CN105158167A - Method for measuring content of mannitol injection - Google Patents
Method for measuring content of mannitol injection Download PDFInfo
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- CN105158167A CN105158167A CN201510695076.5A CN201510695076A CN105158167A CN 105158167 A CN105158167 A CN 105158167A CN 201510695076 A CN201510695076 A CN 201510695076A CN 105158167 A CN105158167 A CN 105158167A
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- China
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- final product
- sulfuric acid
- shake
- mannitol injection
- ammonium molybdate
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Abstract
The invention discloses an improved method for measuring the content of mannitol injection. The content of mannitol injection is measured through an optical rotation measuring method, operation is easy, time is saved, production cost is reduced, economic benefits are improved, medicine is effectively prevented from being contaminated, and safety risks of medicine (intermediate products) are reduced. Compared with the prior measuring art, the method is more suitable for measuring the content of intermediate products in the production process of medicine preparing enterprises.
Description
Technical field
The present invention relates to pharmaceutical preparation inspection technology field, be specifically related to a kind of assay method of formula mannitol injection liquid content.
Background technology
Sweet mellow wine, chemical name: D-mannital, molecular formula: C
6h
14o
6, molecular weight: 182.17.Formula mannitol injection liquid is the sterile water solution of sweet mellow wine, containing sweet mellow wine (C
6h
14o
6) should be the 95.0-105.0% of labelled amount, be dehydrant.
" Chinese Pharmacopoeia " version in 2010 two, disclose sweet mellow wine and formula mannitol injection liquid content assaying method, sweet mellow wine (raw material) content assaying method is: get this product and be about 0.2g, accurately weighed, put in 250ml measuring bottle, add water and make dissolving and be diluted to scale, shake up, precision measures 10ml, put in iodine flask, precision adds sodium periodate solution (get sulfuric acid solution (1 → 20) 90ml and sodium periodate solution (2.3 → 1000) 110ml is mixed) 50ml, put in water-bath and heat 15 minutes, let cool, add potassium iodide test solution 10ml, close plug, place 5 minutes, with sodium thiosulfate vs (0.05mol/L) titration, during to nearly terminal, add starch indicator solution 1ml, continue to be titrated to blue disappearance, and titration results blank test is corrected, the sodium thiosulfate vs (0.05mol/L) of every 1ml is equivalent to the C of 0.9109mg
6h
14o
6, formula mannitol injection liquid content assaying method is: measure according to high performance liquid chromatography (QJ/ZG-004).The SDVB multipolymer that chromatographic condition and system suitability sulfonation are cross-linked is the strong cation calcium exchange column (or separation efficiency suitable chromatographic column) of filling agent, take water as mobile phase, flow velocity is 0.5ml per minute, column temperature is 80 DEG C, differential refraction detector, detected temperatures is 55 DEG C.Separately get sweet mellow wine and each 0.5g of sorbierite, put in 100ml measuring bottle, be dissolved in water and be diluted to scale, shaking up, get 20 μ l injection liquid chromatographies, record chromatogram, sweet mellow wine and the peak-to-peak degree of separation of sorbierite chromatogram should be greater than 2.0.Precision measures this product appropriate (being about equivalent to sweet mellow wine 5g), and be dissolved in water and quantitatively dilute the solution made containing 5mg in every 1ml, precision measures 20 μ l injection liquid chromatographies, record chromatogram, separately gets sweet mellow wine reference substance, is measured in the same method, by external standard method with calculated by peak area, to obtain final product.
Existing formula mannitol injection liquid content assaying method, statutory standards, pharmaceutical producing enterprise must test to the formula mannitol injection liquid product that dispatches from the factory by statutory standards, and can perform if enterprise oneself innovation content assaying method has to pass through application declaration, this can increase manpower and materials.But along with the development in epoch, the improvement of technology, and the requirement of environmental protection and energy saving, to the improvement of existing medicine detection technique also in the middle of constantly carrying out, improving each time is all constantly perfect to prior art, is also cost-saving accordingly, save time, increase the benefit.
Summary of the invention
The object of the invention is the deficiency in order to solve existing formula mannitol injection liquid content detection technology, one formula mannitol injection liquid content assaying method is fast and effectively provided.
The assay method of a kind of formula mannitol injection liquid content of the present invention, main contents are as follows: sample thief 10ml, put in 250ml measuring bottle, add the ammonium molybdate solution (analyze pure ammonium molybdate 26.6g and be diluted with water to 1000ml) of 200ml2.66%, then add the dilute sulfuric acid (analytical pure sulfuric acid 10ml is diluted to 100ml) of 5ml10%, be diluted with water to scale again, shake up, at 25 DEG C, measure with Optical Rotation, parallel testing two parts
Specifically comprise the steps:
1) prepare before measuring:
1. 2.66% ammonium molybdate solution preparation: precision takes analyzes pure ammonium molybdate 26.6g, adds water and makes to be dissolved into 1000ml, shake up, to obtain final product;
2. 10% dilution heat of sulfuric acid preparation: get analytical pure sulfuric acid 10ml, with water rare one-tenth 100ml, shake up, to obtain final product;
2) test sample preparation:
Under 25 DEG C of environment, get normal temperature sample 10ml, put in 250ml measuring bottle, add 200ml step 1) obtain 2.66% ammonium molybdate solution, then add 5ml step 1) obtain 10% dilute sulfuric acid, then be diluted with water to scale, shake up, to obtain final product;
3) measure:
Step 2) test sample for preparing, at 25 DEG C, measure test sample α value with polarimeter according to Polarimetry, Parallel testing 2 parts,
α1＝，α2＝
Computing formula: sweet mellow wine % (mark)=[(α-0.05688)/2.176] X100%
Calculate measurement result and get final product.
Hydromining prior art standard of the present invention.
Step 1) described in precision take, preferably use ten thousand/analytical balance to take.
Compare with existing formula mannitol injection liquid content assaying method, the present invention has the following advantages:
1, detecting step is simple: existing assay method system carries out according to high performance liquid chromatography, chromatographic condition and system suitability test must be done in mensuration process, mobile phase, sweet mellow wine and sorbitol solution must be prepared, prepare sweet mellow wine reference substance solution and need testing solution again, also will adjust the various processes such as instrument parameter.And the present invention only need prepare need testing solution, the ammonium molybdate solution of 2.66% and the dilution heat of sulfuric acid of 10%, directly measure with polarimeter after preparing need testing solution, operation steps is simple and convenient.
2, measurement result saves time fast: existing assay method is high-performance liquid chromatogram determination method, prepare a series of solution and will spend many time, do chromatographic condition and system suitability also needs about 50 minutes, carry out also needing just can draw testing result in more than 1 hour when test sample detects, this largely have impact on work efficiency, and the present invention adopts polarimeter determination method, before and after mensuration terminates, about 25 minutes are only needed from preparation test sample, this greatly shortens detection time, particularly pharmacy corporation production run intermediate product are detected, only need after preparing liquid just to draw assay result in about 25 minutes.If testing result conforms with the regulations just can carry out filling next step operation such as grade fast.This effectively prevent dosing storage and fills with herb liquid and polluted due to overlong time.And existing determination method needs to wait 2 hours just can draw testing result, liquid medicine contamination may be caused, also have impact on speed of production.
3, save cost, increase economic efficiency: existing determination method instrument is high performance liquid chromatograph, expensive, testing process needs sweet mellow wine reference substance and timing to change chromatographic column, and this also causes the raising of testing cost.And determination method of the present invention adopts polarimeter, itself is cheap, testing process ammonium molybdate used and sulfuric acid market price also lower, this greatly reduces testing cost, improves production economy benefit.
4, measurement result factor is affected less: affecting measurement result factor in existing determination method is: equipment factor, test solution factor, environmental factor, operative skill factor etc., all be difficult to control, very large on testing result impact, and determination method of the present invention has influence on testing result factor simply and easily control, show according to checking, under the same conditions, the testing result adopting determination method of the present invention and existing determination method to draw is basically identical.But change greatly in testing environment humiture, supply voltage be unstable, instrument start service time is longer, after test sample preparation rest time too short (degassed) etc. adopt determination method of the present invention to draw when condition changes testing result is more stable, more accurate.
Embodiment
With embodiment, the invention will be further described below, but the present invention is not limited to these embodiments.
Embodiment:
An assay method for formula mannitol injection liquid content, comprises the steps:
1, prepare before measuring
(1) 2.66% ammonium molybdate solution preparation
Precision takes, and (with ten thousand/analytical balance) analyzes pure ammonium molybdate 26.6g, adds water and makes in right amount to be dissolved into 1000ml, shake up, to obtain final product;
(2) 10% dilution heat of sulfuric acid preparation
Get analytical pure sulfuric acid 10ml with transfer pipet, with water rare one-tenth 100ml, shake up, to obtain final product;
2, test sample preparation
Under 25 DEG C of environment, get normal temperature sample 10ml, put in 250ml measuring bottle, add the ammonium molybdate solution (analyze pure ammonium molybdate 26.6g and be diluted with water to 1000ml) of 200ml2.66%, add the dilute sulfuric acid (analytical pure sulfuric acid 10ml is diluted to 100ml) of 5ml10% again, be diluted with water to scale again, shake up, to obtain final product;
3, measure
(1) the test sample prepared is moved in polarimeter instrument room, at 25 DEG C, measure test sample α value with polarimeter according to Polarimetry, Parallel testing 2 parts;
(2) calculate
By computing formula: sweet mellow wine % (mark)=[(α-0.05688)/2.176] X100%
Calculate measurement result and get final product.
