CN103760275B - Content determination method of glucosamine hydrochloride raw material - Google Patents
Content determination method of glucosamine hydrochloride raw material Download PDFInfo
- Publication number
- CN103760275B CN103760275B CN201310569620.2A CN201310569620A CN103760275B CN 103760275 B CN103760275 B CN 103760275B CN 201310569620 A CN201310569620 A CN 201310569620A CN 103760275 B CN103760275 B CN 103760275B
- Authority
- CN
- China
- Prior art keywords
- solution
- need testing
- aminoglucose hydrochloride
- preparation
- reference substance
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Investigating Or Analysing Biological Materials (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a content determination method of a glucosamine hydrochloride raw material. The method adopts a high performance liquid chromatography-evaporative light scattering detection method, which is as below: a chromatographic column: NH2 column, 5 um, 250*4.6 um, a mobile phase containing acetonitrile and water in a proportion of 8-6:2.5-3.5, a flow rate of 0.8-1.2 ml/min, a column temperature of 30-40 DEG C, a detector of AlltechELSD2000, a drift tube temperature of 65-75 DEG C, and nitrogen pressure of 0.6-3.0 MPA; a control stock solution, a test solution and a blank solvent are injected into the liquid chromatograph; chromatograms are recorded; a value X of concentration of a standard substance solution and a value Y of a corresponding peak area are calculated out and subjected to linearity fitting to obtain an equation of linearity regression, wherein linearity scope is 0.2-1.2 mg/ml.
Description
Technical field
The present invention relates to a kind of method of quality control of medicine, particularly the content assaying method of aminoglucose hydrochloride raw material.
Background technology
The former national standard WS1-of aminoglucose hydrochloride capsule (X-090)-2005Z adopts ultraviolet-visible spectrophotometry to measure, this method is the content by measuring derivative reaction product content indirect determination aminoglucose hydrochloride, but the repeatability measured is poor.Sample preparation needs derivative reaction, and operate comparatively loaded down with trivial details, and the stability of sample solution is not high, repeatability is not strong.
Number of patent application: a kind of assay method of aminoglucose hydrochloride raw material of the content assaying method publicity of 201210012194.8 aminoglucose hydrochloride raw materials, the method uses acetonitrile, water and trifluoroacetic acid to be mobile phase, use C
18for the chromatographic column of filler.Trifluoroacetic acid in the method mobile phase has corrosivity, and in chromatogram, peak retention time is shorter, and separating effect is poor, and the range of linearity of the method is 0.8 ~ 1.2mg/ml, measures concentration range narrow.
The method of quality control of current aminoglucose hydrochloride raw material is not perfect.
Summary of the invention
The object of the invention is the content assaying method providing aminoglucose hydrochloride raw material.
The object of the invention is to be achieved through the following technical solutions.
The content assaying method of aminoglucose hydrochloride raw material of the present invention, the method comprises the steps:
Chromatographic column NH2 post, 5um, 250 × 4.6um, mobile phase consists of acetonitrile: water=(8-6:2.5-3.5), and flow velocity is 0.8-1.2ml/min, and column temperature is 30-40 DEG C, detecting device is Alltech ELSD 2000, and drift tube temperature is 65-75 DEG C, and nitrogen pressure is 0.6-3.0MPA.
The preparation of need testing solution: get the test sample being equivalent to 100mg aminoglucose hydrochloride, accurately weighed, put in 100ml volumetric flask, be dissolved in water, be diluted to scale, shake up, the solution of obtained concentration 1mg/ml, the miillpore filter through 0.45um filters, and precision measures subsequent filtrate as need testing solution.
The preparation of contrast solution: get aminoglucose hydrochloride reference substance appropriate, accurately weighed, from the solution product solution in contrast of the concentration 1.0mg/ml of need testing solution preparation method, 2mg/ml reference substance solution is for subsequent use as stock solution.
The preparation of blank solvent: using dissolve test sample, contrast solution solvent as blank.
