Method for detection of maltopentaose by ultra-high performance liquid chromatography-mass spectrometry

An ultra-high-efficiency liquid phase, maltopentasaccharide technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of high boiling point of carbohydrates, qualitative and quantitative interference, actual analysis errors, etc., to achieve weak ultraviolet color, Qualitative precision, high accuracy effect

Active Publication Date: 2018-11-02
SHANGHAI BAINIAN SHIDANDE INSPECTION TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the characteristics of high boiling point, difficult volatilization, and difficult gasification of sugar substances, it must be detected through one or two derivatization reactions, which will bring errors and inconvenience to the actual analysis.
Wu Hongjing and others used high performance liquid chromatography-differential refractive index detector to qualitatively and quantify the components of maltooligosaccharides. Although the method is simple, it needs to use time window method and standard sample plus sample overlapping method to analyze the six components in the sample. Qualitative analysis of various sugars, and maltopentaose presents double peaks, poor linear fit, too high detection limit, low sensitivity, and interference with given and quantified

Method used

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  • Method for detection of maltopentaose by ultra-high performance liquid chromatography-mass spectrometry
  • Method for detection of maltopentaose by ultra-high performance liquid chromatography-mass spectrometry
  • Method for detection of maltopentaose by ultra-high performance liquid chromatography-mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Chromatographic conditions: Agilent1290; Chromatographic column: Waters Xbridge BEH Amide (2.1x100mm), PartNo.: 186006091; Mobile phase: Acetonitrile-water gradient elution, 0-15min 87% acetonitrile, 15-20min 87% acetonitrile-15% acetonitrile, 20-30min 15% acetonitrile; flow rate: 0.4mL / min; column temperature: 40°C; injection volume: 0.5μL.

[0038] Mass spectrometry conditions: Agilent6460; ESI source, SIM mode, fragmentation voltage: 130v, sheath gas flow rate: 12L / min, capillary voltage: 4000v, extracted accurate mass number 827.4 ([M-H] - ), using the common logarithm of concentration and peak area for linear quantification.

[0039] Preparation of the test solution: Take 2.84mg of maltopentaose, accurately weighed, put in a 10mL volumetric flask, add water to dissolve and constant volume, shake well, accurately pipette 1mL, put in a 10mL volumetric flask, add water to dissolve and constant volume. Concentrate, shake well, and prepare maltopentaose mother liquor, ...

Embodiment 2

[0046] Chromatographic conditions: Agilent1290; Chromatographic column: Waters Xbridge BEH Amide (2.1x100mm), PartNo.: 186006091; Mobile phase: Acetonitrile-water gradient elution, 0-15min 87% acetonitrile, 15-20min 87% acetonitrile-15% acetonitrile, 20-30min 15% acetonitrile; flow rate: 0.4mL / min; column temperature: 40°C; injection volume: 0.5μL.

[0047] Mass spectrometry conditions: Agilent6460; ESI source, SIM mode, fragmentation voltage: 130v, sheath gas flow rate: 12 L / min, capillary voltage: 4000v, extracted accurate mass number 827.4 ([M-H] - ), using the common logarithm of concentration and peak area for linear quantification.

[0048] Preparation of the test solution: take 2.84 mg of maltopentaose, accurately weigh it, put it in a 10ml volumetric flask, add water to dissolve it and constant volume, shake well, pipette 1ml precisely, put it in a 10ml volumetric flask, add water to dissolve it and constant volume. Mix and shake well to prepare maltopentaose mother l...

Embodiment 3

[0054] Chromatographic conditions: Agilent1290; Chromatographic column: Waters Xbridge BEH Amide (2.1x100mm), PartNo.: 186006091; Mobile phase: Acetonitrile-water gradient elution, 0-15min 87% acetonitrile, 15-20min 87% acetonitrile-15% acetonitrile, 20-30min 15% acetonitrile; flow rate: 0.4mL / min; column temperature: 40°C; injection volume: 0.5μL.

[0055] Mass spectrometry conditions: Agilent6460; ESI source, SIM mode, fragmentation voltage: 130v, sheath gas flow rate: 12L / min, capillary voltage: 4000v, extracted accurate mass number 827.4 ([M-H] - ), using the common logarithm of concentration and peak area for linear quantification.

[0056] Preparation of the test solution: take 2.84 mg of maltopentaose, accurately weigh it, put it in a 10ml volumetric flask, add water to dissolve it and constant volume, shake well, pipette 1ml precisely, put it in a 10ml volumetric flask, add water to dissolve it and constant volume. Mix and shake well to prepare maltopentaose mother li...

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Abstract

The invention discloses a method for detection of maltopentaose by ultra-high performance liquid chromatography-mass spectrometry. The method includes the steps of: (1) taking an appropriate amount ofmaltopentaose, adding water for dissolving to prepare a test solution of certain solution; (2) performing sample introduction, and conducting detection according to the following chromatographic andmass spectrometric conditions that: according to the chromatographic conditions: Waters Xbridge BEH Amide 2.1*100mm is adopted as the chromatographic column, acetonitrile-water is used as the mobile phase for gradient elution, 87% acetonitrile can be maintained in 0-15min, and in 15-20min, 87% acetonitrile gradually decreases to 15% acetonitrile, and in 20-30min, 15% acetonitrile is maintained; according to the mass spectrometric conditions: an ESI source is taken, a selected ion monitoring (SIM) mode is used, the fragmentor is 130v, the sheath gas flow is 12L / min, the caplliary voltage is 4000v, the accurate mass number [M-H]<->827.4 is extracted, and the common logarithm of concentration and peak area is utilized for linear quantitation. The method has the characteristics of accurate qualitative analysis, high sensitivity, high precision, good linearity and simple operation, and is suitable for analysis and detection of maltopentose.

Description

technical field [0001] The invention relates to a method for detecting maltopentasaccharide by using ultra-high performance liquid chromatography-mass spectrometry technology, and belongs to the field of chemical analysis and detection. Background technique [0002] Maltopentaose is an oligosaccharide with low sweetness and has inhibitory effect on spoilage bacteria in the intestinal tract. It is widely used in food, cosmetics, medicine and other fields. Honey is the honey made by the Chinese bee Apis cerana Fabricius or the Italian bee Apis mellifera Linnaeus. In recent years, the situation of doping honey with various cheap fructose syrup and maltose syrup in natural honey is very serious. The starch-rich plants are used to produce hydrolyzed syrups such as fructose syrup through hydrolysis. There will be oligosaccharides with incomplete hydrolysis, such as maltopentaose and sugar compounds with higher molecular weight; and natural honey does not contain pentasaccharide...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88
Inventor 沈君子许纪锋张磊谢良山钱勇谢天培
Owner SHANGHAI BAINIAN SHIDANDE INSPECTION TECH
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