CN103353499A - Method for simultaneously measuring gulonic acid, gulonic acid methyl ester and vitamin C through constant current performance liquid chromatography - Google Patents
Method for simultaneously measuring gulonic acid, gulonic acid methyl ester and vitamin C through constant current performance liquid chromatography Download PDFInfo
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- CN103353499A CN103353499A CN2013102850608A CN201310285060A CN103353499A CN 103353499 A CN103353499 A CN 103353499A CN 2013102850608 A CN2013102850608 A CN 2013102850608A CN 201310285060 A CN201310285060 A CN 201310285060A CN 103353499 A CN103353499 A CN 103353499A
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Abstract
The invention relates to a method for simultaneously measuring gulonic acid, gulonic acid methyl ester and vitamin C through a constant current performance liquid chromatography method. The method adopts the constant current, and has a low requirement for instruments and equipment. The method simultaneously measures gulonic acid, gulonic acid methyl ester and vitamin C, so that the problem that two or more than two methods are adopted to measure the different components of the same sample is solved, the method is fast, the whole separation process costs less than 10 minutes, degrees of separation of three kinds of components are all greater than 1.5, and the requirement of the relevant chromatography for the degree of separation is satisfied.
Description
Technical field
The invention belongs to biological raw material detection technique field, particularly relate to a kind of constant current liquid phase chromatography and measure simultaneously 2-KLG, methyl 2-keto-L-gulonate and ascorbic method.
Background technology
The mensuration of 2-KLG generally is that acid adding is boiled the generation vitamin C, and the vitamin C that generates with iodometric titrationiodimetry titration is again calculated 2-KLG content with this.Ascorbic mensuration all adopts iodometric determination in pharmacopoeia of each country.And in sample, having simultaneously 2-KLG, methyl 2-keto-L-gulonate, vitamin C, assay method yet there are no report.
High performance liquid chromatography with its efficiently, characteristic fast, be widely used in the Pharmaceutical Analysis field.In real work, how to use same chromatographic condition and many components sample is carried out express-analysis seem particularly important.The present invention adopts the constant current high performance liquid chromatography, simultaneously 2-KLG, methyl 2-keto-L-gulonate and vitamin C in the sample are analyzed, analysis time not enough 10min.
Summary of the invention
Purpose of the present invention just is to set up a kind of while and can measures 2-KLG, methyl 2-keto-L-gulonate and ascorbic method, avoids adopting two kinds and above method to measure different component in the same sample.
The technical scheme of taking for achieving the above object is: chromatographic condition: chromatographic column: the C18 post; Mobile phase: 0.3%～0.4% 4-butyl ammonium hydrogen sulfate (is regulated pH to 6.5～6.7 with ammoniacal liquor; Flow rate of mobile phase is: 0.8ml/min～1.0ml/min; Detect wavelength: 210nm～220nm; Sample solution preparation: sample thief is diluted with water to and contains 2-KLG and methyl 2-keto-L-gulonate is no more than 4mg/ml, contains the solution that vitamin C is no more than 2mg/ml.
Description of drawings
Accompanying drawing is the chromatogram of embodiment.
Embodiment
1 chromatographic condition:
Chromatographic column: C18 post; Mobile phase: 0.3%～0.4% 4-butyl ammonium hydrogen sulfate (is regulated pH to 6.5～6.7 with ammoniacal liquor; Flow rate of mobile phase is: 0.8ml/min～1.0ml/min; Detect wavelength: 210nm～220nm
2 solution preparation: sample solution preparation: sample thief is diluted with water to and contains 2-KLG and methyl 2-keto-L-gulonate is no more than 4mg/ml, contains the solution that vitamin C is no more than 2mg/ml.
3 measure: solution is injected high performance liquid chromatograph, and the record chromatogram is also analyzed.
Embodiment 1,
1 chromatographic condition:
Chromatographic column: Agilent XDB C18 post; Mobile phase: 0.30% 4-butyl ammonium hydrogen sulfate (regulating pH to 6.5 with ammoniacal liquor); Flow rate of mobile phase is: 1.0ml/min; Detect wavelength: 210nm
2 sample solutions preparations: sample thief is diluted with water to and contains 2-KLG and methyl 2-keto-L-gulonate is no more than 4mg/ml, contains the solution that vitamin C is no more than 2mg/ml.Get simultaneously 2-KLG, methyl 2-keto-L-gulonate and vitamin C reference substance and prepare contrast solution.
3 measure: solution is injected high performance liquid chromatograph, and the record chromatogram is also analyzed
The test sample lot number: 121223, test sample source: Qiyuan Pharmaceutical Co., Ltd., Ningxia
Measurement result: 121223 batch sample middle ancient times the dragon acid contents be 0.51%, methyl 2-keto-L-gulonate content is 5.24%, vitamin C is 15.23%.
Embodiment 2
1 chromatographic condition:
Chromatographic column: Agilent XDB C18 post; Mobile phase: 0.35% 4-butyl ammonium hydrogen sulfate (regulating pH to 6.6 with ammoniacal liquor); Flow rate of mobile phase is: 0.9ml/min; Detect wavelength: 215nm
2 sample solutions preparations: sample thief is diluted with water to and contains 2-KLG and methyl 2-keto-L-gulonate is no more than 4mg/ml, contains the solution that vitamin C is no more than 2mg/ml.Get simultaneously 2-KLG, methyl 2-keto-L-gulonate and vitamin C reference substance and prepare contrast solution.
