Yanming, WANG Yanli, LI Haixia, ZHANG Hui, LIANG Xiuqing, LI Fangfang, JU Xiang, WANG Jun, HU Mei

(Key Laboratory of Supervising Technology for Meat and Meat Products for State Market Regulation, Shandong Research Center of Engineering and Technology for Quality Control of Food for Special Medical Purposes, Industrial Technology Foundation Public Service Platform, Shandong Institute for Food and Drug Control, Jinan 250101, China)

Online:2024-05-25 Published:2024-06-08

摘要/Abstract

摘要： 针对氨基酸和乳蛋白深度水解特殊医学用途婴儿配方食品，建立改进的乙酰氯甲醇法，实现特殊医学用途婴儿配方食品中亚油酸、α-亚麻酸、二十二碳六烯酸（docosahexaenoic acid，DHA）和二十碳四烯酸（arachidonic acid，ARA）的快速、准确测定。结果表明，加入6 mL反应试剂、反应时间为60 min、萃取剂异辛烷为最优的前处理条件，亚油酸和α-亚麻酸的检测线性范围分别为0.8～8.0、0.2～2.0 mg/mL，DHA和ARA的检测线性范围均为0.02～0.40 mg/mL，决定系数均≥0.999 7，方法的检出限为2 mg/100 g，定量限为5 mg/100 g。方法的重复性好（相对标准偏差（relative standard deviation，RSD）≤3.3%）、精密度高（RSD≤3.8%）、稳定性好（RSD≤2.6%）、加标回收结果准确可靠（平均回收率93.1%～101.7%）。该方法有效解决了乙酰氯甲醇法在测定氨基酸和乳蛋白深度水解特殊医学用途婴儿配方食品时样品结块反应不彻底的问题，与传统方法相比，工作效率至少提高了100%。

关键词: 特殊医学用途；氨基酸配方；乳蛋白深度水解；模拟实验；脂肪酸

Abstract: An improved acetyl chloride-methanol method was established for the rapid and accurate determination of linoleic acid, α-linolenic acid, docosahexaenoic acid (DHA) and arachidonic acid (ARA) in infant foods for special medicinal purpose with deeply hydrolyzed milk proteins and amino acids. The results showed that the optimal pretreatment conditions were 6 mL of reaction reagent, reaction for 60 minutes, and use of isooctane as extraction solvent. The linear range of linolenic acid and α-linolenic acid were 0.8–8.0 and 0.2–2.0 mg/mL, respectively. The linear ranges of DHA and ARA were 0.02–0.40 mg/mL, and the determination coefficients for all analytes were greater than or equal to 0.999 7. The limits of detection (LOD) and limits of quantitation (LOQ) of the developed method were 2 and 5 mg/100 g, respectively. This method was characterized by good repeatability (relative standard deviation (RSD) ≤ 3.3%), high precision (RSD ≤ 3.8%), good stability (RSD ≤ 2.6%), and high spiked recovery (ranging from 93.1% to 101.7%). Compared with its original version, the developed method could effectively solve the problem of incomplete reaction due to caking, with an at least 100% higher working efficiency.

Key words: special medicinal purpose; amino acid formula; deep hydrolysis of milk protein; simulation experiments; fatty acids

中图分类号:

O657.7

李洁，田其燕，刘艳明，王艳丽，李海霞，张卉，梁秀清，李芳芳，鞠香，王骏，胡梅. 基于模拟实验建立改进的乙酰氯甲醇法测定特殊医学用途婴儿配方食品中的脂肪酸[J]. 食品科学, 2024, 45(10): 194-200.

LI Jie, TIAN Qiyan, LIU Yanming, WANG Yanli, LI Haixia, ZHANG Hui, LIANG Xiuqing, LI Fangfang, JU Xiang, WANG Jun, HU Mei. Establishment of an Improved Acetyl Chloride-Methanol Method for the Determination of Fatty Acids in Infant Foods for Special Medical Purpose Based on Simulation Experiments[J]. FOOD SCIENCE, 2024, 45(10): 194-200.

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基于模拟实验建立改进的乙酰氯甲醇法测定特殊医学用途婴儿配方食品中的脂肪酸

Establishment of an Improved Acetyl Chloride-Methanol Method for the Determination of Fatty Acids in Infant Foods for Special Medical Purpose Based on Simulation Experiments

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