CN110579540A - Quality standard of dexamethasone sodium phosphate injection and detection method thereof - Google Patents
Quality standard of dexamethasone sodium phosphate injection and detection method thereof Download PDFInfo
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- CN110579540A CN110579540A CN201910728970.6A CN201910728970A CN110579540A CN 110579540 A CN110579540 A CN 110579540A CN 201910728970 A CN201910728970 A CN 201910728970A CN 110579540 A CN110579540 A CN 110579540A
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- nicotinamide
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- sodium phosphate
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- phosphate injection
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
Abstract
The invention provides a quality standard detection method of dexamethasone sodium phosphate injection, which comprises the following steps: preparing a reference solution: weighing a nicotinamide reference substance, and dissolving the nicotinamide reference substance in water to prepare a nicotinamide reference substance solution; preparing a test solution: weighing dexamethasone sodium phosphate injection to be detected, and adding water to dissolve the dexamethasone sodium phosphate injection to prepare a nicotinamide test solution; preparing a system adaptive solution: measuring dexamethasone sodium phosphate injection, and adding water to dilute to prepare solution A; weighing a nicotinic acid reference substance, and adding water to dissolve the nicotinic acid reference substance to prepare a solution B; respectively measuring the solution A and the solution B, and adding water to dilute to prepare a mixed solution containing nicotinic acid and nicotinamide; and injecting the prepared mixed solution into a liquid chromatograph for detection, and if the separation degree of the nicotinamide and the nicotinic acid is not less than 3.0 and the theoretical plate number is not less than 2000 calculated according to the nicotinamide, respectively measuring a nicotinamide reference substance solution and a nicotinamide test solution, and injecting the two solutions into the liquid chromatograph for detection to obtain the content of the nicotinamide in the nicotinamide test solution.
Description
Technical Field
The invention relates to the technical field of chemical injection, in particular to a quality standard of dexamethasone sodium phosphate injection and a detection method thereof.
Background
Dexamethasone sodium phosphate belongs to glucocorticoid medicaments, is white or yellowish powder, has no odor and slight bitter taste, is easy to absorb moisture, is easy to dissolve in water and is difficult to dissolve in chloroform, diethyl ether and acetone. Dexamethasone sodium phosphate injection belongs to an injection, is a common medicine, is a white clear solution, is mainly used for treating allergic and autoimmune inflammatory diseases, is mainly used for treating connective tissue diseases, active rheumatism, rheumatoid arthritis, lupus erythematosus, severe bronchial asthma, severe dermatitis, ulcerative colitis, acute leukemia and the like, is also used for comprehensively treating some severe infections, poisoning and malignant lymphoma, and is widely applied clinically due to obvious curative effect and low price.
Nicotinamide is one of B vitamins, is involved in the metabolic process in vivo, is necessary for lipid metabolism, oxidation of tissue respiration and glycogenolysis, can be used for preventing and treating niacin-deficient rough skin disease, coronary heart disease, viral myocarditis, rheumatic myocarditis, and arrhythmia accompanied by digitalis poisoning, and has the effect of preventing and treating heart conduction block. The addition amount of nicotinamide in the dexamethasone sodium phosphate injection is about 3 times of that of dexamethasone sodium phosphate serving as a main component, but the content of the dexamethasone sodium phosphate in the injection is only determined in the original quality standard, and the content of the dexamethasone sodium phosphate cannot well represent the quality of the product.