Claims (2)
1. an assay method for formula mannitol injection liquid content, is characterized in that, comprises the steps:
1) prepare before measuring:
1. 2.66% ammonium molybdate solution preparation: precision takes analyzes pure ammonium molybdate 26.6g, adds water and makes to be dissolved into 1000ml, shake up, to obtain final product;
2. 10% dilution heat of sulfuric acid preparation: get analytical pure sulfuric acid 10ml, with water rare one-tenth 100ml, shake up, to obtain final product;
2) test sample preparation:
Under 25 DEG C of environment, get normal temperature sample 10ml, put in 250ml measuring bottle, add 200ml step 1) obtain 2.66% ammonium molybdate solution, then add 5ml step 1) obtain 10% dilute sulfuric acid, then be diluted with water to scale, shake up, to obtain final product;
3) measure:
Step 2) test sample for preparing, at 25 DEG C, measure test sample α value with polarimeter according to Polarimetry, Parallel testing 2 parts,
α1＝，α2＝
Computing formula: sweet mellow wine % (mark)=[(α-0.05688)/2.176] X100%
Calculate measurement result and get final product.
2. the assay method of a kind of formula mannitol injection liquid content according to claim 1, is characterized in that: step 1) described in precision take, take for adopting ten thousand/analytical balance.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510695076.5A CN105158167A (en) | 2015-10-23 | 2015-10-23 | Method for measuring content of mannitol injection |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510695076.5A CN105158167A (en) | 2015-10-23 | 2015-10-23 | Method for measuring content of mannitol injection |
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| CN105158167A true CN105158167A (en) | 2015-12-16 |
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| CN201510695076.5A Pending CN105158167A (en) | 2015-10-23 | 2015-10-23 | Method for measuring content of mannitol injection |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108593646A (en) * | 2018-04-27 | 2018-09-28 | 四川科伦药业股份有限公司 | A kind of rapid detection method of compound formula mannitol injection liquid intermediate mannitol content |
| CN111256792A (en) * | 2020-02-21 | 2020-06-09 | 康立泰药业有限公司 | Method for detecting filling amount of small-volume injection preparation |
| CN114660196A (en) * | 2022-03-18 | 2022-06-24 | 广东大冢制药有限公司 | Method for determining related substances in medicine containing multi-component compound sorbitol solution |
Citations (4)
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|---|---|---|---|---|
| SU388223A1 (en) * | 1971-04-02 | 1973-06-22 | Е. И. Клабуновский , Л. Н. Кайгородова Институт органической химии Н. Д. Зелинского СССР | METHOD OF QUANTITATIVE SPLIT DETERMINATION |
| CN1199168A (en) * | 1997-05-13 | 1998-11-18 | 西安市中心血站 | Mannitol content measuring method for mixed preparation of mannitol and glucose |
| JP3362509B2 (en) * | 1994-06-24 | 2003-01-07 | 王子製紙株式会社 | Mannitol measurement method |
| CN102967670A (en) * | 2012-11-22 | 2013-03-13 | 黄宏南 | Method for measuring cordycepin, adenosine and mannitol in cordyceps sinensis mycelium powder |
-
2015
- 2015-10-23 CN CN201510695076.5A patent/CN105158167A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU388223A1 (en) * | 1971-04-02 | 1973-06-22 | Е. И. Клабуновский , Л. Н. Кайгородова Институт органической химии Н. Д. Зелинского СССР | METHOD OF QUANTITATIVE SPLIT DETERMINATION |
| JP3362509B2 (en) * | 1994-06-24 | 2003-01-07 | 王子製紙株式会社 | Mannitol measurement method |
| CN1199168A (en) * | 1997-05-13 | 1998-11-18 | 西安市中心血站 | Mannitol content measuring method for mixed preparation of mannitol and glucose |
| CN102967670A (en) * | 2012-11-22 | 2013-03-13 | 黄宏南 | Method for measuring cordycepin, adenosine and mannitol in cordyceps sinensis mycelium powder |
Non-Patent Citations (1)
| Title |
|---|
| 林玉洪 等: "钼酸铵增旋法测定甘露醇注射液的含量", 《淮海医药》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108593646A (en) * | 2018-04-27 | 2018-09-28 | 四川科伦药业股份有限公司 | A kind of rapid detection method of compound formula mannitol injection liquid intermediate mannitol content |
| CN111256792A (en) * | 2020-02-21 | 2020-06-09 | 康立泰药业有限公司 | Method for detecting filling amount of small-volume injection preparation |
| CN111256792B (en) * | 2020-02-21 | 2021-08-03 | 康立泰药业有限公司 | Method for detecting filling amount of small-volume injection preparation |
| CN114660196A (en) * | 2022-03-18 | 2022-06-24 | 广东大冢制药有限公司 | Method for determining related substances in medicine containing multi-component compound sorbitol solution |
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