CN103698417B - Content detection method of D-sodium erythorbate - Google Patents
Content detection method of D-sodium erythorbate Download PDFInfo
- Publication number
- CN103698417B CN103698417B CN201310478788.2A CN201310478788A CN103698417B CN 103698417 B CN103698417 B CN 103698417B CN 201310478788 A CN201310478788 A CN 201310478788A CN 103698417 B CN103698417 B CN 103698417B
- Authority
- CN
- China
- Prior art keywords
- acid sodium
- content
- araboascorbic acid
- detection method
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The invention relates to a content detection method of D-sodium erythorbate. Octadecylsilane chemically bonded silica is used as chromatographic column filling material; potassium dihydrogen phosphate solution-methanol is used as mobile phase; an ultraviolet detector is used for detection. Chromatographic peaks of D-sodium erythorbate and other components in the tea beverage and other sample are baseline resolved symmetrical Gaussian peaks with good peak patterns, thereby satisfying qualitative and quantified requirements; According to the invention, the chromatogram condition has few damages to the used chromatographic column, so the chromatographic column life is longer and the detection cost is lower in normal usage condition; the detection method of the invention has the advantages of accuracy, simple operation, good reappearance, high sensitivity and good practicality in work.
Description
Technical field
The present invention relates to a kind of detection method of content of D-araboascorbic acid sodium.
Background technology
D-araboascorbic acid sodium, formal name used at school: D-2,3,5,6-tetrahydroxy-2-hexenoic acid-gamma lactone sodium salt, has another name called sodium isoascorbate, erythorbic acid sodium.Molecular formula is: C
6h
7naO
6h
2o.This product is white powder or particle, and odorless, slightly saline taste are soluble in water.
D-araboascorbic acid sodium, as a kind of antioxidant generally added in current beverage industry, plays color-protecting function to content.Because it is easily oxidized, in the storage process of beverage easily by the oxygen in bottom clearance in the dissolved oxygen DO in content, container or by packaging infiltration come in dioxygen oxidation and decay, when its content decays to a certain degree, its color-protecting function cannot be played, content will variable color, thus affects the sense organ of product.Therefore, in beverage, the initial addition of D-araboascorbic acid sodium must can ensure that product variable color does not occur during shelf life, and this initial addition rule need based on the grasp to the attenuation law of D-araboascorbic acid sodium in this product under specific condition of storage really.As can be seen here, in beverage, the foundation of D-araboascorbic acid sodium content assay method is particularly important.
The report that the method for current mensuration D-araboascorbic acid sodium is in the field of business is also fewer, Li Hong once reported the method with iodometric determination D-araboascorbic acid sodium effective content, cloth all can wait to be improved the method for iodometric determination D-araboascorbic acid sodium, the pertinent literature applying Modern Analytical Instrument mensuration is then more rare, only Kang Lidong reported and made separating column in order to C18 chromatographic column, measured the effective content of the D-araboascorbic acid sodium in beer using 0.05M potassium dihydrogen phosphate as mobile phase.And the mensuration of D-araboascorbic acid sodium does not have ripe national standard yet at present, only Department of Public Health of Jilin Province has issued the provincial standard of D-sodium isoascorbate assay method in food in Dec, 2012, adopt hydrophilic interaction power post to make separating column, acetonitrile-0.1% phosphate aqueous solution is made mobile phase and is measured.
Summary of the invention
Adopt the method for Kang Lidong report to measure the content of the D-araboascorbic acid sodium in tea beverage, find that D-araboascorbic acid sodium chromatographic peak is abnormal, fail to form symmetrical Gaussian peak, illustrate that this method is not suitable for the mensuration of D-araboascorbic acid sodium in tea beverage.And method involved by Jilin Province's provincial standard is comparatively large to the loss in mensuration process of adopted hydrophilic interaction power post, the chromatographic column life-span is shorter, and testing cost is higher.
