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

引用本文: 解鸿蕾, 李春, 刘宁. 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[J]. 色谱, 2013, 31(8): 781-785. doi: 10.3724/SP.J.1123.2012.12051 shu

Citation: XIE Honglei, LI Chun, LIU Ning. Analysis of sialic acid in infant formulas using ultra performance liquid chromatography-triple quadrupole mass spectrometry[J]. Chinese Journal of Chromatography, 2013, 31(8): 781-785. doi: 10.3724/SP.J.1123.2012.12051 shu

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,
,}

通讯作者: 李春,刘宁; 李春,刘宁

基金项目:
"十二五"国家科技支撑课题(2011BAD09B0304). (2011BAD09B0304)

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:

English

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

XIE Honglei ^1,2, ,
LI Chun ^{1,
,} ,
LIU Ning ^{1,2,
,}

1.
1. College of Food Sciences, Northeast Agricultural University, Key Laboratory of Dairy Science, Ministry of Education, Harbin 150030, China;

Corresponding author: 李春,刘宁; 李春,刘宁

Received Date: 28 December 2012
Fund Project:
"十二五"国家科技支撑课题(2011BAD09B0304).

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 UPLC^TM 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:

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

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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

通讯作者: 李春,刘宁; 李春,刘宁

English

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

Corresponding author: 李春,刘宁; 李春,刘宁

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中国化学会秘书处

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

通讯作者: 李春,刘宁; 李春,刘宁

English

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

Corresponding author: 李春,刘宁; 李春,刘宁

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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