CN105319307A - Analytic method of detecting monosaccharide composition in crocus sativus polysaccharide - Google Patents
Analytic method of detecting monosaccharide composition in crocus sativus polysaccharide Download PDFInfo
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- CN105319307A CN105319307A CN201410270426.9A CN201410270426A CN105319307A CN 105319307 A CN105319307 A CN 105319307A CN 201410270426 A CN201410270426 A CN 201410270426A CN 105319307 A CN105319307 A CN 105319307A
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Abstract
The invention relates to an analytic method of detecting monosaccharide composition in crocus sativus polysaccharide through ion chromatography method and belongs to the technical field of chromatography analysis. In the method, because of weak acidity and hydrophility of the saccharide compounds, the saccharide compounds exist in a strong alkaline solution in the form of negative ions, so that the strong alkaline solution can be used as a mobile phase to perform anion exchange separation. Meanwhile, reducibility of the saccharide compounds enables direct Ampere detection to be possible. The method solves the defects that a colorimetric method, a titration method and a gel chromatography method cannot separate and detect some specific monosaccharides, and at the same time, the method is also free of derivatization operations which are necessary in gas chromatography and capillary electrophoresis. The method detects the composition of the crocus sativus polysaccharide directly through the ion chromatography-pulsed amperometric detection and is simple and high-effective. In the method, the pulsed amperometric method is employed to detect the saccharide compounds, so that the method is high in sensitivity and selectivity and is suitable for detection of the saccharide compounds in a complex traditional Chinese medicine system.
Description
Technical field
The present invention relates to a kind of analytical approach utilizing the monose in ion-chromatographic determination west safflower polysaccharide to form, belong to technical field of chromatographic analysis.
Background technology
West safflower has another name called saffron, safflower, is the dry column cap of irides saffron, originates in the states such as Spain, Iran and India, introduces Tibet, be called safflower, commonly use so far through India.West safflower is a kind of very expensive medicinal material, has very high economic worth.Main containing compounds such as flavones, lignanoid, polyyne in west safflower, polysaccharide is also one of principle active component in west safflower.Polysaccharide is the macromolecular compound be formed by connecting by glycosidic bond by the monosaccharide groups of more than 10.Traditional idea thinks that polysaccharide physiologically active is not strong, extracts in preparation process usually removed as impurity by polysaccharide at Chinese herbal medicine.Since 20 century 70s, found that polysaccharide and polysaccharide compound participate in metabolism and the adjustment of cell life successively; there is the biological effect strengthening immunologic function, antitumor, anti-oxidant, anti-ageing, protection digestive system etc., the effects such as antibacterial, antiviral, hypoglycemic, reducing blood lipid in addition, radioresistance, anticoagulation.Therefore, develop west safflower polysaccharide to have important practical significance.
The assay method of current polysaccharide mainly contains colourimetry, titrimetry, high performance liquid chromatography, vapor-phase chromatography and high performance capillary electrophoresis.Colourimetry use with a long history, be widely used in determination of polysaccharide, particularly phend-sulphuric acid and a species of orchid ketone-sulfuric acid process most widely used.Film titrimetry is a kind of reductometry, is applied to the qualitative reaction of polysaccharide already, and rear development is used for determination of polysaccharide.External beginning since 20 century 70s applies the macromolecular organic compounds such as gel exclusion chromatography mensuration protein, and along with the appearance of high pressure resistant filler, efficient gel exclusion chromatography method is progressively applied on determination of polysaccharide.With other Measures compare, it is fast that high performance liquid chromatography has analysis speed, and the advantage of the aspects such as separation efficiency, selectivity, sensitivity height is a kind of method adopted that is worthy to be popularized.Gas chromatography determination polysaccharide increases its volatility by derivatization method, generally polysaccharide acid hydrolysis thing or Methanolysis is converted into hydrosilylation product or second phthalein product.High performance capillary electrophoresis is that the one developed in recent ten years is quick, efficient, easy, high resolving power and sample and solvent consumption few, the method for point analysis of variance bioactivator.The former analysis being mainly used in the macromolecular substances such as protein, polypeptide, nucleic acid of this law, and apply less in carbohydrate analysis.
