食品与发酵工业 >

2025 , Vol. 51 >Issue 15: 332 - 339

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.042499

分析与检测

超高效液相色谱-串联质谱法测定婴幼儿配方乳粉中磷脂含量

  • 梁敏慧 ,
  • 叶颖慧 ,
  • 施鹏斐 ,
  • 徐明轩 ,
  • 张晓敏 ,
  • 刘雪园 ,
  • 刘忠伟 ,
  • 刘玉洁 ,
  • 王思程 ,
  • 王雨蒙 ,
  • 刘汉霞
展开
  • (中国质量检验检测科学研究院,北京,100123)
第一作者:硕士,助理研究员(叶颖慧工程师和刘汉霞研究员为共同通信作者,E-mail:yeyinghui@caiqtest.com;liuhanxia@caiqtest.com)

收稿日期: 2025-02-24

  修回日期: 2025-03-21

  网络出版日期: 2025-08-22

基金资助

中国质量检验检测科学研究院基本科研业务费项目(2022JK23-S)

收起

Determination of phospholipids in infant formula milk powder by ultra-high performance liquid chromatography-tandem mass spectrometry

  • LIANG Minhui ,
  • YE Yinghui ,
  • SHI Pengfei ,
  • XU Mingxuan ,
  • ZHANG Xiaomin ,
  • LIU Xueyuan ,
  • LIU Zhongwei ,
  • LIU Yujie ,
  • WANG Sicheng ,
  • WANG Yumeng ,
  • LIU Hanxia
Expand
  • (Chinese Academy of Inspection and Quarantine,Beijing 100123, China)

Received date: 2025-02-24

  Revised date: 2025-03-21

  Online published: 2025-08-22

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摘要

为实现婴幼儿配方乳粉中6种磷脂化合物的快速精准测定,该研究建立了一种基于超高效液相色谱-串联质谱(ultra-performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)的分析方法。样品经水溶解后,采用二氯甲烷-甲醇(体积比2∶1)超声提取,以20 mmol/L甲酸铵水溶液和乙腈-异丙醇(体积比1∶1)溶液为流动相进行梯度洗脱,采用电喷雾正/负离子切换模式及多反应监测检测,外标法定量。结果表明,6种磷脂化合物在0.5~10 μg/mL范围内线性关系良好(r＞0.999);婴幼儿配方乳粉样品加标回收率为86%~107%,相对标准偏差为1.4%~9.0%;磷脂酰甘油、磷脂酰肌醇、磷脂酰乙醇胺的检出限和定量限分别为2.0 mg/100 g和6.0 mg/100 g,磷脂酰胆碱、磷脂酰丝氨酸(phosphatidylserine,PS)、鞘磷脂的检出限和定量限分别为10 mg/100 g和30 mg/100 g。实际样品分析显示,12种市售乳粉中磷脂总含量为80.7~566 mg/100 g,其中PS占比最高(30.4%~69.9%),且原料差异显著影响各组分含量。该方法具有灵敏度高、重现性好、分析结果准确的优势,可满足婴幼儿配方乳粉中磷脂含量的测定要求,为婴幼儿配方乳粉产品设计、质量控制及市场监管提供可靠技术支撑。

关键词： 磷脂; 超高效液相色谱-串联质谱法; 婴幼儿配方乳粉

本文引用格式

梁敏慧 , 叶颖慧 , 施鹏斐 , 徐明轩 , 张晓敏 , 刘雪园 , 刘忠伟 , 刘玉洁 , 王思程 , 王雨蒙 , 刘汉霞 . 超高效液相色谱-串联质谱法测定婴幼儿配方乳粉中磷脂含量[J]. 食品与发酵工业, 2025 , 51(15) : 332 -339 . DOI: 10.13995/j.cnki.11-1802/ts.042499

Abstract

To achieve a rapid and accurate determination of six phospholipid compounds in infant formula milk powder, this study established an analytical method based on ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).Samples were dissolved in water and subjected to ultrasonic extraction with dichloromethane-methanol (2∶1, volume ratio).Chromatic separation was achieved using gradient elution with 20 mmol/L ammonium formate aqueous solution and acetonitrile-isopropanol (1∶1, volume ratio) as mobile phases.Detection was carried out via electrospray ionization in positive and negative switching modes coupled with multiple reaction monitoring, and quantification was achieved using an external standard method.Results demonstrated excellent linear relationships (r>0.999) over a concentration range of 0.5-10 μg/mL for all six phospholipids.Spiking infant formula samples yielded recoveries ranging from 86% to 107% with relative standard deviations of 1.4%-9.0%.The detection limits and quantification limits for phosphatidylglycerol, phosphatidylinositol, and phosphatidylethanolamine were 2.0 mg/100 g and 6.0 mg/100 g, respectively, and 10 mg/100 g and 30 mg/100 g for phosphatidylcholine, phosphatidylserine (PS), and sphingomyelin, respectively.Analysis of 12 commercial samples revealed total phospholipid contents ranging from 80.7 mg/100 g to 566 mg/100 g, with PS constituting the highest proportion (30.4%-69.9%).Notably, raw material differences significantly affected the phospholipid concentrations.This highly sensitive, reproducible, and accurate method provides robust technical support for product formulation, quality control, and regulatory supervision of phospholipids in infant formula milk powder.

Key words： phospholipid; ultra-performance liquid chromatography-tandem mass spectrometry; infant formula milk powder

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