Disclosure of Invention
In view of the above, the invention provides a quality standard of dexamethasone sodium phosphate injection and a detection method thereof, which increase the content determination of nicotinamide by high performance liquid chromatography on the basis of the original quality standard and improve the product quality.
the invention provides a quality standard detection method of dexamethasone sodium phosphate injection, which comprises the following steps:
S1, preparing a control solution: weighing a nicotinamide reference substance, and dissolving the nicotinamide reference substance in water to prepare a nicotinamide reference substance solution;
S2, preparing a test solution: measuring the dexamethasone sodium phosphate injection to be detected, adding water to dissolve the dexamethasone sodium phosphate injection to prepare a nicotinamide test solution, wherein the content of nicotinamide in the dexamethasone sodium phosphate injection is equal to the mass of the nicotinamide reference substance in the step S1, and the concentration of the nicotinamide test solution is equal to that of the nicotinamide reference substance solution;
S3, preparing a system adaptive solution: measuring dexamethasone sodium phosphate injection, and adding water to dilute to prepare solution A; weighing a nicotinic acid reference substance, and adding water to dissolve the nicotinic acid reference substance to prepare a solution B; respectively measuring the solution A and the solution B, and adding water to dilute to prepare a mixed solution containing nicotinic acid and nicotinamide;
s4, injecting the mixed solution prepared in the step S3 into a liquid chromatograph for detection, and if the separation degree of the nicotinamide and the nicotinic acid is not less than 3.0 and the theoretical plate number is not less than 2000 calculated according to the nicotinamide, performing the step S5;
S5, respectively measuring the nicotinamide reference solution and the nicotinamide test solution, injecting into a liquid chromatograph, and detecting to obtain the content of nicotinamide in the nicotinamide test solution.
Further, the concentration of the nicotinamide control solution is 0.1mg/ml, and the concentration of the nicotinamide test solution is 0.1 mg/ml.
further, 2mg of nicotinamide was contained in 1ml of solution A, 1mg of nicotinic acid was contained in 1ml of solution B, and 20. mu.g of nicotinic acid and 100. mu.g of nicotinamide were contained in 1ml of the mixed solution.
Further, in steps S4 and S5, the setting conditions of the liquid chromatograph are: octadecylsilane chemically bonded silica is used as a filling agent; taking a methanol-0.005M sodium heptanesulfonate solution as a mobile phase, wherein the volume ratio of the methanol to the sodium heptanesulfonate solution is 30: 70; the detection wavelength is 262 nm; the flow rate is 1.0 ml/min; the column temperature was 30 ℃.
The invention also provides a quality standard of the dexamethasone sodium phosphate injection, and the dexamethasone sodium phosphate injection is judged to be a qualified product when the content of nicotinamide in the nicotinamide test sample solution detected by the quality standard detection method is 90.0-110.0%; and when the content of the nicotinamide in the nicotinamide test solution is lower than 90.0%, judging that the dexamethasone sodium phosphate injection is an unqualified product.
The technical scheme provided by the invention has the beneficial effects that: the quality standard detection method provided by the invention is additionally provided with the content determination of nicotinamide in the injection by utilizing the high performance liquid chromatography on the basis of the existing quality standard of the dexamethasone sodium phosphate injection, is stable and reliable, has strong specificity, and can effectively improve the quality control of the dexamethasone sodium phosphate injection.
Drawings
FIG. 1 is a liquid chromatogram of a mixed solution measured by a high performance liquid chromatograph of Dyan U-3000;
FIG. 2 is a nicotinamide content spectrum measured by a high performance liquid chromatograph of Daian U-3000;
Figure 3 is a linear plot of nicotinamide content.
Detailed Description
in order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be further described with reference to the accompanying drawings.
In the following examples:
The setting conditions of the liquid chromatograph are as follows: octadecylsilane chemically bonded silica is used as a filling agent; using methanol-0.005M (M represents mol/l) sodium heptanesulfonate solution as a mobile phase, wherein the volume ratio of methanol to the sodium heptanesulfonate solution is 30: 70; the detection wavelength is 262 nm; the flow rate is 1.0 ml/min; the column temperature was 30 ℃.
Instruments and reagents: a Dyan U-3000 high performance liquid chromatograph; an Agilent high performance liquid chromatograph; a VWD variable wavelength ultraviolet detector; an intelligent column oven; a chromatographic column: thermo C18150X 4.6 mm.
Niacinamide control: purchased at check out; niacin control: purchased at check out; dexamethasone sodium phosphate impurity I control: purchased from check-in.
the methanol is chromatographically pure; the water is ultrapure water; other reagents were analytically pure.
