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Method for rapidly determining oligoguluronic acid by employing UPLC-Q-TOF/MS (ultra-high performance liquid chromatography-quadrupole rods tandem time-of-flight/mass spectrometry) technology

A technology of guluronic acid and guluronic acid disaccharide, which is applied in the detection field of oligomeric guluronic acid (G1-G4), which can solve complex steps, time-consuming, unsatisfactory rapid analysis and detection, etc. question

Inactive Publication Date: 2015-09-09
JIANGNAN UNIV
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Problems solved by technology

This method takes a long time and has complicated steps, which cannot meet the requirements of rapid analysis and detection

Method used

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  • Method for rapidly determining oligoguluronic acid by employing UPLC-Q-TOF/MS (ultra-high performance liquid chromatography-quadrupole rods tandem time-of-flight/mass spectrometry) technology
  • Method for rapidly determining oligoguluronic acid by employing UPLC-Q-TOF/MS (ultra-high performance liquid chromatography-quadrupole rods tandem time-of-flight/mass spectrometry) technology
  • Method for rapidly determining oligoguluronic acid by employing UPLC-Q-TOF/MS (ultra-high performance liquid chromatography-quadrupole rods tandem time-of-flight/mass spectrometry) technology

Examples

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Embodiment 1

[0017] Example 1 Detection of oligomeric guluronic acid in brown algae polysaccharide hydrolysate

[0018] 1. Standard samples: guluronic acid monosaccharide (G1), guluronic acid disaccharide (G2), guluronic acid triose (G3), guluronic acid tetraose (G4).

[0019] 2. Sample pretreatment: add 0.1g of fucoidan hydrolysate to 1mL of ultrapure water, vortex to mix and dissolve, pass through a 0.22 μm filter membrane at room temperature, to be tested.

[0020] 3. Chromatographic conditions: ACQUITY UPLC CSH C18 Column, 2.1 mm×100 mm, 1.7 μm, mobile phases are acetonitrile phase A and 0.1% formic acid phase B, flow gradient elution program: 0-1 min, 2% A+ 98 %B; 1-15 min, 2%A+98%B-60%A+40%B; 15-17 min, 60%A+40%B-100%A, flow rate 0.3 mL / min, column temperature : 45°C, injection volume 1 μL.

[0021] 4. Mass spectrometry conditions: WATERS MALDI SYNAPT-Q TOF / MS, electrospray ion source, negative ion scan mode. Ion source temperature 100℃, desolvent temperature 400℃, desolvent gas flow rate ...

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Abstract

The invention discloses a method for rapidly determining an oligoguluronic acid employing a UPLC-Q-TOF / MS (ultra-high performance liquid chromatography-quadrupole rods tandem time-of-flight / mass spectrometry) technology and belongs to the technical field of UPLC-Q-TOF / MS detection. The oligoguluronic acid is rapidly determined by the following steps: preparing a standard substance, pretreating a sample, and building a chromatographic condition, a mass spectrum condition and a qualitative and quantitative method for the oligoguluronic acid. The oligoguluronic acid is rapidly and accurately detected; and the characteristics of the oligoguluronic acid in parent ions and fragment ions in the mass spectrum are given, so that accurately qualitative and quantitative determination of a guluronic acid from monosaccharide to tetrasccharide in the sample can be realized; and meanwhile, the unknown oligoguluronic acid which is possibly contained in the sample can be speculated and analyzed according to the mass spectrum information.

Description

Technical field [0001] The present invention relates to a detection method of oligoguluronic acid (G1-G4), in particular to an ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC Q TOF / MS) combination technology. A rapid qualitative and quantitative method for rouronic acid belongs to the field of detection technology. Background technique [0002] The detection method of oligoguluronic acid related to the present invention can be used in the quality control of related medicines, health products and the like. Oligomeric guluronic acid is a hydrolysate of alginate. Studies have shown that sodium oligomeric alginate has the effects of lowering blood pressure, lowering blood lipids, anti-oxidation, anti-inflammatory, etc., and has been used in the treatment of cardiovascular diseases. There are few reports about the detection method of oligoguluronic acid. At present, it can be seen in the literature that the characterization of oligogulu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/60G01N30/72G01N30/34
Inventor 张爽陶冠军秦昉陈洁
Owner JIANGNAN UNIV
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