A gas chromatography detection method for xylobiose

A gas chromatography and detection method technology, which is applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of great influence on the life of the chromatographic column, unsatisfactory quantitative effect, long analysis time, etc. Quick response and good specificity

Active Publication Date: 2015-09-02
XIAMEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The first two methods are qualitative methods, the quantitative effect is not ideal, and it is difficult to detect if it is lower than the mg level
High performance liquid chromatography is the most common method for quantitative analysis of xylobiose, but when there are many sugar components in the sample, its separation effect is often poor, the detection sensitivity is poor, the reproducibility is not good, and the analysis time is long and consumes There are many mobile phases, and the natural sugar components often have many impurities, which have a great impact on the life of the chromatographic column
The derivatization method combined with gas chromatography is a common method for the analysis of monosaccharides, which has the advantages of high speed and high sensitivity, but it has not been reported for the analysis of xylobiose

Method used

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  • A gas chromatography detection method for xylobiose
  • A gas chromatography detection method for xylobiose
  • A gas chromatography detection method for xylobiose

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Experimental program
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Embodiment 1

[0043] The analysis of xylobiose in the unknown sample of embodiment 1

[0044] Take 10 mg of xylooligosaccharide sample containing xylobiose, 10 mg of ribitol internal standard, add 50 mg of NaBH 4 Mix well with 2mL deionized water and react for 2h, add acetic acid dropwise until no bubbles are generated, add 5mL methanol, concentrate to dryness under reduced pressure at 60°C, add 1mL acetic anhydride and 1mL pyridine, mix well, react at 100°C for 1h, then add 1mL acetic acid The derivatized product was extracted with ethyl ester and washed with 1 mL of water. The prepared standard samples were used for gas chromatographic analysis, and their components were analyzed by GC-MS. Finally, with the help of analysis software, a calibration curve of xylobiose was obtained, which was used for quantitative analysis of xylobiose in the sample. Equipment Shimadzu GCMS-QP2010 gas chromatography-mass spectrometer, TCD detector temperature is 270°C, sampler temperature is 280°C, BP-15 c...

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Abstract

The invention discloses a method for detecting gas chromatogram of xylobiose and relates to xylobiose. The method comprises the following steps: adding NaBH4 and deionized water to a xylobiose-containing xylooligosaccharide sample and ribitol interior label, performing reaction, adding acetic acid until air bubbles are not generated, adding methanol, performing vacuum concentration until the mixture is dried, adding acetic anhydride and pyridine, continuing to react, adding ethyl acetate for extracting a derived product, and washing to obtain a standard sample to be used for gas chromatography; setting operating conditions of the instrument, wherein the temperature of a gas chromatographic column is 150-400 DEG C, the flow velocity of a mobile phase is 0.1-10.0mL.min<-1>, the temperature of a detector is 150-400 DEG C; performing sample introduction on a solution to be detected into an injection hole, detecting and recording a chromatogram, and analyzing the components by using a gas chromatograph-mass spectrometer; and acquiring a xylobiose calibration curve by means of analysis software, performing quantitative analysis on xylobiose in the sample, and judging the content of the xylobiose according to a ratio of peak elution area of a xylobiose peak to area of an internal standard peak.

Description

technical field [0001] The invention relates to xylobiose, in particular to a gas chromatography detection method for xylobiose. Background technique [0002] Xylooligosaccharide is a non-digestible oligosaccharide, which is an oligosaccharide composed of 2 to 7 D-xylose combined with β-1,4-xylosidic bonds. It is a new generation of functional oligosaccharide product. Xylo-oligosaccharides have excellent stability, can maintain stability in a wide range of pH and temperature, can selectively proliferate bifidobacteria in the intestinal tract, and can promote the growth of bifidobacteria and improve intestinal function. Its sweetness is lower than that of sucrose and glucose, only 40% of that of sucrose, and it has anti-caries properties. Its unique physiological activity and good physical and chemical properties make xylooligosaccharides considered to be one of the most promising and most widely studied functional oligosaccharides at home and abroad. Xylobiose is the main...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 刘健龙敏南甘礼惠
Owner XIAMEN UNIV
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