色谱

色谱 ›› 2013, Vol. 31 ›› Issue (8): 781-785.DOI: 10.3724/SP.J.1123.2012.12051

• 技术与应用 • 上一篇    下一篇

超高效液相色谱-串联四极杆质谱法分析婴儿乳粉中的唾液酸

解鸿蕾1,2, 李春1, 刘宁1,2   

  1. 1. 东北农业大学食品学院, 乳品科学教育部重点实验室, 黑龙江 哈尔滨 150030;
    2. 国家乳业工程技术研究中心, 黑龙江省乳品工业技术开发中心, 黑龙江 哈尔滨 150086
  • 收稿日期:2012-12-28 修回日期:2013-02-01 出版日期:2013-08-28 发布日期:2013-09-29
  • 通讯作者: 李春,刘宁
  • 基金资助:

    "十二五"国家科技支撑课题(2011BAD09B0304).

Analysis of sialic acid in infant formulas using ultra performance liquid chromatography-triple quadrupole mass spectrometry

XIE Honglei1,2, LI Chun1, LIU Ning1,2   

  1. 1. College of Food Sciences, Northeast Agricultural University, Key Laboratory of Dairy Science, Ministry of Education, Harbin 150030, China;
    2. National Dairy Engineering & Technical Research Center, Heilongjiang Dairy Industry Technical Development Center, Harbin 150086, China
  • Received:2012-12-28 Revised:2013-02-01 Online:2013-08-28 Published:2013-09-29
  • Contact: O658

PDF

333

被引次数

9

摘要：

建立了超高效液相色谱-串联质谱(UPLC-MS/MS)测定婴儿配方乳粉中唾液酸含量的分析方法。利用酸水解方法释放出婴儿配方乳中的唾液酸,经HLB反相色谱固相萃取柱净化,采用BEH HILIC色谱柱分离,以0.1%甲酸水溶液和100%乙腈溶液作为流动相进行梯度洗脱,流速为0.25 mL/min,进样体积5 μL,柱温30℃,电喷雾质谱检测,正离子多反应监测模式进行定性和定量分析。结果表明:唾液酸在0.05~5.0 mg/L范围内与唾液酸峰面积的线性关系良好(R2=0.9989);以0.1、0.5、2.5和5.0 mg/L 4个添加水平进行添加回收试验,唾液酸的平均回收率为84.3%~98.9%,相对标准偏差为4.9%~8.2%;唾液酸的检出限为0.01 mg/L。该方法简单、快速、重复性好、灵敏度高,可广泛用于奶粉、牛奶及母乳中唾液酸含量的分析测定。

关键词: 超高效液相色谱-串联质谱, 唾液酸, 婴儿配方乳

Abstract:

The method for analysing sialic acid in infant formulas by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) has been established. Sialic acid in milk was released via acid hydrolysis, and purified by an HLB solid phase extraction cartridge. The UPLC separation was performed on an ACQUITY UPLCTM BEH HILIC column (50 mm×2.1 mm, 1.7 μm) utilizing a gradient elution program of acetonitrile and water (containing 0.1% formic acid) as the mobile phases at a flow rate of 0.25 mL/min. Injection volume and column temperature were set at 5 μL and 30℃, respectively. The identification and quantification were achieved by using electrospray ionisation (ESI)-MS/MS in positive ion mode and multiple reaction monitoring (MRM) mode. The linear range was from 0.05 to 5.0 mg/L for sialic acid and the correlation coefficient (R2) was greater than 0.99. The average recoveries spiked at the four concentration levels of 0.1, 0.5, 2.5 and 5.0 mg/L ranged between 84.3% and 98.9% with the relative standard deviations from 4.9% to 8.2%. The limit of detection was 0.01 mg/L. Therefore, this method has the characteristics of simple operation, high reproducibility and sensitivity. It can be widely applied to determine the total contents of sialic acid in infant formula, cow milk and human milk.

Key words: infant formula, sialic acid, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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