CN111157638A - Method for detecting oxalic acid content in vitamin C - Google Patents
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Abstract
The invention relates to an analysis method for detecting oxalic acid content, which adopts a high performance liquid chromatograph, and has the following chromatographic conditions: octadecylsilane chemically bonded silica chromatographic column, mobile phase: phosphate buffered solution (containing tetrabutylammonium hydroxide) -acetonitrile, mobile phase A, B was performed according to a gradient procedure; the flow rate is 0.9-1.6 ml/min; the column temperature is 28-40 ℃, the detection wavelength is 200-210nm, and the sample injection amount is 20-50 μ l. The detection method has high sensitivity and good linear relation, and is suitable for detecting the content of oxalic acid in vitamin C or a preparation containing vitamin C.
Description
Technical Field
The invention belongs to the field of analytical chemistry, and particularly relates to a high performance liquid analysis method for detecting oxalic acid content in vitamin C.
Background
Vitamin C (Ascorbic Acid), also known as L-Ascorbic Acid, is a water-soluble Vitamin. The vitamin C has the main functions of improving immunity, preventing cancer, heart disease and stroke, protecting teeth and gums and the like. Oxalic acid is one of the main degradation products of vitamin C, can reduce the bioavailability of mineral elements, is easy to form calcium oxalate with calcium ions in a human body to cause kidney stones, and is often considered as an antagonist for the absorption and utilization of the mineral elements. The structural formulas are respectively as follows:
vitamin C
Oxalic acid
The detection method of vitamin C oxalic acid in domestic and foreign pharmacopoeia is turbidimetry, and for various vitamins (12) for injection containing raw material of vitamin C, the sample solution is colored, so that it is not suitable for turbidimetry, and in the reference document "HPLC method determination of oxalic acid in composite vitamins for injection" disclosed in Lianwei et al, high performance liquid chromatography and strong cation exchange column (H) are adopted+Type) is used for measuring oxalic acid, but chromatographic columns of the type are not commonly used and are not ideal in specificity, other single impurities and total impurities are controlled by other literature related to measurement of vitamin C related substances, and oxalic acid is not controlled independently; in addition, the methods for measuring the oxalic acid content in food in the literature are not completely applicable to vitamin C or vitamin C-containing preparations.
The invention content is as follows:
in order to solve the problems, the invention provides a method for detecting vitamin C raw materials and simultaneously suitable for detecting preparations containing the vitamin C raw materials, in particular the oxalic acid content in various vitamin preparations, and the technical scheme of the method is as follows:
an analysis method for detecting the oxalic acid content in vitamin C adopts a high performance liquid chromatograph, and the chromatographic conditions are as follows:
a chromatographic column: octadecylsilane chemically bonded silica chromatographic column;
mobile phase A: phosphate buffered solution (containing tetrabutylammonium hydroxide) -acetonitrile;
mobile phase B: phosphate buffered solution (containing tetrabutylammonium hydroxide) -acetonitrile;
flow rate: 0.9-1.6 ml/min;
column temperature: 28-40 ℃;
detection wavelength: 200-210 nm;
sample introduction amount: 20 to 50 mul;
the mobile phase A, B was performed in a gradient program.
Wherein, the preferred chromatographic column is an Agela Venusil C18 Plus, 250mm × 4.6mm, 5 μm or equivalent-performance octadecylsilane chemically bonded silica chromatographic column;
a phosphate buffer solution with a mobile phase A of 0.01mol/L-0.05mol/L, wherein the phosphate is one of potassium dihydrogen phosphate, dipotassium hydrogen phosphate, sodium dihydrogen phosphate or disodium hydrogen phosphate, the tetrabutyl ammonium hydroxide is contained in the phosphate buffer solution, the pH value of the phosphate buffer solution is adjusted to 3.0-7.0 by phosphoric acid, and the phosphate buffer solution (containing the tetrabutyl ammonium hydroxide) is prepared by the following steps: the acetonitrile is 85-99: 15-1.
Mobile phase B is 0.01mol/L-0.05mol/L phosphate buffer solution, phosphate can be potassium dihydrogen phosphate, dipotassium hydrogen phosphate, sodium dihydrogen phosphate or disodium hydrogen phosphate, etc., and contains tetrabutyl ammonium hydroxide of 0.1% -0.4%, the pH value of the buffer solution is adjusted to 3.0-7.0 by phosphoric acid, phosphate buffer solution (contains tetrabutyl ammonium hydroxide): the acetonitrile is 15-25: 85-75.
The preferred flow rate is 1.2ml/min
The preferred column temperature is 30 ℃;
the injection gradient elution procedure was:
the method can be used for detecting oxalic acid content in vitamin C raw material or vitamin C raw material-containing preparation such as vitamin preparation for injection, thereby performing quality control of oxalic acid content in raw material and preparation.
The invention has the following beneficial effects:
1) by using the technology of a high performance liquid chromatograph, the method for detecting the oxalic acid content in the vitamin C raw material or the preparation containing the vitamin C raw material, such as vitamin preparation for injection, is provided, the material consumption is easy to obtain, and the accuracy and the sensitivity are high.
2) Through detection, the limit of oxalic acid quantification is 40.02ng, and the limit of detection is 20.01ng, which indicates that the method has higher detection sensitivity.
3) Oxalic acid is in the concentration range of 0.8004 mug/ml to 4.8024 mug/ml, the linear regression equation is A30540C-208, the correlation coefficient is 0.9997, and the linear relation is good.
4) A known amount of oxalic acid control was added to the sample and the average recovery measured was 100.6%, meeting the acceptance criteria, indicating good accuracy of the method.
Description of the drawings:
FIG. 1 is a standard graph of oxalic acid in example 2;
FIG. 2 is a chromatogram for detecting a sample to be tested in example 6.
The specific implementation mode is as follows:
the present invention is further described in the following detailed description, which is for the purpose of illustration only, and the scope of the invention is not limited to these examples, and it will be understood by those skilled in the art that various equivalent substitutions and modifications may be made within the scope of the invention.
Example 1 detection of detection and quantitation limits
Taking about 20mg of oxalic acid reference substance, precisely weighing, placing in a 25ml measuring flask, adding water for dissolving, diluting to a scale, and shaking up;
precisely measuring 5ml of the solution obtained in the step (1), placing the solution in a 50ml measuring flask, diluting the solution to a scale with water, and shaking up;
precisely measuring 0.5ml of the solution obtained in the step (2), placing the solution in a 100ml measuring flask, adding water to dilute the solution to a scale, shaking the solution uniformly, precisely measuring 50 mu l of the solution, injecting the solution into a liquid chromatograph, wherein the signal-to-noise ratio S/N is about 10:1, and the concentration of oxalic acid is 0.8004 mu g/ml;
and (4) precisely measuring 5ml of the solution obtained in the step (3), putting the solution into a 10ml measuring flask, adding water to dilute the solution to a scale, shaking the solution uniformly, precisely measuring 50 mu l of the solution, injecting the solution into a liquid chromatograph, and taking the S/N ratio of the solution to the liquid chromatograph as about 3:1 as a detection limit and the concentration of oxalic acid as 0.4002 mu g/ml.
EXAMPLE 2 determination of the Standard Curve
Taking about 20mg of oxalic acid reference substance, precisely weighing, placing in a 25ml measuring flask, adding water for dissolving, diluting to a scale, and shaking up;
precisely measuring 5ml of the solution obtained in the step (1), placing the solution in a 50ml measuring flask, diluting the solution to a scale with water, and shaking up;
and (3) precisely measuring the solutions 1, 2, 3, 4, 5 and 6ml in the step (2), placing the solutions in different 100ml measuring bottles, adding water to dilute the solutions to a scale, and shaking the solutions uniformly to obtain linear solutions of 20%, 40%, 60%, 80%, 100% and 120%.
And (4) precisely measuring 50 mu l of each linear solution in the step (3), injecting the linear solution into a liquid chromatograph, and performing linear regression by taking the concentration C (mu g/ml) as an abscissa and the peak area A as an ordinate, wherein the linear equation is A30540C-208, and the correlation coefficient r is 0.9997, as shown in the attached figure 1 of the specification.
Example 3 determination of recovery
Taking about 20mg of an oxalic acid reference substance, precisely weighing, placing the oxalic acid reference substance in a 25ml measuring flask, dissolving the oxalic acid reference substance with water, diluting the oxalic acid reference substance to scale, shaking up, precisely weighing 5ml, placing the oxalic acid reference substance in a 50ml measuring flask, diluting the oxalic acid reference substance with water to scale, and shaking up to obtain an oxalic acid reference substance stock solution;
precisely measuring 5ml of reference substance storage solution, placing the reference substance storage solution in a 100ml measuring flask, diluting the reference substance storage solution to a scale with water, and shaking up to obtain an oxalic acid reference substance solution;
and (3) precisely weighing about 390mg of the multivitamin (12) for injection, placing the multivitamin in a 50ml measuring flask, adding water to dissolve and dilute the multivitamin to a scale, and shaking up to obtain the multivitamin injection.
Step (4) taking 390mg of the multi-vitamin (12) for injection, precisely weighing, respectively placing three parts into different 50ml measuring bottles, respectively and precisely adding 2ml, 2.5ml and 3ml of the solution obtained in the step (1), adding water to dilute to a scale, shaking up, respectively taking the solution as 80%, 100% and 120% sample solutions, and preparing three parts in parallel at each concentration level;
and (5) precisely measuring 50 mu l of the solution, respectively injecting the solution into a liquid chromatograph, and recording a chromatogram. According to an external standard method, calculating the content of oxalic acid in a test sample by peak area, and calculating the recovery rate by the ratio of the difference between the measured amount and the original amount to the added amount, wherein the results are as follows:
EXAMPLE 4 determination of oxalic acid content in vitamin C
Step 1, preparation of solution
Precisely weighing about 20mg of oxalic acid reference substance, placing in a 50ml measuring flask, dissolving with water, diluting to scale, and shaking; precisely measuring 1ml, placing into a 100ml measuring flask, diluting with water to scale, and shaking.
Preparing a test solution: precisely weighing about 65mg of vitamin C, placing in a 50ml measuring flask, adding water to dissolve and dilute to scale, and shaking up to obtain the final product.
And 2, the liquid chromatography conditions are as follows:
a chromatographic column: octadecylsilane chemically bonded silica chromatographic column;
mobile phase A: 0.01mol/L potassium dihydrogen phosphate solution (1.36 g potassium dihydrogen phosphate, 8ml 25% tetrabutyl ammonium hydroxide solution, water dissolution and dilution to 1000ml, pH value adjusted to 6.6 with phosphoric acid) -acetonitrile (85: 15);
mobile phase B: 0.01mol/L potassium dihydrogen phosphate solution (1.36 g potassium dihydrogen phosphate, 8ml 25% tetrabutyl ammonium hydroxide solution, water dissolution and dilution to 1000ml, pH value adjusted to 6.6 with phosphoric acid) -acetonitrile (15: 85);
flow rate: 0.9-1.6 ml/min;
column temperature: 28-40 ℃;
detection wavelength: 200-210 nm;
sample introduction amount: 20 to 50 mul;
the mobile phase A, B was performed in a gradient program.
Precisely measuring the above solutions at a volume of 50 μ l each, injecting into a liquid chromatograph, and recording chromatogram. According to an external standard method, the oxalic acid content in the test solution is 0.01 percent by peak area calculation.
EXAMPLE 5 determination of oxalic acid content in vitamin C
Step 1, preparation of solution
Precisely weighing about 20mg of oxalic acid reference substance, placing in a 50ml measuring flask, dissolving with water, diluting to scale, and shaking; precisely measuring 1ml, placing into a 100ml measuring flask, diluting with water to scale, and shaking.
Preparing a test solution: precisely weighing about 65mg of vitamin C, placing in a 50ml measuring flask, adding water to dissolve and dilute to scale, and shaking up to obtain the final product.
And 2, the liquid chromatography conditions are as follows:
a chromatographic column: octadecylsilane chemically bonded silica chromatographic column;
mobile phase A: 0.05mol/L potassium dihydrogen phosphate solution-acetonitrile (99:1), and the preparation method of the 0.05mol/L potassium dihydrogen phosphate solution comprises the following steps: taking 6.8g of monopotassium phosphate, adding 16ml of 25% tetrabutylammonium hydroxide solution, adding water for dissolving and diluting to 1000ml, and adjusting the pH value to 7.0 by using phosphoric acid;
mobile phase B: 0.05mol/L potassium dihydrogen phosphate solution-acetonitrile (25:75), and the preparation method of the 0.05mol/L potassium dihydrogen phosphate solution comprises the following steps: taking 6.8g of monopotassium phosphate, adding 16ml of 25% tetrabutylammonium hydroxide solution, adding water for dissolving and diluting to 1000ml, and adjusting the pH value to 7.0 by using phosphoric acid;
flow rate: 0.9-1.6 ml/min;
column temperature: 28-40 ℃;
detection wavelength: 200-210 nm;
sample introduction amount: 20 to 50 mul;
the mobile phase A, B was performed in a gradient program.
Precisely measuring the above solutions at a volume of 50 μ l each, injecting into a liquid chromatograph, and recording chromatogram. According to an external standard method, the oxalic acid content in the test solution is 0.01 percent by peak area calculation.
EXAMPLE 6 determination of oxalic acid content in multivitamin for injection (12) (this preparation contains vitamin D3, rac- α -tocopherol, vitamin A palmitate, vitamin C, cocarboxylase tetrahydrate, dexpanthenol, niacinamide, vitamin B6, riboflavin sodium phosphate, folic acid, biotin, vitamin B12, glycocholic acid, soybean phosphatidylcholine, glycine, appropriate amounts of hydrochloric acid/sodium hydroxide)
Step 1, preparation of solution
Preparing a reference substance solution: precisely weighing about 20mg of oxalic acid reference substance, placing in a 50ml measuring flask, dissolving with water, diluting to scale, and shaking; precisely measuring 1ml, placing into a 100ml measuring flask, diluting with water to scale, and shaking.
Preparing a test solution: precisely weighing 390mg of multivitamin (12) for injection, placing into a 50ml measuring flask, adding water to dissolve, diluting to scale, and shaking.
And 2, the liquid chromatography conditions are as follows:
a chromatographic column: an Agela Venusil C18 Plus, 250 mm. times.4.6 mm, 5 μm or equivalent performance octadecylsilane bonded silica chromatographic column;
mobile phase A: 0.01mol/L-0.05mol/L phosphate buffer solution-acetonitrile (85-99: 15-1), wherein the buffer solution contains 0.1% -0.4% of tetrabutylammonium hydroxide, and the pH value is adjusted to 3.0-7.0 by using phosphoric acid;
mobile phase B: 0.01mol/L-0.05mol/L phosphate buffer solution-acetonitrile (15-25: 85-75), wherein the buffer solution contains 0.1% -0.4% of tetrabutylammonium hydroxide, and the pH value is adjusted to 3.0-7.0 by using phosphoric acid;
flow rate: 0.9-1.6 ml/min;
column temperature: 28-40 ℃;
detection wavelength: 200-210 nm;
sample introduction amount: 20 to 50 mul;
the mobile phase A, B was performed in a gradient program.
Precisely measuring the above solutions at 20 μ l, respectively injecting into liquid chromatograph, and recording chromatogram, which is shown in figure 2 of the specification. According to an external standard method, the oxalic acid content in the test solution is 0.02 percent by peak area calculation.
Example 7 determination of oxalic acid content in Compound vitamin injection (13) bottle 1 (bottle 1 contains vitamin D3, vitamin E, vitamin A palmitate, vitamin K1, vitamin C, vitamin B1, dexpanthenol, niacinamide, vitamin B6, riboflavin sodium phosphate, polysorbate 80, hydrochloric acid/sodium hydroxide in proper amount)
Step 1, preparation of solution
Preparing a reference substance solution: taking about 15mg of oxalic acid reference substance, precisely weighing, placing in a 25ml measuring flask, dissolving with water, diluting to scale, and shaking; precisely measuring 1ml, placing into a 100ml measuring flask, diluting with water to scale, and shaking.
Preparing a test solution: taking 5ml of compound vitamin injection (13) in a bottle 1, placing in a 100ml measuring flask, adding water to dissolve, diluting to scale, and shaking up to obtain the final product.
And 2, the liquid chromatography conditions are as follows:
a chromatographic column: an Agela Innoval C18, 250mm × 4.6mm, 5 μm or an octadecylsilane bonded silica chromatographic column of equivalent potency;
mobile phase A: 0.01mol/L-0.05mol/L phosphate buffer solution-acetonitrile (85-99: 15-1,) buffer solution contains 0.1% -0.4% tetrabutyl ammonium hydroxide, and pH value is adjusted to 3.0-7.0 by phosphoric acid;
mobile phase B: 0.01mol/L-0.05mol/L phosphate buffer solution-acetonitrile (15-25: 85-75), wherein the buffer solution contains 0.1% -0.4% of tetrabutylammonium hydroxide, and the pH value is adjusted to 3.0-7.0 by using phosphoric acid;
flow rate: 0.9-1.6 ml/min;
column temperature: 28-40 ℃;
detection wavelength: 200-210 nm;
sample introduction amount: 20 to 50 mul;
the mobile phase A, B was performed in a gradient program.
Precisely measuring 20 μ l of each solution, injecting into a liquid chromatograph, recording chromatogram, and calculating the oxalic acid content in the test solution to be 0.08% by peak area according to an external standard method.
Claims (10)
1. A method for detecting the oxalic acid content in vitamin C by adopting a high performance liquid chromatograph is characterized in that the chromatographic conditions are as follows:
a chromatographic column: octadecylsilane chemically bonded silica chromatographic column;
mobile phase A: phosphate buffer-acetonitrile;
mobile phase B: phosphate buffer-acetonitrile;
flow rate: 0.9-1.6 ml/min;
column temperature: 28-40 ℃;
detection wavelength: 200-210 nm;
sample introduction amount: 20 to 50 mul;
the mobile phase A, B was performed in a gradient program.
2. The method of claim 1, wherein: the chromatographic column is an Agela Venusil C18 Plus, 250mm × 4.6mm, 5 μm or equivalent-performance octadecylsilane bonded silica chromatographic column.
3. The method according to claim 1, wherein the phosphate is one of potassium dihydrogen phosphate, dipotassium hydrogen phosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, or the like, the concentration of the phosphate buffer solution is 0.01mol/L to 0.05mol/L, and the pH is adjusted to 3.0 to 7.0 with phosphoric acid; the phosphate buffer solution contains 0.1% -0.4% tetrabutylammonium hydroxide.
4. The method according to claim 1, wherein in mobile phase a, the phosphate buffer solution: acetonitrile is 85-99: 15-1; potassium dihydrogen phosphate buffer solution in mobile phase B: the acetonitrile is 15-25: 85-75.
5. The method of claim 1, wherein the flow rate is 1.2 ml/min; the column temperature is 30 ℃; the injection gradient elution procedure was:
6. the method of claim 1 for detecting the amount of oxalic acid in vitamin C.
7. The method of claim 1 for detecting oxalate content in a vitamin C-containing formulation.
8. The method of claim 1 for detecting the amount of oxalic acid in vitamin C-containing injectable formulations.
9. The method for detecting the oxalic acid content of the multivitamins for injection (12) according to claim 1, wherein the chromatographic conditions are as follows:
a chromatographic column: an Agela Venusil C18 Plus, 250 mm. times.4.6 mm, 5 μm or equivalent performance octadecylsilane bonded silica chromatographic column;
mobile phase A: 0.01mol/L-0.05mol/L phosphate buffer solution-acetonitrile;
mobile phase B: 0.01mol/L-0.05mol/L phosphate buffer solution-acetonitrile;
flow rate: 0.9-1.6 ml/min;
column temperature: 28-40 ℃;
detection wavelength: 200-210 nm;
sample introduction amount: 20 to 50 mul;
the mobile phase A, B was run according to a gradient program with the following gradient elution program:
the phosphate buffer solution contains 0.1% -0.4% of tetrabutylammonium hydroxide, the pH value is adjusted to 3.0-7.0 by phosphoric acid, and in the mobile phase A, the phosphate buffer solution: acetonitrile is 85-99: 15-1; potassium dihydrogen phosphate buffer solution in mobile phase B: the acetonitrile is 15-25: 85-75.
10. The method for detecting the content of oxalic acid in the compound vitamin injection (13) is characterized in that the chromatographic conditions are as follows:
a chromatographic column: an Agela Innoval C18, 250mm × 4.6mm, 5 μm or performance equivalent octadecylsilane bonded silica chromatography column;
mobile phase A: 0.01mol/L-0.05mol/L phosphate buffer solution-acetonitrile;
mobile phase B: 0.01mol/L-0.05mol/L phosphate buffer solution-acetonitrile;
flow rate: 0.9-1.6 ml/min;
column temperature: 28-40 ℃;
detection wavelength: 200-210 nm;
sample introduction amount: 20 to 50 mul;
the mobile phase A, B was run according to a gradient program with the following gradient elution program:
the phosphate buffer solution contains 0.1 to 0.4 percent of tetrabutylammonium hydroxide, and the pH value is adjusted to 3.0 to 7.0 by phosphoric acid; in mobile phase a, the phosphate buffer solution: acetonitrile is 85-99: 15-1; potassium dihydrogen phosphate buffer solution in mobile phase B: the acetonitrile is 15-25: 85-75.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114791469A (en) * | 2022-04-25 | 2022-07-26 | 四川启源药业有限公司 | Method for detecting content of vitamin C in famotidine injection |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2003216279A1 (en) * | 2002-02-28 | 2003-09-16 | Mallinckrodt Inc. | Method and system for separation and purification of at least one narcotic alkaloid using reverse phase preparative chromatography |
| CN101101284A (en) * | 2007-07-26 | 2008-01-09 | 复旦大学 | Method for simultaneously determining multiple organic acid content of fruit |
| CN103543236A (en) * | 2013-10-12 | 2014-01-29 | 福建省农业科学院农业工程技术研究所 | Method for determining organic acid content of fermented wine by ion-exclusion chromatography |
| US20170368208A1 (en) * | 2015-01-11 | 2017-12-28 | Endocyte, Inc. | Cancer imaging agent |
| WO2018118826A1 (en) * | 2016-12-22 | 2018-06-28 | Merck Sharp & Dohme Corp. | Antiviral benzyl-amine phosphodiamide compounds |
-
2019
- 2019-12-31 CN CN201911405608.1A patent/CN111157638A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2003216279A1 (en) * | 2002-02-28 | 2003-09-16 | Mallinckrodt Inc. | Method and system for separation and purification of at least one narcotic alkaloid using reverse phase preparative chromatography |
| CN101101284A (en) * | 2007-07-26 | 2008-01-09 | 复旦大学 | Method for simultaneously determining multiple organic acid content of fruit |
| CN103543236A (en) * | 2013-10-12 | 2014-01-29 | 福建省农业科学院农业工程技术研究所 | Method for determining organic acid content of fermented wine by ion-exclusion chromatography |
| US20170368208A1 (en) * | 2015-01-11 | 2017-12-28 | Endocyte, Inc. | Cancer imaging agent |
| WO2018118826A1 (en) * | 2016-12-22 | 2018-06-28 | Merck Sharp & Dohme Corp. | Antiviral benzyl-amine phosphodiamide compounds |
Non-Patent Citations (3)
| Title |
|---|
| HUSSEIN G. DAOOD 等: "Ion-Pair Chromatography and Photodiode-Array Detection of Vitamin C and Organic Acids", 《JOURNAL OF CHROMATOGRAPHIC SCIENCE》 * |
| 彭婕等: "饲料对大鼠尿液中草酸含量的影响", 《江苏药学与临床研究》 * |
| 杨剑宇: "维生素C母液回收生产试验中水不溶物的鉴定", 《煤炭与化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114791469A (en) * | 2022-04-25 | 2022-07-26 | 四川启源药业有限公司 | Method for detecting content of vitamin C in famotidine injection |
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