Under above-mentioned chromatographic condition; accurate absorption contrast solution 20ul, need testing solution 20ul, blank solvent 20ul injection liquid chromatography; record chromatogram, calculates the value of standard solution concentration and the equation of linear regression of respective peaks area value, related coefficient and should be not less than 0.99; Accurate absorption need testing solution 20ul injection liquid chromatography, in need testing solution chromatogram, have identical peak at retention time place identical with reference substance solution, peak shape is symmetrical, theoretical cam curve more than 2000; Negative auxiliary material sample solution chromatogram, occurs without the peak identical with aminoglucose hydrochloride reference substance, namely negative noiseless: test sample of the present invention is containing Glucosamine C
6h
13o
5n.HCl should be the 99%-101% of labelled amount, and concentration range is 0.2-1.2mg/ml.
The method for optimizing that aminoglucose hydrochloride material content of the present invention measures is as follows:
Chromatographic column NH2 post, 5um, 250 × 4.6mm, mobile phase consists of acetonitrile: water (7:3), and flow velocity is 1.0ml/min, and column temperature is 35 DEG C, and detecting device is Alltech ELSD 2000, and drift tube temperature is 70 DEG C, and nitrogen pressure is 1.0MPA.
The preparation of need testing solution: get the test sample being equivalent to 100mg aminoglucose hydrochloride, accurately weighed, put in 100ml volumetric flask, be dissolved in water, be diluted to scale, shake up, the solution of obtained concentration 1mg/ml, the miillpore filter through 0.45um filters, and precision measures subsequent filtrate as need testing solution.
The preparation of contrast solution: get aminoglucose hydrochloride reference substance appropriate, accurately weighed, from the solution product solution in contrast of the concentration 1.0mg/ml of need testing solution preparation method.2mg/ml reference substance solution is for subsequent use as stock solution.
The preparation of blank solvent: using dissolve test sample, contrast solution solvent as blank.
Under above-mentioned chromatographic condition; accurate absorption contrast solution 20ul, need testing solution 20ul, blank solvent 20ul injection liquid chromatography; record chromatogram, calculates the value of standard solution concentration and the equation of linear regression of respective peaks area value, related coefficient and should be not less than 0.99; Accurate absorption need testing solution 20ul injection liquid chromatography, in need testing solution chromatogram, have identical peak at retention time place identical with reference substance solution, peak shape is symmetrical, theoretical cam curve more than 2000; Negative auxiliary material sample solution chromatogram, occurs without the peak identical with aminoglucose hydrochloride reference substance, namely negative noiseless: test sample of the present invention is containing Glucosamine C
6h
13o
5n.HCl should be the 99%-101% of labelled amount, and concentration range is 0.2-1.2mg/ml.
Chromatographic column NH2 post, 5um, 250 × 4.6mm, mobile phase consists of acetonitrile: water (7.5:3), and flow velocity is 1.2ml/min, and column temperature is 30 DEG C, and detecting device is Alltech ELSD 2000, and drift tube temperature is 75 DEG C, and nitrogen pressure is 1.2MPA.
The preparation of need testing solution: get the test sample being equivalent to 100mg aminoglucose hydrochloride, accurately weighed, put in 100ml volumetric flask, be dissolved in water, be diluted to scale, shake up, the solution of obtained concentration 1mg/ml, the miillpore filter through 0.45um filters, and precision measures subsequent filtrate as need testing solution.
The preparation of contrast solution: get aminoglucose hydrochloride reference substance appropriate, accurately weighed, from the solution product solution in contrast of the concentration 1.0mg/ml of need testing solution preparation method.2mg/ml reference substance solution is for subsequent use as stock solution.
The preparation of blank solvent: using dissolve test sample, contrast solution solvent as blank.