The embodiment of the invention provides a quality standard detection method of dexamethasone sodium phosphate injection, which comprises the following steps:
Step S1, preparing a reference solution: accurately weighing 20mg nicotinamide reference substance into a 200ml measuring flask, dissolving with water, diluting, and fixing volume to scale to obtain 0.1mg/ml nicotinamide reference substance solution;
Step S2, preparing a test solution: precisely measuring a proper amount of dexamethasone sodium phosphate injection to be detected, placing the dexamethasone sodium phosphate injection into a 200ml measuring flask, dissolving the dexamethasone sodium phosphate injection with water, diluting the dexamethasone sodium phosphate injection, and fixing the volume to a scale to prepare a nicotinamide test solution of 0.1mg/ml, wherein the content of nicotinamide in the dexamethasone sodium phosphate injection is 20 mg;
Step S3, preparing a system adaptation solution: diluting dexamethasone sodium phosphate injection with water to obtain a solution A containing nicotinamide 2mg in each 1ml, dissolving nicotinic acid reference substance in water to obtain a solution B containing nicotinic acid 1mg in each 1ml, precisely measuring appropriate amounts of the solution A and the solution B, respectively, and diluting with water to obtain a mixed solution containing nicotinic acid 20 μ g and nicotinamide 100 μ g in each 1 ml;
step S4, injecting the mixed solution prepared in the step S3 into a liquid chromatograph for detection, and if the separation degree of nicotinamide and nicotinic acid is not less than 3.0 and the theoretical plate number is not less than 2000 calculated according to nicotinamide, performing the step S5; if the separation degree of the nicotinamide and the nicotinic acid is less than 3.0 or the theoretical plate number is less than 2000 calculated according to the nicotinamide, the problem of the liquid phase chromatographic system is shown, and the high performance liquid chromatograph, the chromatographic column or the mobile phase are checked and corrected and then the experiment is started;
Step S5, respectively measuring a nicotinamide reference substance solution and a nicotinamide test sample solution, injecting the nicotinamide reference substance solution and the nicotinamide test sample solution into a liquid chromatograph for detection to obtain the content of nicotinamide in the nicotinamide test sample solution, and judging that the dexamethasone sodium phosphate injection is a qualified product when the content of nicotinamide in the nicotinamide test sample solution is 90.0% -110.0% through detection; and when the content of the nicotinamide in the nicotinamide test solution is lower than 90.0%, judging that the dexamethasone sodium phosphate injection is an unqualified product.
In order to verify the reliability of the quality standard detection method provided in this embodiment, a specificity test, a recovery rate test, a linearity test, an instrument precision test, a repeatability test, an intermediate precision test, a solution stability test, and a durability test were performed below, respectively.
First, specificity test
and (3) auxiliary material interference test:
The method comprises the following steps: and taking a proper amount of blank solvent-ultrapure water and blank auxiliary material solution for testing.
As a result: the solvent and the blank auxiliary materials can not generate peaks at the peak position of the nicotinamide, and have no interference on content measurement.
mixed solution test:
the method comprises the following steps: respectively taking appropriate amounts of a nicotinic acid reference substance, a nicotinamide reference substance, a dexamethasone sodium phosphate impurity I reference substance, a dexamethasone sodium phosphate reference substance and a dexamethasone reference substance, adding water to dissolve and prepare positioning solutions with appropriate concentrations, respectively taking appropriate amounts of the positioning solutions, diluting with water and mixing to prepare mixed solutions. And (3) taking 20 mu L of each positioning solution and each mixed solution according to a chromatographic program, and injecting the positioning solution and the mixed solution into a liquid chromatograph, wherein the separation degree between any two adjacent chromatographic peaks in the chromatogram obtained from the mixed solution is required to be not less than 1.5.
as a result: the results are shown in FIG. 1, with a degree of separation between the peaks of greater than 1.5. Test solution:
the method comprises the following steps: and precisely measuring a proper amount of dexamethasone sodium phosphate injection to be detected, preparing the dexamethasone sodium phosphate injection according to the test solution and carrying out experiments.