The technical solution adopted for the present invention to solve the technical problems comprises the following steps:
(1) chromatographic condition: be the chromatographic column of filler with octadecylsilane chemically bonded silica; With potassium dihydrogen phosphate-methyl alcohol for mobile phase; Detect with UV-detector;
(2) preparation of testing sample solution: get testing sample 5-10g, is placed in 100mL volumetric flask, adds pure water and fully dissolves, and be diluted to scale, shake up, and filters, gets filtrate as testing sample solution;
(3) preparation of reference substance solution: separately get reference substance D-araboascorbic acid sodium 3mg, be placed in 100mL volumetric flask, add pure water and fully dissolve, and be diluted to scale, shake up, filters, product solution in contrast;
(4) content assaying method: draw testing sample solution and each 5 μ L ~ 10 μ L injection high performance liquid chromatographs of reference substance solution respectively, record chromatogram; By external standard method respectively with the content of D-araboascorbic acid sodium in calculated by peak area sample.
The detection method of content of D-araboascorbic acid sodium of the present invention, the mobile phase of step (1) chromatographic condition is 0.5%-0.8% by concentration, pH value is potassium dihydrogen phosphate and the methyl alcohol composition of 3-5, the volume ratio of two components is (85: 15)-(95:5), and the wavelength coverage that UV-detector detects is 240nm ~ 250nm.
The detection method of content of D-araboascorbic acid sodium of the present invention, have good linear relationship when the solution concentration of D-araboascorbic acid sodium is between 1mg/kg-200mg/kg, its linearly dependent coefficient reaches more than 0.9990, and the recovery is 106%-109%.
The present invention can be used for the content detection of D-araboascorbic acid sodium in various liquid beverage.
The present invention's good effect is compared with the prior art:
1. the present invention measures D-araboascorbic acid sodium gained chromatographic peak in the samples such as tea beverage and other component chromatogram peak energy reaches baseline separation, Gaussian peak symmetrically, and peak type is good, can meet quantitative and qualitative analysis requirement;
2. chromatographic condition involved in the present invention is less to the damage of adopted chromatographic column, and the normal use lower chromatographic column life-span is longer, and testing cost is lower;
3. detection method is accurate, easy and simple to handle, and favorable reproducibility is highly sensitive, practical at work.
Accompanying drawing explanation
Fig. 1 is the D-araboascorbic acid sodium 30mg/L reference substance chromatogram that the inventive method measures;
Embodiment
Below in conjunction with drawings and Examples, the present invention is further described.
Embodiment one:
1. chromatographic condition and system suitability:
Agilent 1260Infinity type high performance liquid chromatograph (Agilent company of the U.S.); Agilent diode array detector; Chromatographic column: PROSHELL120EC-C18(3.0 × 50mm2.7Micron); Mobile phase: concentration 0.8%, pH is the potassium dihydrogen phosphate-methyl alcohol of 4.0, two volume components are than being (80: 20);
2. the selection of determined wavelength
Precision takes D-araboascorbic acid sodium reference substance 3mg, is placed in 100mL volumetric flask, adds pure water and fully dissolve, and be diluted to scale, shake up, and filters, product solution in contrast.5 μ L injection liquid chromatographies are drawn by Agilent automatic sampler precision, must the chromatogram (accompanying drawing 1) of this composition and ultraviolet spectrogram by Agilent diode array detector.From chromatogram and ultraviolet spectrogram result, this component content measures determined wavelength and elects 240nm as.
3. the preparation of reference substance solution
Precision takes D-araboascorbic acid sodium reference substance 3mg, is placed in 100mL volumetric flask, adds pure water and fully dissolve, and be diluted to scale, shake up, and filters, product solution in contrast.
4. green tea D-araboascorbic acid sodium content measures solution preparation
Get green tea sample 10g to be measured, be placed in 100mL volumetric flask, add pure water and fully dissolve, and be diluted to scale, shake up, filter, get filtrate as need testing solution.
5. measure
Accurate absorption green tea testing sample solution and each 5 μ L of reference substance solution inject high performance liquid chromatographs, record chromatogram respectively; By external standard method respectively with the content of D-araboascorbic acid sodium in calculated by peak area sample, result is 21.191mg/L.
