高效液相色谱法测定婴幼儿配方奶粉中1,3-二油酸-2-棕榈酸甘油三酯

doi:10.7506/spkx1002-6630-20230712-153

食品科学 ›› 2024, Vol. 45 ›› Issue (8): 265-271.doi: 10.7506/spkx1002-6630-20230712-153

高效液相色谱法测定婴幼儿配方奶粉中1,3-二油酸-2-棕榈酸甘油三酯

戴嵘德，刘峰，傅武胜，黄思婷，杨贵芝，刘文菁

（1.福建医科大学公共卫生学院，福建福州 350122；2.福建省疾病预防控制中心，福建福州 350012；3.宁夏疾病预防控制中心，宁夏银川 750000；4.福建中医药大学药学院，福建福州 350122；5.福建省产品质量检验研究院，福建福州 350002）

出版日期:2024-04-25 发布日期:2024-05-01
基金资助:
卫生部食品安全国家标准制定项目（spaq-2012-71）

Determination of 1,3-Dioleic acid-2-palmitoyl triglyceride in Infant Formula by High Performance Liquid Chromatography

DAI Rongde, LIU Feng, FU Wusheng, HUANG Siting, YANG Guizhi, LIU Wenjing

(1. School of Public Health, Fujian Medical University, Fuzhou 350122, China; 2. Fujian Provincial Center for Disease Control and Prevention, Fuzhou 350012, China; 3. Ningxia Center for Disease Control and Prevention, Yinchuan 750000, China; 4. School of Pharmacy, Fujian University of Traditional Chinese Medicine, Fuzhou 350122, China; 5. Fujian Inspection and Research Institute for Product Quality, Fuzhou 350002, China)

Online:2024-04-25 Published:2024-05-01

摘要/Abstract

摘要： 建立了婴幼儿配方乳粉中1,3-二油酸-2-棕榈酸甘油三酯（1,3-dioleyl-2-palmitoyl-glycerol，OPO）的检测方法。样品经氨水水解，用有机溶剂提取脂肪，氨基固相萃取柱净化，使用银离子色谱柱分离，以0.55%乙腈-正己烷为流动相洗脱，用高效液相色谱-蒸发光散射检测器检测。该方法实现了OPO和1,2-二油酸-3-棕榈酸甘油三酯的基线分离，可对OPO进行准确定性定量分析；方法在25～500 μg/mL质量浓度范围内线性关系良好，决定系数R2＝0.999 6，检出限和定量限分别为0.30、0.90 g/kg，加标含量为1～96 g/kg的范围内，OPO的平均回收率在97.1%～104.2%之间，相对标准偏差为1.2%～2.9%，精密度和正确度等方法学指标均符合要求；还通过了实验室间的协同性验证。调查分析了我国39 份市售OPO强化婴幼儿配方奶粉，OPO含量仅为标签标示量的28.4%～59.7%，这主要是因为检测方法不一致。

关键词: 高效液相色谱；1,3-二油酸-2-棕榈酸甘油三酯；婴幼儿配方奶粉

Abstract: A method for the quantification of 1,3-dioleyl-2-palmitoyl-glycerol (OPO) in infant formula was developed. The samples were treated with ammonia and extracted with organic solvents. The fat containing OPO was purified on a NH2 solid-phase extraction (SPE) cartridge packed with aminopropyl as the sorbent. The eluate was separated by silver ion chromatography using 0.55% acetonitrile-hexane as the mobile phase. The detection was carried out with a high performance liquid chromatography-evaporative light scattering detector (HPLC-ELSD). This novel procedure enabled the complete separation of OPO and its isomer 1,2-dioleyl-3-palmitoyl-glycerol (OOP), thus allowing for the accurate quantification of OPO. The developed method showed the desired linearity in the concentration range of 25–500 μg/mL with a determination coefficient (R2) of 0.999 6. The limits of detection (LOD) and limits of quantification (LOQ) were 0.30 and 0.90 g/kg, respectively. At spiked concentrations from 1 to 96 g/kg, the average recoveries of OPO varied from 97.1% to 104.2% with relative standard deviations (RSD) between 1.2% and 2.9%. The precision and accuracy of this method met the relevant requirements, and it passed the inter-laboratory collaborative validation. Our investigation analyzed 39 commercial samples of OPO-fortified infant formula in China, revealing that the measured OPO content only accounted for 28.4% to 59.7% of the labelled value, which is mainly due to the inconsistency of detection methods.

Key words: high performance liquid chromatography; 1,3-dioleic acid-2-palmitoyl triglyceride; infant formula

中图分类号:

TS252.7

戴嵘德，刘峰，傅武胜，黄思婷，杨贵芝，刘文菁. 高效液相色谱法测定婴幼儿配方奶粉中1,3-二油酸-2-棕榈酸甘油三酯[J]. 食品科学, 2024, 45(8): 265-271.

DAI Rongde, LIU Feng, FU Wusheng, HUANG Siting, YANG Guizhi, LIU Wenjing. Determination of 1,3-Dioleic acid-2-palmitoyl triglyceride in Infant Formula by High Performance Liquid Chromatography[J]. FOOD SCIENCE, 2024, 45(8): 265-271.

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高效液相色谱法测定婴幼儿配方奶粉中1,3-二油酸-2-棕榈酸甘油三酯

Determination of 1,3-Dioleic acid-2-palmitoyl triglyceride in Infant Formula by High Performance Liquid Chromatography

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