As a result: the result is shown in figure 2, no impurity peak in the test solution interferes with main peak of nicotinamide, and the separation degree of nicotinamide peak and dexamethasone sodium phosphate peak is greater than 1.5, which shows that the method has good specificity
II, recovery rate test:
Accurately weighing 20mg of nicotinamide control substance, placing in a 200ml measuring flask, dissolving with water, and diluting to scale to obtain 0.1mg/ml nicotinamide control substance solution; respectively taking 16mg, 20mg and 24mg of nicotinamide raw materials into a 200ml measuring flask, respectively adding 8mg of blank raw and auxiliary materials except for nicotinamide, dissolving with water, diluting to a scale, shaking up to obtain nicotinamide test solution, preparing 3 parts of nicotinamide test solution in parallel at each concentration, testing text conditions, and calculating the recovery rate according to the following formula:
The results of the recovery test are shown in table 1.
table 1: results of recovery test
The result shows that the relative standard deviation RSD of the recovery rate is less than 2 percent, and the recovery rate of the nicotinamide content measured by the method is good.
Thirdly, linear test:
Accurately measuring 20mg of a nicotinamide reference substance, putting the nicotinamide reference substance into a 20ml measuring flask, dissolving the nicotinamide reference substance with water and diluting the nicotinamide reference substance to a scale, taking a reference substance stock solution, respectively and accurately measuring 1ml, 3ml, 4ml, 5ml and 6ml of the stock solution, putting the stock solution into a 50ml measuring flask, diluting the stock solution to a constant volume to a scale with water, and testing according to the text chromatographic conditions, wherein the results are shown in table 2:
Table 2: results of the Linear test
And (3) drawing a standard curve by taking the peak area as a vertical coordinate and the sample concentration as a horizontal coordinate to obtain a graph 3, wherein the regression equation is as follows: y 467.2243x + 0.0554; r ═ 1.0000.
as can be seen from the linear relationship chart in FIG. 3, nicotinamide has a good linear relationship in the range of 0.02-0.12 mg.
fourthly, testing the precision of the instrument:
The nicotinamide control solution was sampled 6 times, 20. mu.l each time, and tested according to the text chromatographic conditions, and the results are shown in Table 3:
Table 3: results of instrumental precision test
The result shows that the relative standard deviation RSD of the peak area is less than 2.0 percent, and the precision is good.
Fifthly, repeatability test:
6 parts of dexamethasone sodium phosphate injection sample is precisely measured and tested according to a text content determination method, and the result is shown in table 4:
table 4: results of the repeatability test
The results show that the relative standard deviation RSD of the nicotinamide content is less than 2.0% (n ═ 6) and that the reproducibility is good.
Sixthly, intermediate precision test:
the same repetitive operation is carried out, another experimenter is used for operating, 6 parts of dexamethasone sodium phosphate injection sample is precisely measured, the dexamethasone sodium phosphate injection sample is tested according to the text content determination method, the relative standard deviation of 12 parts of sample is compared, and the result is shown in a table 5:
table 5: results of intermediate precision test
the results show that the relative standard deviation RSD of the nicotinamide content is less than 2.0% (n-12) and that the intermediate precision is good.
seventhly, testing the stability of the solution:
taking the sample solution 1 under the repeatability item, placing the sample solution at room temperature for 24 hours, sampling the sample solution at 0h, 2h, 6h, 8h, 12h and 24h, injecting the sample solution into a liquid chromatograph, recording peak areas, and obtaining results shown in table 5:
table 5: results of stability test
the results show that at 24 hours at room temperature, the relative standard deviation RSD of the nicotinamide content is less than 2%, which indicates that the nicotinamide test solution is stable at room temperature within 24 hours.