Under above-mentioned chromatographic condition; accurate absorption contrast solution 20ul, need testing solution 20ul, blank solvent 20ul injection liquid chromatography; record chromatogram, calculates the value of standard solution concentration and the equation of linear regression of respective peaks area value, related coefficient and should be not less than 0.99; Accurate absorption need testing solution 20ul injection liquid chromatography, in need testing solution chromatogram, have identical peak at retention time place identical with reference substance solution, peak shape is symmetrical, theoretical cam curve more than 2000; Negative auxiliary material sample solution chromatogram, occurs without the peak identical with aminoglucose hydrochloride reference substance, namely negative noiseless: test sample of the present invention is containing Glucosamine C
6h
13o
5n.HCl should be the 99%-101% of labelled amount, and concentration range is 0.2-1.2mg/ml.
Chromatographic column NH2 post, 5um, 250 × 4.6mm, mobile phase consists of acetonitrile: water (6.5:3), and flow velocity is 0.9ml/min, and column temperature is 40 DEG C, and detecting device is Alltech ELSD 2000, and drift tube temperature is 72 DEG C, and nitrogen pressure is 1.4MPA.
The preparation of need testing solution: get the test sample being equivalent to 100mg aminoglucose hydrochloride, accurately weighed, put in 100ml volumetric flask, be dissolved in water, be diluted to scale, shake up, the solution of obtained concentration 1mg/ml, the miillpore filter through 0.45um filters, and precision measures subsequent filtrate as need testing solution.
The preparation of contrast solution: get aminoglucose hydrochloride reference substance appropriate, accurately weighed, from the solution product solution in contrast of the concentration 1.0mg/ml of need testing solution preparation method.2mg/ml reference substance solution is for subsequent use as stock solution.
The preparation of blank solvent: using dissolve test sample, contrast solution solvent as blank.
Under above-mentioned chromatographic condition; accurate absorption contrast solution 20ul, need testing solution 20ul, blank solvent 20ul injection liquid chromatography; record chromatogram, calculates the value of standard solution concentration and the equation of linear regression of respective peaks area value, related coefficient and should be not less than 0.99; Accurate absorption need testing solution 20ul injection liquid chromatography, in need testing solution chromatogram, have identical peak at retention time place identical with reference substance solution, peak shape is symmetrical, theoretical cam curve more than 2000; Negative auxiliary material sample solution chromatogram, occurs without the peak identical with aminoglucose hydrochloride reference substance, namely negative noiseless: test sample of the present invention is containing Glucosamine C
6h
13o
5n.HCl should be the 99%-101% of labelled amount, and concentration range is 0.2-1.2mg/ml.
Aminoglucose hydrochloride raw material is made by the following method: be main ingredient by aminoglucose hydrochloride, and microcrystalline cellulose is filling agent, through granulating, always mixes, and raw material is filled, and packs and get final product.
According to test findings, method of quality control of the present invention shows that its repeatability is good, linear relationship is good, and precision is good, and stability of solution is good, and the recovery is good, and the range of linearity is wide.
Accompanying drawing illustrates:
System suitability reference substance Fig. 1;
System suitability test sample Fig. 2;
System suitability blank sheet 3;
Linear relationship typical curve Fig. 4.
Form is described in further detail content of the present invention more by the following examples, but should not be interpreted as in the above-mentioned subject area of the present invention at this point and be only limitted to following examples.Do not departing under the above-mentioned technology prerequisite of the present invention, the corresponding replacement made according to ordinary skill knowledge and customary means or the amendment of change, include within the scope of the invention
.
Embodiment 1
System suitability is tested
Chromatographic column NH2 post, 5um, 250 × 4.6mm, mobile phase consists of acetonitrile: water (7:3), and flow velocity is 1.0ml/min, and column temperature is 35 DEG C, and detecting device is Alltech ELSD 2000, and drift tube temperature is 70 DEG C, and nitrogen pressure is 1.0MPA.
The preparation of need testing solution: get the test sample being equivalent to 100mg aminoglucose hydrochloride, accurately weighed, put in 100ml volumetric flask, be dissolved in water, be diluted to scale, shake up, the solution of obtained concentration 1mg/ml, the miillpore filter through 0.45um filters, and precision measures subsequent filtrate as need testing solution.
The preparation of contrast solution: get aminoglucose hydrochloride reference substance appropriate, accurately weighed, from the solution product solution in contrast of the concentration 1.0mg/ml of need testing solution preparation method.2mg/ml reference substance solution is for subsequent use as stock solution.
The preparation of blank solvent: using dissolve test sample, contrast solution solvent as blank.
Under above-mentioned chromatographic condition, accurate absorption contrast solution 20ul, need testing solution 20ul, blank solvent 20ul injection liquid chromatography, record chromatogram.
Result shows: in need testing solution chromatogram, at retention time place identical with reference substance solution chromatogram, has identical peak, peak shape is symmetrical, and theoretical cam curve is more than 2000, in blank solvent chromatogram, occur without the peak identical with aminoglucose hydrochloride reference substance, namely blank noiseless.The results are shown in Figure 1, Fig. 2, Fig. 3.
Embodiment 2
Linear relationship is tested
Get reference substance stock solution (2mg/ml), thin up becomes the reference substance solution of 0.2mg/ml, 0.4mg/ml, 0.6mg/ml, 0.8mg/ml, 1.0mg/ml, 1.2mg/ml variable concentrations respectively, draws each contrast solution 20ul respectively, injection liquid chromatography.The linear equation of calculating concentration value and peak area value and regression coefficient, the results are shown in Table
1see Fig. 4.
Table 1 linear relationship experimental data table
Regression equation: y=7171696.1810 x-201307.8667, coefficient R 2=0.9999.
Experimental result shows, within the scope of 0.202mg/ml-1.212mg/ml, the value of solution concentration and the linear relationship of respective peaks area value good.
Embodiment 3
Precision Experiment
Accurate absorption reference substance solution (1.0mg/ml) 20ul injecting chromatograph, replication 5 times, calculates its precision, the results are shown in Table 2.
Table 2 Precision Experiment tables of data
Experimental result shows, precision is good.
Embodiment 4
Stability experiment
Get aminoglucose hydrochloride reference substance appropriate, add water and make 1mg/ml solution, measure peak area, 0 hour, 2 hours, 4 hours, 8 hours, 12 hours 20ul injecting chromatographs, the results are shown in Table 3 respectively.
Table 3 stability experiment tables of data
Experimental result shows, solution is stable in 12 hours.
Embodiment 5
Repeated experiment
Get aminoglucose hydrochloride material sample appropriate, precision takes and is equivalent to the putting in 25ml volumetric flask of aminoglucose hydrochloride 25mg, makes the solution that concentration is about 1mg/ml.Using such method repeats to prepare 5 parts, sample, and 20ul injecting chromatograph, the results are shown in Table 4.
Table 4 repeated experiment tables of data
Experimental result shows, this method repeatability better.
Embodiment 6
The recovery is tested
It is appropriate that precision takes aminoglucose hydrochloride, is respectively 80% of normal concentration, 100%, 120% each three parts, adds corresponding auxiliary material, put in volumetric flask, be dissolved in water and be diluted to scale, filter in prescription ratio.Calculate the recovery.Investigate relative standard deviation, the results are shown in Table 5.
Table 5 recovery experimental data table
Experimental result shows, this method recovery is good.
Embodiment 7
Durability is tested
In order to study the influence degree of subtle change to test findings of liquid phase chromatogram condition, carry out durability experiment.The principal element affecting efficient liquid phase-evaporative light-scattering content assaying method has mobile phase ratio, flow velocity, chromatographic column, drift tube temperature, nitrogen pressure.The condition that assay method adopts is flow velocity 1.0ml/min, and drift tube temperature is 70 DEG C, and nitrogen pressure is 1.0MPA, and mobile phase consists of acetonitrile: water (7:3) chromatographic column NH2 post.The preparation method of test sample and reference substance solution is with experimental example 1 lower requirement.The theoretical content of aminoglucose hydrochloride is 847.9mg/g.The results are shown in Table 6.
Table 6 durability experimental data table
Experimental result shows, the method content assaying method is reliable and stable, and durability is better.
Embodiment 8
Assay is tested
Experiment 1
Chromatographic column NH2 post, 5um, 250 × 4.6mm, mobile phase consists of acetonitrile: water (7:3), and flow velocity is 1.0ml/min, and column temperature is 35 DEG C, and detecting device is Alltech ELSD 2000, and drift tube temperature is 70 DEG C, and nitrogen pressure is 1.0MPA.
The preparation of need testing solution: precision takes the aminoglucose hydrochloride raw material that lot number is 130506, puts in 100ml volumetric flask, is dissolved in water, be diluted to scale, shake up, obtained concentration is about the solution of 1mg/ml, miillpore filter through 0.45um filters, as need testing solution.
The preparation of contrast solution: get aminoglucose hydrochloride reference substance appropriate, accurately weighed, make the solution product solution in contrast of concentration 1.0mg/ml.
Accurate absorption contrast solution 20ul, need testing solution 20ul injection liquid chromatography, record chromatogram.Record that content is 99.7%.
Experiment 2
Chromatographic column NH2 post, 5um, 250 × 4.6mm, mobile phase consists of acetonitrile: water (7:3), and flow velocity is 1.0ml/min, and column temperature is 35 DEG C, and detecting device is Alltech ELSD 2000, and drift tube temperature is 70 DEG C, and nitrogen pressure is 1.0MPA.
The preparation of need testing solution: precision takes the aminoglucose hydrochloride raw material that lot number is 130507, puts in 100ml volumetric flask, is dissolved in water, be diluted to scale, shake up, obtained concentration is about the solution of 1mg/ml, miillpore filter through 0.45um filters, as need testing solution.
The preparation of contrast solution: get aminoglucose hydrochloride reference substance appropriate, accurately weighed, make the solution product solution in contrast of concentration 1.0mg/ml.
Accurate absorption contrast solution 20ul, need testing solution 20ul injection liquid chromatography, record chromatogram.Recording content is 100.2%.
Experiment 3
Chromatographic column NH2 post, 5um, 250 × 4.6mm, mobile phase consists of acetonitrile: water (7:3), and flow velocity is 1.0ml/min, and column temperature is 35 DEG C, and detecting device is Alltech ELSD 2000, and drift tube temperature is 70 DEG C, and nitrogen pressure is 1.0MPA.
The preparation of need testing solution: precision takes the aminoglucose hydrochloride raw material that lot number is 130508, puts in 100ml volumetric flask, is dissolved in water, be diluted to scale, shake up, obtained concentration is about the solution of 1mg/ml, miillpore filter through 0.45um filters, as need testing solution.
The preparation of contrast solution: get aminoglucose hydrochloride reference substance appropriate, accurately weighed, make the solution product solution in contrast of concentration 1.0mg/ml.
Accurate absorption contrast solution 20ul, need testing solution 20ul injection liquid chromatography, record chromatogram.Recording content is 100.1%.
Claims (4)
1. a content assaying method for aminoglucose hydrochloride raw material, is characterized in that the method comprises the steps:
The content assaying method of aminoglucose hydrochloride raw material of the present invention, the method comprises the steps:
1) chromatographic column NH
2post, 5 μm, 250 × 4.6mm, mobile phase consists of acetonitrile: water=8-6:2.5-3.5(v/v), flow velocity is 0.8-1.2ml/min, and column temperature is 30-40 DEG C, detecting device is Alltech ELSD 2000, and drift tube temperature is 65-75 DEG C, and nitrogen pressure is 0.6-3.0MPA;
2) preparation of need testing solution: get the test sample being equivalent to 100mg aminoglucose hydrochloride, accurately weighed, put in 100ml volumetric flask, be dissolved in water, be diluted to scale, shake up, the solution of obtained concentration 1mg/ml, filter through the miillpore filter of 0.45 μm, precision measures subsequent filtrate as need testing solution;
3) preparation of contrast solution: get aminoglucose hydrochloride reference substance appropriate, accurately weighed, the solution product solution in contrast of the concentration 1.0mg/ml of need testing solution preparation method, 2mg/ml reference substance solution is for subsequent use as stock solution;
4) preparation of blank solvent: using dissolve need testing solution, contrast solution solvent as blank;
5) under above-mentioned chromatographic condition; accurate absorption contrast solution 20 μ l, need testing solution 20 μ l, blank solvent 20 μ l injection liquid chromatography; record chromatogram, calculates the value of standard solution concentration and the equation of linear regression of respective peaks area value, related coefficient and should be not less than 0.99; Accurate absorption need testing solution 20 μ l injection liquid chromatography, in need testing solution chromatogram, have identical peak at retention time place identical with reference substance solution, peak shape is symmetrical, theoretical cam curve more than 2000; Blank solvent solution chromatogram, occurs without the peak identical with aminoglucose hydrochloride reference substance, namely negative noiseless; Aminoglucose hydrochloride concentration range is 0.2-1.2mg/ml;
6) described aminoglucose hydrochloride raw material is made by the following method: be main ingredient by aminoglucose hydrochloride, and microcrystalline cellulose is filling agent, through granulating, always mixes, and pressure raw material, packs and get final product.
2. the content assaying method of aminoglucose hydrochloride raw material according to claim 1, is characterized in that the method comprises the steps:
1) chromatographic column NH
2post, 5 μm, 250 × 4.6mm, mobile phase consists of acetonitrile: water=7:3(v/v), flow velocity is 1.0ml/min, and column temperature is 35 DEG C, and detecting device is Alltech ELSD 2000, and drift tube temperature is 70 DEG C, and nitrogen pressure is 1.0MPA;
2) preparation of need testing solution: get the test sample being equivalent to 100mg aminoglucose hydrochloride, accurately weighed, put in 100ml volumetric flask, be dissolved in water, be diluted to scale, shake up, the solution of obtained concentration 1mg/ml, filter through the miillpore filter of 0.45 μm, precision measures subsequent filtrate as need testing solution;
3) preparation of contrast solution: get aminoglucose hydrochloride reference substance appropriate, accurately weighed, from the solution product solution in contrast of the concentration 1.0mg/ml of need testing solution preparation method, 2mg/ml reference substance solution is for subsequent use as stock solution;
4) preparation of blank solvent: using dissolve test sample, contrast solution solvent as blank;
5) under above-mentioned chromatographic condition; accurate absorption contrast solution 20 μ l, need testing solution 20 μ l, blank solvent 20 μ l injection liquid chromatography; record chromatogram, calculates the value of standard solution concentration and the equation of linear regression of respective peaks area value, related coefficient and should be not less than 0.99; Accurate absorption need testing solution 20 μ l injection liquid chromatography, in need testing solution chromatogram, have identical peak at retention time place identical with reference substance solution, peak shape is symmetrical, theoretical cam curve more than 2000; Negative auxiliary material sample solution chromatogram, occur without the peak identical with aminoglucose hydrochloride reference substance, namely solvent is noiseless; Aminoglucose hydrochloride concentration range is 0.2-1.2mg/ml.
3. the content assaying method of aminoglucose hydrochloride raw material according to claim 1, is characterized in that the method comprises the steps:
1) chromatographic column NH
2post, 5 μm, 250 × 4.6mm, mobile phase consists of acetonitrile: water=7.5:3(v/v), flow velocity is 1.2ml/min, and column temperature is 30 DEG C, and detecting device is Alltech ELSD 2000, and drift tube temperature is 75 DEG C, and nitrogen pressure is 1.2MPA;
2) preparation of need testing solution: get the test sample being equivalent to 100mg aminoglucose hydrochloride, accurately weighed, put in 100ml volumetric flask, be dissolved in water, be diluted to scale, shake up, the solution of obtained concentration 1mg/ml, filter through the miillpore filter of 0.45 μm, precision measures subsequent filtrate as need testing solution;
3) preparation of contrast solution: get aminoglucose hydrochloride reference substance appropriate, accurately weighed, from the solution product solution in contrast of the concentration 1.0mg/ml of need testing solution preparation method, 2mg/ml reference substance solution is for subsequent use as stock solution;
4) preparation of blank solvent: using dissolve test sample, contrast solution solvent as blank;
5) under above-mentioned chromatographic condition; accurate absorption contrast solution 20 μ l, need testing solution 20 μ l, blank solvent 20 μ l injection liquid chromatography; record chromatogram, calculates the value of standard solution concentration and the equation of linear regression of respective peaks area value, related coefficient and should be not less than 0.99; Accurate absorption need testing solution 20 μ l injection liquid chromatography, in need testing solution chromatogram, have identical peak at retention time place identical with reference substance solution, peak shape is symmetrical, theoretical cam curve more than 2000; Negative auxiliary material sample solution chromatogram, occurs without the peak identical with aminoglucose hydrochloride reference substance, namely negative noiseless; Aminoglucose hydrochloride concentration range is 0.2-1.2mg/ml.
4. the content assaying method of aminoglucose hydrochloride raw material according to claim 1, is characterized in that the method comprises the steps:
1) chromatographic column NH
2post, 5 μm, 250 × 4.6mm, mobile phase consists of acetonitrile: water=6.5:3(v/v), flow velocity is 0.9ml/min, and column temperature is 40 DEG C, and detecting device is Alltech ELSD 2000, and drift tube temperature is 72 DEG C, and nitrogen pressure is 1.4MPA;
2) preparation of need testing solution: get the test sample being equivalent to 100mg aminoglucose hydrochloride, accurately weighed, put in 100ml volumetric flask, be dissolved in water, be diluted to scale, shake up, the solution of obtained concentration 1mg/ml, filter through the miillpore filter of 0.45 μm, precision measures subsequent filtrate as need testing solution;
3) preparation of contrast solution: get aminoglucose hydrochloride reference substance appropriate, accurately weighed, from the solution product solution in contrast of the concentration 1.0mg/ml of need testing solution preparation method, 2mg/ml reference substance solution is for subsequent use as stock solution;
4) preparation of blank solvent: using dissolve test sample, contrast solution solvent as blank;
5) under above-mentioned chromatographic condition; accurate absorption contrast solution 20 μ l, need testing solution 20 μ l, blank solvent 20 μ l injection liquid chromatography; record chromatogram, calculates the value of standard solution concentration and the equation of linear regression of respective peaks area value, related coefficient and should be not less than 0.99; Accurate absorption need testing solution 20 μ l injection liquid chromatography, in need testing solution chromatogram, have identical peak at retention time place identical with reference substance solution, peak shape is symmetrical, theoretical cam curve more than 2000; Negative auxiliary material sample solution chromatogram, occurs without the peak identical with aminoglucose hydrochloride reference substance, namely negative noiseless; Aminoglucose hydrochloride concentration range is 0.2-1.2mg/ml.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310569620.2A CN103760275B (en) | 2013-11-13 | 2013-11-13 | Content determination method of glucosamine hydrochloride raw material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310569620.2A CN103760275B (en) | 2013-11-13 | 2013-11-13 | Content determination method of glucosamine hydrochloride raw material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103760275A CN103760275A (en) | 2014-04-30 |
| CN103760275B true CN103760275B (en) | 2015-07-15 |
Family
ID=50527548
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310569620.2A Active CN103760275B (en) | 2013-11-13 | 2013-11-13 | Content determination method of glucosamine hydrochloride raw material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103760275B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112578067A (en) * | 2019-09-29 | 2021-03-30 | 山东绿叶制药有限公司 | Method for measuring content of glucose in star-shaped PLGA |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590410A (en) * | 2012-01-13 | 2012-07-18 | 亚宝药业太原制药有限公司 | Content detection method for glucosamine hydrochloride capsules |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56114760A (en) * | 1980-02-13 | 1981-09-09 | Hitachi Ltd | Analytical method of amino sugar |
| CN102103133A (en) * | 2010-10-27 | 2011-06-22 | 南京威尔曼药物研究所 | Method for measuring related substances in glucosamine by using high performance liquid chromatography-evaporative light scattering detector (HPLC-ELSD) |
| CN102253143B (en) * | 2011-06-28 | 2013-09-04 | 南京海赋医药科技有限公司 | Rapid, simple, convenient and sensitive detection method for related impurities of glucosamine salt medicines |
-
2013
- 2013-11-13 CN CN201310569620.2A patent/CN103760275B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590410A (en) * | 2012-01-13 | 2012-07-18 | 亚宝药业太原制药有限公司 | Content detection method for glucosamine hydrochloride capsules |
Non-Patent Citations (1)
| Title |
|---|
| HPLC法测定盐酸氨基酸葡萄糖口腔崩解片中盐酸氨基葡萄糖的含量;李璟 等;《河北医科大学学报》;20100131;第31卷(第1期);第69-71页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103760275A (en) | 2014-04-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104914185A (en) | HPLC method for measuring related substances in Favipiravir | |
| CN104977372B (en) | Method for determining content of sulfonamide-phenylhydrazine hydrochloride in celecoxib raw medicine through high performance liquid chromatography | |
| CN108663448A (en) | Detection method in relation to substance in a kind of Amino Acid Compound Injection | |
| Ghanjaoui et al. | High performance liquid chromatography quality control | |
| CN103926335B (en) | The high-efficient liquid phase chromatogram process measuring method of related substance in a kind of Dapoxetine hydrochloride | |
| CN113671077A (en) | Detection method of acryloyl chloride and related substances thereof | |
| CN105301157A (en) | Quality control method of related substances of methanesulfonic acid kukoamine B | |
| CN104897841A (en) | Method of measuring content of p-Sulfonamide-phenylhydrazine hybrochloride in celecoxib capsules by means of efficient liquid chromatography | |
| CN103760275B (en) | Content determination method of glucosamine hydrochloride raw material | |
| CN110514759A (en) | The detection method of azido compound in a kind of candesartan Cilexetil | |
| CN103760244B (en) | The content assaying method of Glucosamine hydrochloride tablet | |
| CN108398497B (en) | High performance liquid chromatography detection method of tris (nonylphenol) phosphite ester | |
| CN102636582B (en) | Method for determining content of diminazene and antipyrine in diminazene particle | |
| CN102608231A (en) | Method for determining content of vitamin C in vitamin C effervescent tablets by HPLC (high performance liquid chromatography) | |
| CN103063794B (en) | Content detecting and control method of epalrestat tablets | |
| CN103776938B (en) | The content assaying method of aminoglucose hydrochloride capsule | |
| CN109100456A (en) | Method that is a kind of while measuring 3 kinds of liposoluble vitamin contents in multivitamin injection | |
| CN102590410A (en) | Content detection method for glucosamine hydrochloride capsules | |
| CN112345663B (en) | Analysis method for content of 5-chloro-2-methoxycarbonyl-1-indanone ester | |
| CN104374861B (en) | The method of the related substance of the western croak bulk drug of a kind of HPLC separation determination Leo | |
| CN103175930A (en) | High performance liquid chromatography analysis method for measuring sodium sulfite content | |
| CN102841169A (en) | Method for measuring calcium levofolinate-related substances by using high performance liquid chromatography gradient method | |
| CN108107138A (en) | The method that HPLC-CAD measures glucose in Dextrose and Sodium Chloride Inj. | |
| CN114236018B (en) | Caspofungin acetate and detection method of isomer thereof | |
| CN103743832B (en) | HPLC (High Performance Liquid Chromatography) measuring method of related substances in Dabigatran |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |