CN110146604A - The analysis method of low content sodium pyrosulfite in a kind of measurement sustained release pharmaceutical formulation - Google Patents
The analysis method of low content sodium pyrosulfite in a kind of measurement sustained release pharmaceutical formulation Download PDFInfo
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- CN110146604A CN110146604A CN201910317617.9A CN201910317617A CN110146604A CN 110146604 A CN110146604 A CN 110146604A CN 201910317617 A CN201910317617 A CN 201910317617A CN 110146604 A CN110146604 A CN 110146604A
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- sodium pyrosulfite
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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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Abstract
The invention discloses a kind of analysis methods of low content sodium pyrosulfite in measurement sustained release pharmaceutical formulation, the following steps are included: sustained release tablets to be measured are set in a measuring bottle first, organic solvent such as methanol ultrasound is subsequently added into be disintegrated, it is settled to scale with organic solvent (methanol) and water mixed solution again, centrifuging and taking supernatant is analyzed as test sample；Using liquid chromatography analysis test sample, start chromatography collecting computer system acquisition data；Sodium pyrosulfite reference substance is taken, reference substance solution is prepared with the mixed solution of organic solvent (methanol) and water, while carrying out liquid-phase chromatographic analysis, then calculates the content of sodium pyrosulfite in sustained release tablets.The advantages of present invention has specificity strong, and analysis is quick, strong interference immunity, high sensitivity.
Description
Technical field
Present invention relates particularly to a kind of analysis method, the coke of low content is sub- in quick and convenient measurement measurement sustained release pharmaceutical formulation
Sodium sulphate.
Background technique
Sodium pyrosulfite has application in oral, injection and topical preparation as antioxidant.For pyrosulfurous acid
The sterling of sodium measures, and uses titration method in pharmacopeia, such as: in Chinese Pharmacopoeia 2015 editions, containing for sodium pyrosulfite is measured
The method of determining is that sodium pyrosulfite and iodine solution are carried out redox reaction, and remaining iodine is titrated with sodium thiosulfate, root
The amount of sodium thiosulfate is calculated according to the iodine of consumption.This method specificity is poor, and sensitivity is low, needs sample size big, is only applicable in
In the macro-analysis of sterling.In addition, there is document report to go out SO according to what sodium pyrosulfite released in acidity is molten2, and SO2?
It can make the practical colour fading of basic fuchsin and aubergine complex of the generation with quinone structure under the existing acid condition for having EDTA,
Measurement calculates the content of sodium pyrosulfite from outer absorbance value by external standard method at 557nm wavelength.The colorimetric method specificity
It is good, high sensitivity, but be applicable in only for injection and simple compound preparation etc., for containing polymer such as hydroxypropyl methylcelluloses
Sustained release preparation for, the polymer such as process auxiliary material hydroxypropyl methylcellulose that the method prepares sample easily form gel, influence coke
The extraction of sodium sulfite.
Summary of the invention
The purpose of the present invention is to overcome the above shortcomings, provide it is a kind of analysis quickly, strong interference immunity, high sensitivity
Measurement sustained release pharmaceutical formulation in low content sodium pyrosulfite analysis method.
The purpose of the present invention is achieved through the following technical solutions: low content coke sulfurous in a kind of measurement sustained release pharmaceutical formulation
The analysis method of sour sodium, comprising the following steps:
A, test sample is set in a measuring bottle, organic solvent ultrasound is added to being disintegrated, lets cool to room temperature；
B, it is settled to scale with the mixed solution of organic solvent and water, be centrifuged, supernatant is taken to analyze as test sample；
C, using liquid chromatography analysis test sample, while starting chromatography collecting computer system acquisition data；
D, using sodium pyrosulfite as reference substance, it is configured to reference substance solution with the mixed solution of organic solvent and water, simultaneously
Liquid-phase chromatographic analysis is carried out, the content of sodium pyrosulfite in test sample is calculated using external standard method, liquid phase chromatography analytical method: being used
The sulfuric acid solution of 0.01N includes: chromatographic column as mobile phase, chromatographic condition: filler is the stryrene divinyl of sulfonation crosslinking
Base co-polymer cation exchange resin, column length 300mm, internal diameter 8.0mm；1.0 ml/min of flow velocity；Detection wavelength 200nm；Into
50 μ L of sample volume, column temperature: 50-60 °C；Analysis time: 16 minutes.
Organic solvent mentioned above is methanol.In addition, the sodium pyrosulfite in test sample can extract completely, test solution
Prepare not by the interference of the polymer such as auxiliary material hydroxypropyl methylcellulose.
Compared with the prior art, the present invention has the following advantages:
The present invention realize in sustained release pharmaceutical formulation carry out quickly, facilitate analysis low content sodium pyrosulfite, have realistic meaning,
The method that the present invention measures sodium pyrosulfite with the extraction of organic solvent combination water, with efficient liquid phase for the first time removes hypromellose
It is interfered caused by the polymer such as element, present invention analysis is quick, strong interference immunity, high sensitivity.
Detailed description of the invention:
Fig. 1 is solvent blank solution chromatogram；
Fig. 2 is reference substance chromatogram；
Fig. 3 is the sample chromatogram figure of embodiment one；
Fig. 4 is the sample chromatogram figure of embodiment two；
Specific embodiment:
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be to the skill in the embodiment of the present invention
Art scheme is clearly and completely described, it is clear that and described embodiment is a module embodiments of the invention, rather than all
Embodiment.The elements and features described in one embodiment of the invention can be with one or more other embodiment party
Elements and features shown in formula combine.It should be noted that being omitted for purposes of clarity, in explanation unrelated to the invention
, the expression and description of component known to persons of ordinary skill in the art and processing.Based on the embodiments of the present invention, this field
Those of ordinary skill's every other embodiment obtained under the premise of not making the creative labor, belongs to guarantor of the present invention
The range of shield.
The analysis method of low content sodium pyrosulfite in a kind of measurement sustained release pharmaceutical formulation, comprising the following steps: first will
Sustained release tablets to be measured are set in a measuring bottle, are subsequently added into organic solvent such as methanol ultrasound and are disintegrated, then mixed with organic solvent (methanol) and water
It closes solution and is settled to scale, centrifuging and taking supernatant is analyzed as test sample；Using liquid chromatography analysis test sample, start chromatography
Collecting computer system acquisition data；Sodium pyrosulfite reference substance is taken, is prepared with the mixed solution of organic solvent (methanol) and water
Reference substance solution, while liquid-phase chromatographic analysis is carried out, then calculate the content of sodium pyrosulfite in sustained release tablets.
Embodiment one
Sodium pyrosulfite assay in body of Pramipexole dihydrochloride sustained release tablets (specification: 0.375mg):
The theoretical content of sodium pyrosulfite is 0.92mg in the piece, accounts for the 0.4% of entire slice weight.
(1), instrument and condition:
Liquid phase chromatography: 1200 chromatographic system of U.S.'s Agilent and work station；
Chromatographic column: Japanese Showa carbohydrate column, SH1011,300 mm of column length, 8.0 mm of internal diameter；
Flow velocity: 1.0 milliliters per minute；
Detection wavelength: 200 nm of UV；
Sampling volume: 50 μ L；
Column temperature: 50 DEG C；
Analysis time: 16 minutes.
(2), experimental procedure:
The preparation (sulfuric acid of 0.01 N) of mobile phase:
Amount weighs 0.3 milliliter of sulfuric acid dissolution in 1 liter of water, shakes up.
The preparation of test solution:
About 5 body of Pramipexole dihydrochloride sustained release tablets are shifted into the measuring bottle of a 200ml, the methanol solution of 120ml is added to the measuring bottle
In, ultrasound is disintegrated piece completely, lets cool to room temperature, is settled to scale with methanol and water mixed liquid (1:1).Take part
Solution is centrifuged 5 minutes under 4000 turns again, and supernatant is taken to analyze as test sample；
The preparation of reference substance solution:
Precision weighs sodium pyrosulfite standard items 23mg into 100ml measuring bottle, is settled to quarter than water (4:1) mixed solution with methanol
Degree.The solution is reference substance stock solution.It measures in above-mentioned reference substance stock solution 5ml to 50 milliliters of measuring bottle, is mixed with methanol: water
It closes solution and is diluted to scale, shake up.
Methodological study:
Sample introduction reproducibility: reference substance solution is taken continuously into 6 needles, to calculate the %RSD, % in the peak face for the chromatographic peak that sodium pyrosulfite generates
RSD is respectively less than 5, and the precision of illustration method is good.
Specificity: in reference substance solution, the retention time for the chromatographic peak that sodium pyrosulfite generates is 10.023 minutes；Blank
Solution and blank auxiliary are interference in this retention time.
The rate of recovery: the rate of recovery under three kinds of concentration levels is examined, as a result within the scope of 95.0%-105.0%.
Repeatability: 6 parts of samples are prepared in parallel, the %RSD of sodium pyrosulfite measurement result is less than 3.
Measurement result:
Pyrosulfurous acid sodium content is 98.6% in the body of Pramipexole dihydrochloride sustained release tablets (specification: 0.375mg).
Embodiment two
Sodium pyrosulfite assay in body of Pramipexole dihydrochloride sustained release tablets (specification: 0.375mg):
The theoretical content of sodium pyrosulfite is 0.46mg in the piece, accounts for the 0.2% of entire slice weight.
(1), instrument and condition:
Liquid phase chromatography: 1200 chromatographic system of U.S.'s Agilent and work station；
Chromatographic column: Japanese Showa carbohydrate column, SH1011,300 mm of column length, 8.0 mm of internal diameter；
Flow velocity: 1.0 milliliters per minute；
Detection wavelength: 200 nm of UV；
Sampling volume: 50 μ L；
Column temperature: 50 DEG C；
Analysis time: 16 minutes.
(2), experimental procedure:
The preparation (sulfuric acid of 0.01 N) of mobile phase:
Amount weighs 0.3 milliliter of sulfuric acid dissolution in 1 liter of water, shakes up.
The preparation of test solution:
About 5 body of Pramipexole dihydrochloride sustained release tablets are shifted into the measuring bottle of a 200ml, the methanol solution of 120ml is added to the measuring bottle
In, ultrasound is disintegrated piece completely, lets cool to room temperature, is settled to scale with methanol and water mixed liquid (1:1).Take part
Solution is centrifuged 5 minutes under 4000 turns again, and supernatant is taken to analyze as test sample；
The preparation of reference substance solution:
Precision weighs sodium pyrosulfite standard items 23mg into 100ml measuring bottle, is settled to quarter than water (4:1) mixed solution with methanol
Degree.The solution is reference substance stock solution.It measures in above-mentioned reference substance stock solution 5ml to 50 milliliters of measuring bottle, is mixed with methanol: water
It closes solution and is diluted to scale, shake up.
System suitability:
Reference substance solution is taken continuously into 5 needles, to calculate the %RSD for the chromatographic peak that sodium pyrosulfite generates, %RSD is respectively less than 5%, meets
It is required that；
Measurement result:
Pyrosulfurous acid sodium content is 98.0% in the body of Pramipexole dihydrochloride sustained release tablets (specification: 0.375mg).
The present invention solves the measurement in sustained release pharmaceutical formulation in low content sodium pyrosulfite.The present invention has specificity
By force, the advantages of analysis is quick, strong interference immunity, high sensitivity.
Finally, it should be noted that although the present invention and its advantage have been described in detail above it should be appreciated that not
Can be carried out in the case where beyond the spirit and scope of the present invention being defined by the claims appended hereto various changes, substitution and
Transformation.Moreover, the scope of the present invention is not limited only to the specific reality of process, equipment described in specification, means, method and steps
Apply example.One of ordinary skilled in the art holds from the disclosure it will be readily understood that can be used according to the present invention
The row function essentially identical to corresponding embodiment described herein obtains the result essentially identical with it, existing and future
Process, equipment, means, method or step to be developed.Therefore, the attached claims are intended to wrap in the range of them
Include such process, equipment, means, method or step.
Claims (2)
1. the analysis method of low content sodium pyrosulfite in a kind of measurement sustained release pharmaceutical formulation, it is characterised in that: including following step
It is rapid:
A, test sample is set in a measuring bottle, organic solvent ultrasound is added to being disintegrated, lets cool to room temperature；
B, it is settled to scale with the mixed solution of organic solvent and water, be centrifuged, supernatant is taken to analyze as test sample；
C, using liquid chromatography analysis test sample, while starting chromatography collecting computer system acquisition data；
D, using sodium pyrosulfite as reference substance, it is configured to reference substance solution with the mixed solution of organic solvent and water, simultaneously
Liquid-phase chromatographic analysis is carried out, the content of sodium pyrosulfite in test sample is calculated using external standard method, liquid phase chromatography analytical method: being used
The sulfuric acid solution of 0.01N includes: chromatographic column as mobile phase, chromatographic condition: filler is the stryrene divinyl of sulfonation crosslinking
Base co-polymer cation exchange resin, column length 300mm, internal diameter 8.0mm；1.0 ml/min of flow velocity；Detection wavelength 200nm；Into
50 μ L of sample volume, column temperature: 50-60 DEG C；Analysis time: 16 minutes.
2. a kind of analysis method for measuring low content sodium pyrosulfite in sustained release pharmaceutical formulation according to claim 1, special
Sign is: the organic solvent is methanol.
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| CN112326808A (en) * | 2020-09-24 | 2021-02-05 | 南京斯泰尔医药科技有限公司 | Method for determining content of sodium metabisulfite in injection |
| CN113155990A (en) * | 2021-02-24 | 2021-07-23 | 西南药业股份有限公司 | Extraction solvent and extraction method of main drug components in codeine phosphate sustained-release tablets |
| CN113655146A (en) * | 2021-08-17 | 2021-11-16 | 南京恒道医药科技有限公司 | Method for determining content of water-soluble antioxidants sodium bisulfite, sodium sulfite and sodium metabisulfite in preparation by HPLC |
| CN115248141A (en) * | 2021-04-28 | 2022-10-28 | 北京泰德制药股份有限公司 | Method for preparing detection sample of sustained-release pharmaceutical composition |
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| CN115248141A (en) * | 2021-04-28 | 2022-10-28 | 北京泰德制药股份有限公司 | Method for preparing detection sample of sustained-release pharmaceutical composition |
| CN113655146A (en) * | 2021-08-17 | 2021-11-16 | 南京恒道医药科技有限公司 | Method for determining content of water-soluble antioxidants sodium bisulfite, sodium sulfite and sodium metabisulfite in preparation by HPLC |
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