eighthly, durability test:
Taking the sample solution 2 under the repeatability item, finely adjusting the chromatographic conditions as shown in Table 6, respectively carrying out sample injection detection, recording peak areas and calculating the sample content, wherein the results are shown in Table 7.
table 6: durability to fine tune chromatographic conditions
| Chromatographic parameters | Adjustment scheme |
| Flow rate of flow | 1.0±0.1ml/min |
| Column temperature | 30℃±5℃ |
| Flow phase ratio | ±2％ |
| chromatographic column | Using different chromatographic columns |
| replacing instrument | Selecting different liquid chromatographs |
Table 7: durability test results:
The results show that the RSD of the nicotinamide content is 0.3% and less than 2.0% before and after fine adjustment of chromatographic conditions, which indicates that the durability of the method for detecting the nicotinamide content is good.
The test results show that the detection method for nicotinamide in dexamethasone sodium phosphate injection provided by the embodiment is stable and reliable, has strong specificity, and can effectively control the product quality.
the features of the embodiments and embodiments described herein above may be combined with each other without conflict.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. The quality standard detection method of the dexamethasone sodium phosphate injection is characterized by comprising the following steps:
s1, preparing a control solution: weighing a nicotinamide reference substance, and dissolving the nicotinamide reference substance in water to prepare a nicotinamide reference substance solution;
S2, preparing a test solution: measuring the dexamethasone sodium phosphate injection to be detected, adding water to dissolve the dexamethasone sodium phosphate injection to prepare a nicotinamide test solution, wherein the content of nicotinamide in the dexamethasone sodium phosphate injection is equal to the mass of the nicotinamide reference substance in the step S1, and the concentration of the nicotinamide test solution is equal to that of the nicotinamide reference substance solution;
S3, preparing a system adaptive solution: measuring dexamethasone sodium phosphate injection, and adding water to dilute to prepare solution A; weighing a nicotinic acid reference substance, and adding water to dissolve the nicotinic acid reference substance to prepare a solution B; respectively measuring the solution A and the solution B, and adding water to dilute to prepare a mixed solution containing nicotinic acid and nicotinamide;
s4, injecting the mixed solution prepared in the step S3 into a liquid chromatograph for detection, and if the separation degree of the nicotinamide and the nicotinic acid is not less than 3.0 and the theoretical plate number is not less than 2000 calculated according to the nicotinamide, performing the step S5;
s5, respectively measuring the nicotinamide reference solution and the nicotinamide test solution, injecting into a liquid chromatograph, and detecting to obtain the content of nicotinamide in the nicotinamide test solution.
2. The method for detecting the quality standard of the dexamethasone sodium phosphate injection according to claim 1, wherein the concentration of the nicotinamide control solution is 0.1mg/ml, and the concentration of the nicotinamide test solution is 0.1 mg/ml.
3. the method for detecting the quality standard of the dexamethasone sodium phosphate injection according to claim 1, wherein each 1ml of the solution A contains 2mg of nicotinamide, each 1ml of the solution B contains 1mg of nicotinic acid, and each 1ml of the mixed solution contains 20 μ g of nicotinic acid and 100 μ g of nicotinamide.
4. The method for detecting the quality standard of the dexamethasone sodium phosphate injection according to claim 1, wherein in the steps S4 and S5, the setting conditions of the liquid chromatograph are as follows: octadecylsilane chemically bonded silica is used as a filling agent; taking a methanol-0.005M sodium heptanesulfonate solution as a mobile phase, wherein the volume ratio of the methanol to the sodium heptanesulfonate solution is 30: 70; the detection wavelength is 262 nm; the flow rate is 1.0 ml/min; the column temperature was 30 ℃.
5. The quality standard of dexamethasone sodium phosphate injection is characterized in that the dexamethasone sodium phosphate injection is judged to be qualified when the nicotinamide content in the nicotinamide test solution is 90.0% -110.0% according to the quality standard detection method of claim 1; and when the content of the nicotinamide in the nicotinamide test solution is lower than 90.0%, judging that the dexamethasone sodium phosphate injection is an unqualified product.
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