Chromatography of ions, as the one of high performance liquid chromatography, is mainly used in analyzing ionic species, has been widely used in the fields such as environment, electric power, food, semiconductor, medicine chemical industry.In the last few years, along with the development of anion-exchange chromatography-Pulse amperometric detection method and constantly perfect, the analysis for sugar provided strong technical support.Novel organic polymer anion exchange Stationary liquid is stable in the scope of pH0 ~ 14; Saccharide compound has faintly acid and water wettability, exists in stronger alkaline solution with anionic form; Therefore can do mobile phase with strong alkali solution and carry out anion exchange separation.And the reductibility of saccharide compound provides possibility for directly carrying out ampere detection.The method of anion-exchange chromatography-pulsed amperometric method analysis sugar has been widely used in the aspects such as biochemistry, medical and health, food, beverage.Since nineteen ninety-five, the method having had multinomial employing chromatography of ions-pulsed amperometric method to measure saccharide compound in food is approved as International Standards Method by analyst association of the U.S. (AOAC).Up to now, have no directly with the analytical approach of monose composition in ion-chromatographic determination west safflower polysaccharide.
Summary of the invention
The present invention is pin improvements over the prior art just, the method for the monose composition providing a kind of chromatography of ions-Pulse amperometric detection method directly to measure west safflower polysaccharide.Concrete technical scheme of the present invention is as follows:
The present invention is the method that a kind of chromatography of ions-Pulse amperometric detection method measures the monose composition of west safflower polysaccharide, utilize the polysaccharide in water extraction and alcohol precipitation method extraction west safflower, after polysaccharide becomes monose after hydrolysis, utilize the faintly acid of sugar, water wettability and reductibility, directly utilize ion chromatograph-pulsed amperometric method to detect, thus measure kind and the content of monose.
Chromatography of ions of the present invention-Pulse amperometric detection method measures the method for the monose composition of west safflower polysaccharide, and do not need through complex operations such as derivatizations, method is simple and quick, and electrochemical detection method sensitivity and selectivity high.
The method that the monose that chromatography of ions of the present invention-Pulse amperometric detection method measures west safflower polysaccharide forms may be used for the monose component analysis of polysaccharide in a series of Chinese herbal medicine.
Tool of the present invention has the following advantages and effect:
1. the present invention utilizes saccharide compound to have faintly acid and water wettability, exists, therefore can do mobile phase with strong alkali solution and carry out anion exchange separation in stronger alkaline solution with anionic form; And the reductibility of saccharide compound provides possibility for directly carrying out ampere detection.This method solving colourimetry, titrimetry and exclusion chromatography can not the shortcoming of some specific monose of separation determination, do not need the derivatization operation carried out needed for gas chromatography and Capillary Electrophoresis simultaneously yet, direct employing chromatography of ions-pulsed amperometric method detects west safflower polysaccharide composition, method simple and effective.
2. the present invention adopts pulsed amperometric method to measure saccharide compound, and this detection method is highly sensitive, selectivity good, is applicable to the mensuration of traditional Chinese medicine complex system saccharide compound.
Accompanying drawing explanation
Fig. 1 is the standard colors spectrogram of 7 kinds of monose;
Fig. 2 is west safflower polysaccharide after hydrolysis, the chromatogram of simple monosaccharide composition;
Be labeled as in Fig. 1:
1-fucose, 2-rhamnose, 3-arabinose, 4-mannose, 5-glucose, 6-galactose, 7-fructose
Be labeled as in Fig. 2:
1-fucose, 2-rhamnose, 3-arabinose, 4-mannose, 5-glucose, 6-galactose, 7-fructose
Specific embodiments
Below in conjunction with Figure of description, the present invention is described in further detail:
Take west safflower 5.0g, after pulverizing, to spend the night degreasing with 8 times of 95% alcohol steep, filter, it is air-dry that residue puts shady and cool ventilation place.Filter residue adds 15 times of volume distilled water, extracting in boiling water 2h, filters, extracts twice, merge the extract obtained and be concentrated into 20mL, centrifugal, remove precipitation, under agitation slowly add 95% ethanol, 65% is reached, left undisturbed overnight to concentration of alcohol, centrifugal, obtain west safflower Thick many candies.Get 10mg Thick many candies and add 5ml2mol/L sulfuric acid solution in 25ml volumetric flask, in boiling water bath, be hydrolyzed 2h.Be neutralized to neutrality by adding barium carbonate in hydrolyzate, precipitation is removed in centrifugal filtration, and obtain hydrolyzate, after diluting 50 times, filtering membrane enters ion chromatography.Compound concentration is the mixed standard solution of the fucose of 1mg/L, rhamnose, arabinose, galactose, glucose, mannose, fructose 7 kinds of monose, enters ion chromatography.Chromatography of ions condition: chromatographic column: CarboPacPA10 (4 × 250mm) separating column+CarboPacPA10 (4 × 50mm) guard column; Leacheate forms: 15mMNaOH; Sampling volume: 25 μ L; Column temperature: 30 DEG C.Detection mode: Pulse amperometric detection method (gold electrode).
Fig. 1 is under above-mentioned chromatogram and testing conditions, the standard colors spectrogram (1mg/L) of 7 kinds of monose.
Fig. 2 is west safflower polysaccharide through extracting, after purifying and hydrolysis, under above-mentioned chromatogram and testing conditions, and the monose component color spectrogram of sample west safflower polysaccharide.
Claims (2)
1. one kind measures the analytical approach of the monose composition in west safflower polysaccharide, it is characterized in that utilizing saccharide compound to have faintly acid and water wettability, exist with anionic form in stronger alkaline solution, therefore can do mobile phase with strong alkali solution and carry out anion exchange separation; And the reductibility of saccharide compound provides possibility for directly carrying out ampere detection.This method solving colourimetry, titrimetry and exclusion chromatography can not the shortcoming of some specific monose of separation determination, do not need the derivatization operation carried out needed for gas chromatography and Capillary Electrophoresis simultaneously yet, direct employing chromatography of ions-pulsed amperometric method detects west safflower polysaccharide composition, method simple and effective.
2. the analytical approach of the monose composition in mensuration west safflower polysaccharide according to claim 1, it is characterized in that adopting pulsed amperometric method to measure saccharide compound, this detection method is highly sensitive, selectivity good, is applicable to the mensuration of traditional Chinese medicine complex system saccharide compound.
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Cited By (3)
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| CN106589152A (en) * | 2016-12-02 | 2017-04-26 | 伊犁师范学院 | Extraction process of Xinjiang Alatao crocus sativus corm polysaccharides |
| CN110346500A (en) * | 2018-04-04 | 2019-10-18 | 青岛大学附属医院 | A kind of anion-exchange chromatography based on acid hydrolysis of microwave-pulsed amperometric method detects the detection method of contents of monosaccharides in serum |
| CN112444567A (en) * | 2019-08-27 | 2021-03-05 | 江苏奥赛康药业有限公司 | Method for determining glucose and gluconic acid in oxidized dextrin |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106589152A (en) * | 2016-12-02 | 2017-04-26 | 伊犁师范学院 | Extraction process of Xinjiang Alatao crocus sativus corm polysaccharides |
| CN110346500A (en) * | 2018-04-04 | 2019-10-18 | 青岛大学附属医院 | A kind of anion-exchange chromatography based on acid hydrolysis of microwave-pulsed amperometric method detects the detection method of contents of monosaccharides in serum |
| CN110346500B (en) * | 2018-04-04 | 2021-11-30 | 青岛大学附属医院 | Detection method for detecting monosaccharide content in serum based on microwave acid hydrolysis and anion exchange chromatography-pulse amperometry |
| CN112444567A (en) * | 2019-08-27 | 2021-03-05 | 江苏奥赛康药业有限公司 | Method for determining glucose and gluconic acid in oxidized dextrin |
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Application publication date: 20160210 |