食品科学 ›› 2018, Vol. 39 ›› Issue (4): 138-143.doi: 10.7506/spkx1002-6630-201804021

• 成分分析 • 上一篇    下一篇

超高效液相色谱-质谱法测定母乳中12 种低聚糖

陈新新1,2,芦晶1,刘鹭1,逄晓阳1,张书文1,李诚2,*,吕加平1,*   

  1. (1.中国农业科学院农产品加工研究所,北京 100193;2.四川农业大学食品学院,四川雅安 625014)
  • 出版日期:2018-02-25 发布日期:2018-02-02
  • 基金资助:
    国家自然科学基金青年科学基金项目(31401514);“十二五”国家科技支撑计划项目(2013BAD18B10); 现代农业产业技术体系北京市奶牛产业创新团队建设专项;公益性行业(农业)科研专项(201303085)

Determination of 12 Oligosaccharides in Human Milk by Ultra-Performance Liquid Chromatography-Mass Spectrometry

CHEN Xinxin1,2, LU Jing1, LIU Lu1, PANG Xiaoyang1, ZHANG Shuwen1, LI Cheng2,*, Lü Jiaping1,*   

  1. (1. Institute of Food Science and Technology, Chinese Academy of Agricultural Sciences, Beijing 100193, China; 2. College of Food Science, Sichuan Agricultural University, Ya’an 625014, China)
  • Online:2018-02-25 Published:2018-02-02

摘要: 建立母乳中12种低聚糖超高液相色谱-串联三重四极杆质谱的定性及定量测定方法。母乳样品脱脂除蛋白后经液相分离,通过质谱检测,最优梯度洗脱条件为:流动相A为10mmol/L的甲酸铵溶液,流动相B为乙腈;流速0.3mL/min;柱温50℃;0~10min,95%~75%B;10~15min,75%B;15~20min,75%~65%B;20~21min,65%~10%B;21~24min,10%B;24~25min,10%~95%B;25~35min,95%B。12种低聚糖标准品标准曲线在设定质量浓度范围内线性良好(R2>0.98),加标回收率在80.00%~120.00%之间,重复性和仪器精密度(均用相对标准偏差表示)均小于10%。

关键词: 低聚糖, 母乳, 超高效液相色谱-串联三重四极杆质谱

Abstract: A qualitative and quantitative method for the determination of 12 oligosaccharides in human milk was established. The conditions for gradient elution were set as follows: mobile phase A, 10 mmol/L ammonium formate solution; mobile phase B, acetonitrile; flow rate, 0.3 mL/min; and column temperature, 50 ℃. The gradient elution procedure was programmed as follows: 0–10 min, 95%–75% B; 10–15 min, 75% B; 15–20 min, 75%–65% B; 20–21 min, 65%–10% B; 21–24 min, 10% B, 24–25 min, 10%–95% B; and 25–35 min, 95% B. The results showed that the standard curves of 12 oligosaccharides had good linearity within the concentration range investigated (R2 > 0.98) and the recoveries were between 80.00% and 120.00%. The repeatability and instrumental precision (expressed as elative standard deviations) were less than 10%.

Key words: oligosaccharides, human milk, ultra-performance liquid chromatography tandem triple quadrupole mass spectrometry (UPLC-QQQ MS)

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