3 measure: solution is injected high performance liquid chromatograph, and the record chromatogram is also analyzed
The test sample lot number: 121223, test sample source: Qiyuan Pharmaceutical Co., Ltd., Ningxia
Measurement result: 121223 batch sample middle ancient times the dragon acid contents be 0.54%, methyl 2-keto-L-gulonate content is 5.18%, vitamin C is 15.36%.
Embodiment 3
1 chromatographic condition:
Chromatographic column: Agilent XDB C18 post; Mobile phase: 0.4% 4-butyl ammonium hydrogen sulfate (regulating pH to 6.7 with ammoniacal liquor); Flow rate of mobile phase is: 0.8ml/min; Detect wavelength: 220nm
2 sample solutions preparations: sample thief is diluted with water to and contains 2-KLG and methyl 2-keto-L-gulonate is no more than 4mg/ml, contains the solution that vitamin C is no more than 2mg/ml.Get simultaneously 2-KLG, methyl 2-keto-L-gulonate and vitamin C reference substance and prepare contrast solution.
3 measure: solution is injected high performance liquid chromatograph, and the record chromatogram is also analyzed
The test sample lot number: 121223, test sample source: Qiyuan Pharmaceutical Co., Ltd., Ningxia
Measurement result: 121223 batch sample middle ancient times the dragon acid contents be 0.56%, methyl 2-keto-L-gulonate content is 5.23%, vitamin C is 15.28%.
Claims (2)
1. a constant current liquid phase chromatography is measured 2-KLG, methyl 2-keto-L-gulonate and ascorbic method simultaneously, it is characterized in that adopting high performance liquid chromatography.
2. measure simultaneously 2-KLG, methyl 2-keto-L-gulonate and ascorbic method according to constant current liquid phase chromatography claimed in claim 1, it is characterized in that the chromatographic condition of above-mentioned high performance liquid chromatography is:
Chromatographic column: C18 post;
Mobile phase: 0.3%～0.4% 4-butyl ammonium hydrogen sulfate, regulate pH to 6.5～6.7 with ammoniacal liquor;
Flow rate of mobile phase is: 0.8ml/min～1.0ml/min;
Detect wavelength: 210nm～220nm;
Sample solution concentration is that 2-KLG and methyl 2-keto-L-gulonate are no more than 4mg/ml, contain vitamin C and be no more than 2mg/ml.
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| CN2013102850608A CN103353499A (en) | 2013-07-09 | 2013-07-09 | Method for simultaneously measuring gulonic acid, gulonic acid methyl ester and vitamin C through constant current performance liquid chromatography |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107179370A (en) * | 2017-07-27 | 2017-09-19 | 石药集团维生药业（石家庄）有限公司 | A kind of method of gluconic acid content in use high performance liquid chromatography detection vitamin c fermenting liquid |
| 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 |
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| CN102183612A (en) * | 2011-03-15 | 2011-09-14 | 山东润鑫精细化工有限公司 | Method for simultaneously determining content of 2-keto-L-gulonic acid, content of vitamin C and content of 2-keto-L-gulonic acid methyl ester |
| CN102495165A (en) * | 2011-11-30 | 2012-06-13 | 安徽泰格生物技术股份有限公司 | Detection method for liquid chromatogram of keto-L-gulonic acid and/or keto-L-gulonic acid methyl ester |
| CN103115978A (en) * | 2013-01-29 | 2013-05-22 | 南京凯通粮食生化研究设计有限公司 | Rapid and accurate Vc measuring method for Vc production enterprises |
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- 2013-07-09 CN CN2013102850608A patent/CN103353499A/en active Pending
Patent Citations (3)
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| CN102183612A (en) * | 2011-03-15 | 2011-09-14 | 山东润鑫精细化工有限公司 | Method for simultaneously determining content of 2-keto-L-gulonic acid, content of vitamin C and content of 2-keto-L-gulonic acid methyl ester |
| CN102495165A (en) * | 2011-11-30 | 2012-06-13 | 安徽泰格生物技术股份有限公司 | Detection method for liquid chromatogram of keto-L-gulonic acid and/or keto-L-gulonic acid methyl ester |
| CN103115978A (en) * | 2013-01-29 | 2013-05-22 | 南京凯通粮食生化研究设计有限公司 | Rapid and accurate Vc measuring method for Vc production enterprises |
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| WILLY A. BEHRENS ET AL: "Ascorbic acid, isoascorbic acid, dehydroascorbic acid, and dehydroisoascorbic acid in selected food products", 《JOURNAL OF FOOD COMPOSITION AND ANALYSIS》, vol. 7, no. 3, 30 September 1994 (1994-09-30), pages 158 - 170 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107179370A (en) * | 2017-07-27 | 2017-09-19 | 石药集团维生药业（石家庄）有限公司 | A kind of method of gluconic acid content in use high performance liquid chromatography detection vitamin c fermenting liquid |
| 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 |
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Application publication date: 20131016 |