Analyzing method of sialic acid in infant milk powders with ultra-high performance liquid chromatography tandem quadrupole mass spectrometry

An ultra-high-efficiency liquid phase and series quadrupole technology, which is applied in the field of food testing, can solve the problems of sensitivity and accuracy that need to be further improved, and achieve the effect of high sensitivity and accuracy and improved accuracy

Active Publication Date: 2013-06-12
NORTHEAST AGRICULTURAL UNIVERSITY
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Problems solved by technology

Although this method can accurately determine the content of sialic a

Method used

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  • Analyzing method of sialic acid in infant milk powders with ultra-high performance liquid chromatography tandem quadrupole mass spectrometry
  • Analyzing method of sialic acid in infant milk powders with ultra-high performance liquid chromatography tandem quadrupole mass spectrometry
  • Analyzing method of sialic acid in infant milk powders with ultra-high performance liquid chromatography tandem quadrupole mass spectrometry

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Experimental program
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Embodiment 1

[0041] Determination of sialic acid content in infant milk powder of embodiment 1

[0042] method:

[0043] 1. Drawing of standard curve

[0044] Accurately pipette an appropriate amount of sialic acid standard stock solution, and dilute sequentially to obtain standard solutions with concentrations of 0.05, 0.1, 0.2, 0.5, 1.0 and 5.0 μg / mL. Carry out linear regression according to the peak area (Y) of the quantitative ion determination of sialic acid and the mass concentration (X, μ g / mL) of sialic acid, draw standard curve, the linear regression equation of sialic acid is:

[0045] Y=8514.5X-811.09, R 2 =0.9989

[0046] Wherein Y is the chromatographic peak area measured, and X is the mass concentration (μg / mL) of sialic acid, it is known that the linear relationship of this standard curve is good.

[0047] 2. Sample pretreatment

[0048] Take 1.0g each of 3 different brands of infant formula milk powder samples A1, B2, and C3, and extract the three forms of sialic acid ...

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Abstract

The ineveniton discloses an analyzing method of sialic acid in infant milk powders with an ultra-high performance liquid chromatography tandem quadrupole mass spectrometry method. On the basis of an original detecting of the sialic acid in milk powders with high performance liquid chromatography, the ultra-high performance liquid chromatography (UPLC) technology is combined, the sialic acid in three forms in a sample is extracted, and therefore the method of detecting the sialic acid in infant formula milk with the UPLC tandem mass spectrometry, wherein the method is higher in sensitivity and faster. According to the method, the average recovery of the sialic acid is within 84.3%-98.9%, the relative standard deviation (RSD) is 4.9%-8.2%, and the lowest detection limit of the sialic acid is 0.01 microgram/milliliter. The analyzing method of the sialic acid in infant milk powders with the UPLC tandem quadrupole mass spectrometry is simple and convenient to operate, a better separation mode is adopted, matrix effects are relatively small, the process of high-speed centrifugation after hydrolysis is adopted in pretreatment and simple, easy and convenient to operate, the loss of the sialic acid in a pretreatment process is effectively avoided, and the recovery rate is improved.

Description

technical field [0001] The invention relates to a method for analyzing sialic acid in infant milk powder, in particular to a method for analyzing sialic acid in infant milk powder by ultra-high performance liquid chromatography in series with quadrupole mass spectrometry, and belongs to the field of food detection. Background technique [0002] Sialic acid refers to a series of carboxylated monosaccharide acylated derivatives with nine carbon atoms, and its system name is 5-amino-3,5-dideoxy-D-glycerol-D-galactonanulose . It exists in free, oligosaccharide-bound and protein-bound forms in human milk and infant formula respectively. Human milk oligosaccharide-bound sialic acid accounts for about 73%, and infant formula milk protein-bound sialic acid accounts for about 70%. It is N-acetylneuraminic acid (Neu5Ac), so N-acetylneuraminic acid is often called sialic acid, and the content of sialic acid in milk and infant formula is very low. The latest report proves that sialic ...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 李春刘宁刘丽波解鸿蕾
Owner NORTHEAST AGRICULTURAL UNIVERSITY
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