Embodiment two:
1. chromatographic condition and system suitability:
Agilent 1260Infinity type high performance liquid chromatograph (Agilent company of the U.S.); Agilent diode array detector; Chromatographic column: PROSHELL120EC-C18(3.0 × 50mm2.7Micron); Mobile phase: concentration 0.6%, pH is the potassium dihydrogen phosphate-methyl alcohol of 4.0, two volume components are than being (95: 5);
2. the selection of determined wavelength
Precision takes D-araboascorbic acid sodium reference substance 3mg, is placed in 100mL volumetric flask, adds pure water and fully dissolve, and be diluted to scale, shake up, and filters, product solution in contrast.5 μ L injection liquid chromatographies are drawn by Agilent automatic sampler precision, must the chromatogram (accompanying drawing 1) of this composition and ultraviolet spectrogram by Agilent diode array detector.From chromatogram and ultraviolet spectrogram result, this component content measures determined wavelength and elects 250nm as.
3. the preparation of reference substance solution
Precision takes D-araboascorbic acid sodium reference substance 3mg, is placed in 100mL volumetric flask, adds pure water and fully dissolve, and be diluted to scale, shake up, and filters, product solution in contrast.
4. green tea D-araboascorbic acid sodium content measures solution preparation
Get green tea sample 10g to be measured, be placed in 100mL volumetric flask, add pure water and fully dissolve, and be diluted to scale, shake up, filter, get filtrate as need testing solution.
5. measure
Accurate absorption green tea testing sample solution and each 5 μ L of reference substance solution inject high performance liquid chromatographs, record chromatogram respectively; By external standard method respectively with the content of D-araboascorbic acid sodium in calculated by peak area sample, result is 20.797mg/L.
By above-described embodiment, clearly describe technical scheme of the present invention, but above embodiment is only in order to illustrate the use of this patent, but not limitation ot it, any replacement based on invention spirit or change all should belong to the protection category of this patent.
Claims (2)
1. a detection method of content for D-araboascorbic acid sodium, is characterized in that described detection method comprises the following steps:
A, chromatographic condition: be the chromatographic column of filler with octadecylsilane chemically bonded silica; With potassium dihydrogen phosphate-methyl alcohol for mobile phase; Detect with UV-detector;
The preparation of b, testing sample solution: get testing sample 5 ~ 10g, is placed in 100mL volumetric flask, adds pure water and fully dissolves, and be diluted to scale, shake up, as testing sample solution;
C, reference substance solution: employing concentration is the D-araboascorbic acid sodium solution product solution in contrast of 30mg/L;
D, content assaying method: draw testing sample solution and each 5 μ L ~ 10 μ L injection high performance liquid chromatographs of reference substance solution respectively, record chromatogram; By external standard method respectively with the content of D-araboascorbic acid sodium in calculated by peak area sample;
The mobile phase of described step a chromatographic condition is made up of potassium dihydrogen phosphate and pure methyl alcohol, and both volume shares are potassium dihydrogen phosphate 80 ~ 98 parts by volume: methyl alcohol 2 ~ 20 parts by volume; The mass concentration of wherein said potassium dihydrogen phosphate is 0.5% ~ 0.8%, and pH value is 3 ~ 5.
2. the detection method of content of D-araboascorbic acid sodium according to claim 1, is characterized in that, the wavelength coverage that UV-detector detects is 240nm ~ 250nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310478788.2A CN103698417B (en) | 2013-10-14 | 2013-10-14 | Content detection method of D-sodium erythorbate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310478788.2A CN103698417B (en) | 2013-10-14 | 2013-10-14 | Content detection method of D-sodium erythorbate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103698417A CN103698417A (en) | 2014-04-02 |
| CN103698417B true CN103698417B (en) | 2015-04-08 |
Family
ID=50360016
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310478788.2A Active CN103698417B (en) | 2013-10-14 | 2013-10-14 | Content detection method of D-sodium erythorbate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103698417B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107664672B (en) * | 2017-09-19 | 2020-05-29 | 山东世通检测评价技术服务有限公司 | Method for synchronously measuring L-ascorbic acid, D-ascorbic acid and dehydroascorbic acid in milk powder |
| CN111380990A (en) * | 2018-12-27 | 2020-07-07 | 成都平和安康医药科技有限公司 | Method for detecting content of vitamin C and isovitamin C in vitamin C medicament |
| CN111337613B (en) * | 2020-04-18 | 2023-03-21 | 新拓洋生物工程有限公司 | High performance liquid detection method for D-isoascorbic acid potassium |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101216474A (en) * | 2008-01-16 | 2008-07-09 | 方南 | Long validity chloromycetin eyedrop detection method |
| CN102749394A (en) * | 2012-06-06 | 2012-10-24 | 南京农业大学 | Separation and measurement method for reduction-type ascorbic acid and erythorbic acid in fruit and vegetable tissues and related products |
-
2013
- 2013-10-14 CN CN201310478788.2A patent/CN103698417B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN103698417A (en) | 2014-04-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107966514B (en) | Method for detecting content of sanshoamides in pepper extract | |
| CN103698417B (en) | Content detection method of D-sodium erythorbate | |
| CN104991017B (en) | Liquid chromatogram-tandem mass spectrometry method for determining isothiazolinone bactericides contained in water-based adhesive | |
| CN103675153B (en) | Method for measuring main carbonyl compounds in cigarette filter through ultra-performance convergence chromatography | |
| CN102128906A (en) | Method for detecting volatile organic compound in cigarette filter | |
| CN104007218B (en) | The assay method of bisphenol S migration amount in a kind of plastic food packaging materials | |
| CN105067727A (en) | Method for measuring content of polyethylene glycol in polycarboxylate superplasticizer macromonomer | |
| CN103293260B (en) | Method for high-efficiency detection of rhodamine B in food and rapid detection kit | |
| CN112526007A (en) | Method for separating and detecting contents of m-cresol and p-cresol by using ultra-high liquid chromatography and application | |
| CN104535705A (en) | Method for synchronously measuring capsaicin and capsorubin in capsicum oleoresin | |
| CN102033117A (en) | Chromatographic qualitative detection method for identifying water-soluble toluylene bistriazine fluorescent whiteners | |
| CN104198605B (en) | A kind of assay method of cigarette hot melt adhesive phenol antioxidant content | |
| CN104950064A (en) | Method for measuring main carbonyl compounds in smoke-free tobacco by means of UPLC-IE method | |
| CN108152425A (en) | A kind of method of high performance liquid chromatography detection sesame oil lignanoid | |
| CN104237395B (en) | A kind of glacial water inorganic anion measuring method | |
| CN105158351B (en) | Construction method and applications of Shanxi mature vinegar liquid-phase fingerprint | |
| CN111443150A (en) | Method for detecting content of acetylcysteine and acetyltyrosine in compound amino acid injection | |
| CN104280474A (en) | High performance liquid chromatography fluorescence detection method for simultaneously measuring four prohibited and limited additives in tobacco flavors and perfumes | |
| CN103336068A (en) | Rapid measurement method of residual amounts of two photoinitiators in paper packaging material | |
| CN104297379B (en) | The method of high performance liquid chromatography-internal mark method determination pyrogallic acid content | |
| CN102507776B (en) | Method for determining phenol content in water | |
| CN104215720A (en) | Method for determining specific transfer volume of low-molecule aldehyde ketone in paper and paperboards | |
| CN115453022B (en) | Method for rapidly judging formaldehyde content in white spirit | |
| CN103592381B (en) | Method for detecting sulfonic acid phenylhydrazine sulfate series by high performance liquid chromatography | |
| CN102565229B (en) | Ion chromatograph and chemoluminescence detection method for determining catecholamine substances |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C53 | Correction of patent for invention or patent application | ||
| CB02 | Change of applicant information |
Address after: 518000 Guangdong city of Shenzhen province Nanshan District Fifth Industrial Zone Lang mountain C'estbon Food & Beverage Park Applicant after: Huarun C'estbon drinks (China) Co. Ltd. Address before: 518000 Guangdong city of Shenzhen province Nanshan District Fifth Industrial Zone Lang mountain C'estbon Food & Beverage Park Applicant before: Huanrun Estbon Food & Beverage (Shenzhen) Co., Ltd. |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: APPLICANT; FROM: HUANRUN ESTBON FOOD + BEVERAGE (SHENZHEN) CO., LTD. TO: CHINA RESOURCES C ESTBON BEVERAGE (CHINA) CO., LTD. |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |