CN109239223A - A kind of test method for Capsules acetic acid - Google Patents
A kind of test method for Capsules acetic acid Download PDFInfo
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- CN109239223A CN109239223A CN201811189211.9A CN201811189211A CN109239223A CN 109239223 A CN109239223 A CN 109239223A CN 201811189211 A CN201811189211 A CN 201811189211A CN 109239223 A CN109239223 A CN 109239223A
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- acetic acid
- capsules
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- test
- test method
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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
-
- 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
-
- 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
- G01N30/14—Preparation by elimination of some components
-
- 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
-
- 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
- G01N30/14—Preparation by elimination of some components
- G01N2030/146—Preparation by elimination of some components using membranes
Abstract
The invention discloses a kind of test methods for Capsules acetic acid.This method weighs Capsules to be measured, and capsule is shredded；Purified water is added into the capsule shredded, shaking makes it dissolve；Glue after dissolution is placed in a centrifuge, supernatant liquor is taken after centrifugation, through polyamide column decolorization, measures acetic acid through high performance liquid chromatography after filtering.Compared with prior art, test method of the present invention is flexible and convenient, can be tested, and do not need special device for each Capsules, be suitble to the quick test of acetic acid in Capsules.
Description
Technical field
The invention belongs to medicine capsule preparation technical fields, and in particular to a kind of survey for Capsules acetic acid
Method for testing.
Background technique
Capsules are one of major auxiliary burdens of capsule, and Capsules are with gelatin or cellulose etc. for major ingredient, are added
The auxiliary materials such as stabilizer, plasticizer, pigment, are process by special process.Gelatin is by the tissue such as muscle, bone, skin of animal
Collagen boils, and collagen is subject to infecting to external microbe, therefore Capsules microbiological indicator
Control is an important problem.
Traditional Capsules sterilizing methods are sterilized with ethylene oxide gas, the operation of eo sterilization method
Convenient, sterilization effect is good, but its degradation time is long, and there are also certain toxicity, excessive ethylene oxide can not only cause in acute
Poison also has and causes allergy, mutagenesis and carcinogenesis.Therefore, we have developed new capsule sterile production techniques, in capsule
A certain amount of glacial acetic acid is added in production process, inhibits the growth of microorganism.Acetic acid belongs to third class organic solvent, needs to carry out
Remain quantity research.
It is few for acetic acid in existing residual solvent detection method, and without residual for the acetic acid in Capsules
The detection method stayed.Such as No. 201610113454.9 patents of application number, discloses a kind of while detecting residual solvent acetic acid and second
The method of acetoacetic ester, this method use gas chromatography, and pre-treatment is more troublesome, and grope by us, gas chromatography
Carry out Capsules in acetic acid residue detection reproducibility it is bad, since residual quantity is relatively low, often can not appearance, therefore we
Again the Capsules acetic acid method for detecting residue based on high performance liquid chromatography is developed.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the present invention is to provide a kind of surveys for Capsules acetic acid
Method for testing, this method is simple, and pre-treatment is few, and property is high again, and result is accurate.
A kind of test method for Capsules acetic acid, weighs Capsules to be measured, capsule is shredded；To cutting
Purified water is added in broken capsule, shaking makes it dissolve；Glue after dissolution is placed in a centrifuge, supernatant liquor is taken after centrifugation,
Through polyamide column decolorization, acetic acid is measured through high performance liquid chromatography after filtering.
The above-mentioned test method for Capsules acetic acid, the specific steps are as follows:
The first step weighs 1.0g Capsules to be measured and shreds, is placed in 50ml centrifuge tube, and 20ml purified water, vibration are added thereto
It shakes and is allowed to dissolve, centrifuge tube is symmetrically put into a centrifuge to centrifugation, takes supernatant liquor, after polyamide column sloughs pigment, warp
0.45 μm of membrane filtration, takes subsequent filtrate 2mL as test solution；
Second step, precision measure glacial acetic acid 5ml in 1000ml volumetric flask, add purified water dilution to be settled to scale and shake up, are made
The reference substance stock solution that volume fraction is 0.5%；
Third step, it is accurate respectively to measure the reference substance stock solution that volume fraction is 1.0,1.5,2.0,2.5,3.0,3.5ml 0.5%
In the volumetric flask of 50ml, and it is diluted with water to scale, respectively takes above-mentioned solution 2ml, through 0.45 μm of membrane filtration, using efficient
Liquid chromatogram is measured, and using peak area as ordinate, is established standard curve by abscissa of concentration, is calculated regression equation；
4th step, the 4th step are to carry out test test sample under chromatographic column according to ZOBAX SB-C18, obtain sample peak area, generation
Enter regression equation, obtains the concentration of test sample, acetic acid contentC in formulaTest sample: pass through linear regression
The concentration of acetic acid in the test solution that equation calculation obtains；M: test sample quality.
It is that the Capsules are gelatin hollow capsule, enteric gelatin hollow capsule, hypromellose as improved
Plain Capsules, enteric hydroxypropyl methylcellulose Capsules or pulullan polysaccharide empty capsule.
It is that the revolving speed of centrifuge is 10000rpm/min in the first step as improved.
It is flow velocity 0.8-1.0ml/min, sample volume 10-20 μ l when the 4th step high performance liquid chromatography measures as improved,
Detection wavelength 205-220nm.
The utility model has the advantages that
Compared with prior art, test method of the present invention is flexible and convenient, can be tested for each Capsules, and not
Special device is needed, the quick test of acetic acid in Capsules is suitble to.
Detailed description of the invention
Fig. 1 is the chromatogram of glacial acetic acid in embodiment 1；
Fig. 2 is linear relationship figure in embodiment 2；
Fig. 3 is that durability verifying changes the chromatogram after flow velocity in embodiment 2；
Fig. 4 is that durability verifying changes the chromatogram after column temperature in embodiment 2；
Fig. 5 is the chromatogram of test sample in embodiment 3.
Specific embodiment
The present invention is further described in detail below by specific embodiment.
Embodiment 1
Glacial acetic acid 5ml is taken, purified water is added to be settled to 1000ml, precision measures above-mentioned solution 5ml, through filtering with microporous membrane, according to
ZOBAX SB-C18(4.6 × 150mm, 5um) chromatographic column；Mobile phase is that (sodium hydroxide is molten for (5%) -0.07% phosphoric acid solution of methanol
Liquid is adjusted to pH3.0) (95%)；Flow velocity 1.0ml/min；20 μ l of sample volume；The chromatographic condition of Detection wavelength 215nm is detected,
The retention time at the peak of acetic acid is obtained as 2.956min, symmetrical factor 0.6524, tailing factor 1.4198 is shown in Fig. 1.
Embodiment 2
The verifying of acetic acid detection method
Liquid phase chromatogram condition: Agilent ZOBAX SB-C18(4.6 × 150mm, 5um) chromatographic column；Mobile phase is methanol (5%)-
0.07% phosphoric acid solution (sodium hydroxide solution is adjusted to pH3.0) (95%)；Flow velocity 1.0ml/min；10 μ l of sample volume；Detect wave
Long 210nm.
(1) system suitability: precision measure 1ml reference substance solution, be transferred in sample bottle, according to above-mentioned chromatographic condition into
Row measurement；Continuous sample introduction 5 times, with calculated by peak area theoretical cam curve > 1000 of acetic acid, reference substance solution continuous sample introduction 5 times,
RSD≤10% of gained peak retention time, tailing factor≤2.0 of main peak.
(2) specificity: sample introduction blank solution, test solution, reference substance solution, control are distinguished according to above-mentioned chromatographic condition
Target peak is nearby without adjacent peak in product and test solution map, and target peak goes out peak position nearby without significant in blank solution map
Interference Peaks.
(3) linear, quantitative limit, detection limit: it is accurate respectively measure 1.5,2.0,2.5,3.0,3.5ml reference substance solution in
In 5ml volumetric flask, three parts of each concentration is diluted with water to scale respectively.It is measured according to chromatographic condition, is vertical with peak area
Coordinate is that abscissa establishes standard curve with concentration (μ g/ml), calculates regression equation, obtain equation of linear regression y=
1793.9x-2.0728, linearly dependent coefficient R2=0.9999, see Fig. 2；Quantitative limit are as follows: 0.0090%；Detection is limited to: 0.0027%.
(4) precision: reference substance solution is taken, continuous sample introduction six times, peak area RSD is less than 10%.
(5) accuracy: using mark-on reclaims method, with test sample concentration for 100%, adds 80%, 100% and 120% respectively
The reference substance solution of concentration, equal proportion mix, and test sample concentration calculates the rate of recovery, and the rate of recovery is between 80-120%.
(6) durability: changing the column temperature and flow velocity in instrumental method, and inspection result is not influenced by small variations, full
The requirement of pedal system adaptability, as a result as shown in Figure 3 and Figure 4.
Embodiment 3
1.0g test sample is weighed, test sample is shredded and is placed in 50ml centrifuge tube, 20ml purified water is added thereto.Shaking is allowed to
Dissolution；
Centrifuge tube is symmetrically put into a centrifuge, 10000rpm/min is centrifuged 10min；
Supernatant liquor is taken, sloughs pigment through polyamide column, then through 0.45 μm of membrane filtration, take subsequent filtrate 2ml molten as test sample
Liquid；
Test sample is tested according to high performance liquid chromatography, as a result as shown in Figure 5.
It is low in cost by above-mentioned test it is found that test method of the present invention is simple and easy, as a result accurately.
The foregoing is only a preferred embodiment of the present invention, the scope of protection of the present invention is not limited to this, it is any ripe
Know those skilled in the art within the technical scope of the present disclosure, the letter for the technical solution that can be become apparent to
Altered or equivalence replacement are fallen within the protection scope of the present invention.
Claims (5)
1. a kind of test method for Capsules acetic acid, which is characterized in that Capsules to be measured are weighed, by capsule
It shreds；Purified water is added into the capsule shredded, shaking makes it dissolve；Glue after dissolution is placed in a centrifuge, is taken after centrifugation
Supernatant liquor measures acetic acid through high performance liquid chromatography after filtering through polyamide column decolorization.
2. the test method according to claim 1 for Capsules acetic acid, which is characterized in that the first step,
It weighing 1.0g Capsules to be measured to shred, be placed in 50ml centrifuge tube, 20ml purified water is added thereto, shaking is allowed to dissolve,
Centrifuge tube is symmetrically put into a centrifuge to centrifugation, takes supernatant liquor, after polyamide column sloughs pigment, through 0.45 μm of filter membrane mistake
Filter, takes subsequent filtrate 2mL as test solution；Second step, precision measure glacial acetic acid 5ml in 1000ml volumetric flask, add purifying
Water dilution is settled to scale and shakes up, and the reference substance stock solution that volume fraction is 0.5% is made；Third step, it is accurate respectively to measure volume
Score is 1.0,1.5,2.0,2.5,3.0, the reference substance stock solution of 3.5ml 0.5% is diluted with water in the volumetric flask of 50ml
To scale, above-mentioned solution 2ml is respectively taken, through 0.45 μm of membrane filtration, is measured using high performance liquid chromatography, is with peak area
Ordinate establishes standard curve by abscissa of concentration, calculates regression equation；4th step is chromatography according to ZOBAX SB-C18
Column tests test sample, obtains sample peak area, substitutes into regression equation, obtains the concentration of test sample, acetic acid contentC in formulaTest sample: the concentration of acetic acid in the test solution being calculated by equation of linear regression；
M: test sample quality.
3. the test method according to claim 2 for Capsules acetic acid, which is characterized in that the sky
Heart-soothing capsule is gelatin hollow capsule, enteric gelatin hollow capsule, hydroxypropyl methylcellulose Capsules, enteric hydroxypropyl methylcellulose sky
Heart-soothing capsule or pulullan polysaccharide empty capsule.
4. the test method according to claim 2 for Capsules acetic acid, which is characterized in that in the first step
The revolving speed of centrifuge is 10000rpm/min.
5. the test method according to claim 2 for Capsules acetic acid, which is characterized in that the 4th step is high
Flow velocity 0.8-1.0ml/min, sample volume 10-20 μ l, Detection wavelength 205-220nm when effect liquid phase chromatogram measures.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811189211.9A CN109239223B (en) | 2018-10-12 | 2018-10-12 | Method for testing acetic acid residual quantity of empty capsules |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811189211.9A CN109239223B (en) | 2018-10-12 | 2018-10-12 | Method for testing acetic acid residual quantity of empty capsules |
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| Publication Number | Publication Date |
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| CN109239223A true CN109239223A (en) | 2019-01-18 |
| CN109239223B CN109239223B (en) | 2021-11-30 |
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| CN201811189211.9A Active CN109239223B (en) | 2018-10-12 | 2018-10-12 | Method for testing acetic acid residual quantity of empty capsules |
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| GB1093286A (en) * | 1965-02-15 | 1967-11-29 | Biorex Laboratories Ltd | Improvements in or relating to dosage unit forms for the administration of medicaments and diagnostic agents |
| US3625353A (en) * | 1969-02-19 | 1971-12-07 | Jintan Terumo Co | Package for sterilized articles |
| CN103983728A (en) * | 2014-06-06 | 2014-08-13 | 江苏宝众宝达药业有限公司 | Method for measuring residual acetic acid in flubendazole crude drug by high performance liquid chromatography method |
| CN105699533A (en) * | 2016-03-01 | 2016-06-22 | 山东新时代药业有限公司 | Method for simultaneously detecting acetic acid and ethyl acetate in residual solvent |
| CN107505407A (en) * | 2017-07-19 | 2017-12-22 | 贵州茅台酒股份有限公司 | It is a kind of while determine lactic acid in white wine fermented grain, the method for acetic acid content |
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| US3625353A (en) * | 1969-02-19 | 1971-12-07 | Jintan Terumo Co | Package for sterilized articles |
| CN103983728A (en) * | 2014-06-06 | 2014-08-13 | 江苏宝众宝达药业有限公司 | Method for measuring residual acetic acid in flubendazole crude drug by high performance liquid chromatography method |
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