CN106706787A - Detection method and application of lysine content in aspirin-dl-lysine for injection - Google Patents
Detection method and application of lysine content in aspirin-dl-lysine for injection Download PDFInfo
- Publication number
- CN106706787A CN106706787A CN201611215171.1A CN201611215171A CN106706787A CN 106706787 A CN106706787 A CN 106706787A CN 201611215171 A CN201611215171 A CN 201611215171A CN 106706787 A CN106706787 A CN 106706787A
- Authority
- CN
- China
- Prior art keywords
- lysine
- solution
- aspirin
- sample
- detection method
- 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.)
- Granted
Links
Classifications
-
- 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
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Biological Materials (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a high performance liquid chromatography detection method for aspirin-dl-lysine. The method is capable of accurately and reliably measuring the lysine content in the drug aspirin-dl-lysine for injection, wide in linearity range, good in system suitability, high in accuracy, stability, precision, durability and specificity and easy to operate, and greatly reduces detection cost compared with a derivatization method and an automatic amino acid analyzer detection method.
Description
Technical field
Detection method and application the present invention relates to a kind of lysine, medicine is detected more particularly to one kind by HPLC
The detection method of middle lysine and application.
Background technology
Medicine di-lysine-aspirin is aspirin and lysine double salt, is non-steroidal anti-inflammatory analgesic-antipyretic, with antipyretic, town
Bitterly, antiinflammatory action.Its clinical practice formulation is aspirin-Al-lysine for injection.
《Chinese Pharmacopoeia》2015 editions have increased " aspirin-Al-lysine for injection " kind newly, wherein specifying to rely ammonia under " assay " item
Acid and aspirin two parts determine content respectively.But the assay in pharmacopeia to lysine is only described " with suitable
Amino-acid analyzer or high performance liquid chromatograph carry out separation determination ", do not record specific testing conditions.
Detect that amino acid content is mainly by high performance liquid chromatography (HPLC) at present and use derivatization method, such as with neighbour
Phthalaldehyde (OPA), DNFB (CDNB), phenyl isothiocyanate (PITC), DNF (DNFB) are
Derivatization reagent, is measured to amino acid content.But the derivative reaction of the prior art and chromatostrip being currently known
Part is all not applied for the assay of lysine in aspirin-Al-lysine for injection, and the derivative compound detected by existing method is not
Only one, specificity is very poor.
High performance liquid chromatography (HPLC), for specific measured object, is needed although being conventional determination method
To grope by substantial amounts of experiment, can just filter out the optimal selection of various parameters in chromatographic condition.Especially rely to medicine
In the detection of ammonia woods, because there is two kinds of compositions of aspirin and lysine, appearance is fast under the conditions of conventional reverse-phase chromatography, mutually
Interference, it is difficult to be directly separated measure.
Therefore, a kind of detection method of lysine is developed, relying in aspirin-Al-lysine for injection can accurately, be reliably detected
Histidine content is very necessary as drug standard.
The content of the invention
The present invention provides a kind of high-efficiency liquid chromatography method for detecting of lysine, and its chromatographic condition is：With sulfonic group sun from
Son exchanges bonded silica gel is filler, using the mixed liquor of phosphate solution and acetonitrile as mobile phase, wherein phosphate solution
Concentration is 10-60mmol/L, and the percent by volume of acetonitrile is 5-25%, and Detection wavelength is 200-210nm, and the Detection wavelength is energy
Detect the end wavelength of amino acid UV absorption.
Preferably, the present invention provides a kind of high-efficiency liquid chromatography method for detecting of lysine, and its chromatographic condition is：Use sulfonic acid
Base cation exchange bonded silica gel is filler, with 20mmol/L potassium dihydrogen phosphates-acetonitrile (85:15) it is mobile phase, detects ripple
A length of 205nm.
Further, the high-efficiency liquid chromatography method for detecting of lysine of the present invention, its chromatographic condition is：Use sulfonic group
Cation exchange bonded silica gel is filler, with 20mmol/L potassium dihydrogen phosphates-acetonitrile (85:15) it is mobile phase, Detection wavelength
It is 205nm, flow velocity is 1.0ml/min, and column temperature is 35 DEG C.
Further, the high-efficiency liquid chromatography method for detecting of lysine of the present invention, its number of theoretical plate presses lysine peak
Meter is not less than 3000.
Preferably, the high-efficiency liquid chromatography method for detecting of lysine of the present invention, wherein lysine concentration to be detected
Scope is 0.2-2.0058mg/ml.
Preferably, the high-efficiency liquid chromatography method for detecting of lysine of the present invention, wherein product to be tested are used for drug injection
Di-lysine-aspirin.
Preferably, the high-efficiency liquid chromatography method for detecting of lysine of the present invention, its assay method is：
Chromatographic condition and system suitability：It is filler with sulfonic group cation exchange bonded silica gel, with 20mmol/
L potassium dihydrogen phosphates-acetonitrile (85:15) it is mobile phase；Detection wavelength is 205nm, and number of theoretical plate should be not less than based on lysine peak
3000。
Determination method：Take aspirin-Al-lysine for injection test sample appropriate, it is accurately weighed, plus the dissolving of 0.02mmol/L hydrochloric acid solutions is simultaneously
The solution containing about lysine 0.8mg is quantitatively diluted in every 1ml as need testing solution, precision measures 20 μ l, injects liquid phase color
Spectrometer, records chromatogram；The another lysine hydrochloride reference substance that takes is appropriate, is measured in the same method.By external standard method with calculated by peak area lysine
Content, obtain final product.
The present invention also provides a kind of application of the high-efficiency liquid chromatography method for detecting of lysine, and it is used to detect drug injection
With the lysine content in di-lysine-aspirin.
The high-efficiency liquid chromatography method for detecting of lysine of the invention, can to medicine " aspirin-Al-lysine for injection " in rely
Histidine content is accurately and reliably determined, and has good linear relationship, system in the concentration range of 0.2-2.0mg/ml
Applicability is good, and the degree of accuracy is high, and stability, precision, durability and specificity are good, and operation is simple, relatively derives
Change method and automatic amino acid analyzer detection method greatly reduce testing cost.
Brief description of the drawings
Fig. 1：The concentration of lysine hydrochloride reference substance is to peak area linear regression curves figure in embodiment 2.
Fig. 2：The chromatogram result of embodiment 10.
Fig. 3：The chromatogram result of embodiment 11.
Specific embodiment
The present invention is described in more detail for example below, artisan will appreciate that not departing from this hair
The change made in the case of bright scope and spirit, belongs to the scope of the present invention.
Embodiment 1：Chromatographic condition and sample
High performance liquid chromatograph：Shimadzu LC-20A liquid chromatographs.
Chromatographic condition：It is filler with sulfonic group cation exchange bonded silica gel, with 20mmol/L potassium dihydrogen phosphates-acetonitrile
(85:15) it is mobile phase；Flow velocity is 1.0ml/min, and column temperature is 35 DEG C, and Detection wavelength is 205nm, and number of theoretical plate presses lysine peak
Meter should be not less than 3000.
Lysine hydrochloride reference substance：From National Institute for Food and Drugs Control, 140673-201408, content：
99.9%.
Test sample：Sino Pharm Group Guorui Pharmaceutical Co., Ltd, aspirin-Al-lysine for injection, specification：0.9g, lot number：1510101
Diluent：0.02mol/L hydrochloric acid solutions.
Embodiment 2：Linear test
Accurately weighed lysine hydrochloride reference substance 0.10029g, is put in 50ml measuring bottles, and quarter is dissolved and be diluted to diluent
Degree, shakes up, as linear test stock solution (100% concentration).Precision measure linear test storing solution 1ml, 2ml, 3ml,
4ml, 5ml, 6ml, 7ml, 8ml, are put in 10ml measuring bottles respectively, and scale is diluted to diluent, are shaken up, used as linear test series
Strength solution, respectively 10% strength solution, 20% strength solution, 30% strength solution, 40% strength solution, 50% concentration are molten
Liquid, 60% strength solution, 70% strength solution, 80% strength solution.
Precision measures the μ l of each strength solution 20 respectively, injects liquid chromatograph, and each sample feeding 2 times records chromatogram.
Result of the test shows that lysine linear relationship in about 0.20058mg/ml-2.0058mg/ml concentration ranges is good.With concentration
Linear regression is carried out to peak area, result of the test see the table below 1, and linear regression curves are shown in accompanying drawing 1.
The lysine content assay method linear test result of table 1
Embodiment 3：System suitability
Lower 40% strength solution of linear test is taken, used as system suitability solution, precision measures 20 μ l injection liquid phase colors
Spectrometer, continuous sample introduction 6 times records chromatogram.Result of the test shows that this method system suitability is good, and result of the test see the table below
2。
The lysine content assay method system suitability result of table 2
| Determine number of times | 1 | 2 | 3 | 4 | 5 | 6 | Averagely | RSD% |
| Retention time (min) | 25.944 | 25.941 | 25.935 | 25.936 | 25.935 | 25.934 | 25.938 | 0.02 |
| Peak area | 489875 | 489813 | 490356 | 490332 | 490151 | 489632 | 490026.5 | 0.07 |
| Theoretical cam curve | 14735.8 | 14770.2 | 14748.5 | 14745.0 | 14685 | 14762.5 | 14741.2 | 0.20 |
Embodiment 4：Accuracy test (sample-adding recovery test)
It is prepared by determination of recovery rates storing solution：(lysine content is accurate for accurately weighed aspirin-Al-lysine for injection 0.38106g
44.70% is determined, that is, contains the common 0.1703g of lysine), put in 250ml measuring bottles, scale is dissolved and is diluted to diluent, shake
It is even, as determination of recovery rates storing solution.
The preparation of determination of recovery rates solution：Accurately weighed 9 parts of lysine hydrochloride reference substances (reality of lysine in every 1 part
3) input amount is shown in Table, and puts respectively in 9 50ml measuring bottles, and each measuring bottle is accurate to add the above-mentioned determination of recovery rates storing solutions of 25ml (i.e.
Amount containing the lysine in sample in each measuring bottle is 0.01703g), then with diluent scale is settled to respectively, shake up, as
Determination of recovery rates solution.
Above-mentioned each 20 μ l of 9 determination of recovery rates solution are taken, liquid chromatograph is injected, each solution sample introduction 2 times records chromatogram
Figure；Using lower 40% strength solution of linear test as reference substance solution, by external standard method with calculated by peak area measured amount, then press
Formula calculates average recovery.Result of the test shows that this method degree of accuracy is high, disclosure satisfy that detection is required, result of the test see the table below
3。
The lysine content assay method of table 3 is loaded recovery test result
Embodiment 5：Solution stability testing
40% strength solution as reference substance stability test solution is descended using linear test；Accurately weighed test sample
0.07545g puts 50ml measuring bottles, and scale is dissolved and be diluted to diluent, used as test sample stability test solution；Both the above
Solution is put into liquid chromatograph specimen holder, and specimen holder temperature is room temperature.Reference substance stability test solution is in the 0th, 2,5,
9th, 20 μ l injection liquid chromatographs are taken within 14,19,24,29 and 35 hours respectively, record chromatogram；Test sample stability test solution
Take 20 μ l injection liquid chromatographs respectively in the 0th, 3,6,9,14,21,26 and 32 hours, record chromatogram.Result of the test shows,
Reference substance solution room temperature places 35 hours stabilizations；Need testing solution places 32 hours stabilizations at room temperature.Result of the test see the table below 4.
The lysine content of table 4 determines solution stability testing result
Embodiment 6：Precision test
It is sample 1 with stability test need testing solution, 5 parts of need testing solutions is prepared with method, totally 6 parts of samples, above-mentioned molten
Liquid takes 20 μ l injection liquid chromatographs respectively, and each sample feeding 2 times records chromatogram；With lower 40% concentration of linear test
Solution as reference substance solution, by external standard method with lysine content in calculated by peak area test sample.Result of the test shows, this method
Precision is good.Result of the test see the table below 5.
The lysine content assay method Precision test result of table 5
| Sample 1 | Sample 2 | Sample 3 | Sample 4 | Sample 5 | Sample 6 | RSD (%) | |
| 1st peak area of sample introduction | 512097 | 511470 | 509518 | 515252 | 516587 | 516639 | --- |
| 2nd peak area of sample introduction | 512588 | 512155 | 509325 | 515145 | 516240 | 516138 | --- |
| Lysine content (%) | 44.76 | 44.64 | 44.69 | 44.77 | 44.64 | 44.67 | 0.13 |
Embodiment 7：Intermediate precision is tested
Another analyst uses the high performance liquid chromatograph (Shimadzu different from the model of embodiment 6 in the different time
LC-2010CHT), tested with identical chromatographic condition.
Test sample about 76mg is weighed, 50ml measuring bottles are put, scale is dissolved and be diluted to diluent, as need testing solution；
5 parts of need testing solutions are prepared with method again, totally 6 parts of samples, above-mentioned solution takes 20 μ l injection liquid chromatographs respectively, each sample enters
Sample 2 times, records chromatogram；Accurately weighed reference substance 0.02023g, puts 25ml measuring bottles, and scale is dissolved and be diluted to diluent,
As reference substance solution, by external standard method with lysine content in calculated by peak area test sample.Result of the test shows, the He of embodiment 6
Lysine content measured value RSD is 0.59% in two 12 parts of test samples of analysis personnel of embodiment 7, is shown in the middle of this method
Precision is good.Result of the test see the table below 6 and table 7.
The lysine content assay method Intermediate precision result of the test of table 6
| Sample 1 | Sample 2 | Sample 3 | Sample 4 | Sample 5 | Sample 6 | RSD (%) | |
| 1st peak area of sample introduction | 536976 | 530281 | 535771 | 530206 | 538252 | 532216 | --- |
| 2nd peak area of sample introduction | 536467 | 529918 | 535569 | 530544 | 536990 | 534081 | --- |
| Lysine content (%) | 45.11 | 45.08 | 45.10 | 44.87 | 45.50 | 45.00 | 0.48 |
The lysine content precision test result of table 7
Embodiment 8：Durability is tested
Take lysine hydrochloride reference substance appropriate, plus diluent dissolving.Selection column temperature is 30 DEG C and 40 DEG C respectively, and flow velocity is
0.8ml/min and 1.2ml/min, phosphate concn 18mmol and 22mmol, organic phase (acetonitrile) ratio are 13% and 17%, its
His corresponding chromatographic condition is constant.Precision measures 20 μ l, injects liquid chromatograph, records chromatogram.Result of the test shows, this method
Good tolerance.Result of the test see the table below 8.
The lysine content assay method serviceability test result of table 8
Embodiment 9：Specificity is tested
(1) sour water solution (5mol/L HCl room temperatures place 72h)：Weigh during test sample 76mg puts 50ml measuring bottles, add 5ml's
5mol/L HCl room temperatures place 72h, with NaOH and after, plus diluent is diluted to scale, shakes up, and takes solution filtering, obtains final product.
(2) basic hydrolysis (5mol/L NaOH room temperatures place 72h)：Weigh during test sample 76mg puts 50ml measuring bottles, add 5ml
5mol/L NaOH room temperatures place 72h, with HCl and after, plus diluent is diluted to scale, shakes up, and takes solution filtering, obtains final product.
(3) high temperature (85 DEG C of placement 6h)：Weigh during test sample 152mg puts 25*40mm measuring cups, shakeout, at 85 DEG C
Lower heating 6 hours, is cooled to room temperature, is dissolved and is transferred in 100ml measuring bottles with diluent, and is settled to scale with diluent,
Shake up and obtain final product.
(4) Oxidative demage (30%H2O2Room temperature places 72h)：Weigh during test sample 76mg puts 50ml measuring bottles, add 5ml's
30%H2O2 room temperatures place 72h, plus diluent is diluted to scale, shakes up, and take solution filtering, obtain final product.
(5) illumination destruction (4500Lux irradiates 72h)：Weigh during test sample 152mg puts 25*40mm measuring cups, shakeout,
72h is irradiated under the conditions of 4500Lux, is dissolved and is transferred in 100ml measuring bottles with diluent, and scale is settled to diluent, shaken
It is even to obtain final product.
Precision measures each μ l of solution 20 injections liquid chromatograph of the above, is detected with DAD detectors, records chromatogram, each bar
The purity of lysine main peak meets the requirements (be all higher than 0.999) under part, shows the specificity of this method very well, and catabolite
Separating degree between main peak is more than 1.5.
Separately take aspirin reference substance (National Institute for Food and Drugs Control, 100113-201405, content：99.8%),
Salicylic acid reference substance (National Institute for Food and Drugs Control, 100106-201104, content：99.9%), acetic acid (Chinese medicines group
Chemical reagent Co., Ltd, 20131016, content：>=99.5%) each with reference substance appropriate, debita spissitudo is configured to diluent
Solution, take each 20 μ l injections liquid chromatograph of above solution and solvent, record chromatogram.Result of the test shows that injection relies
Principal component aspirin and its major degradants salicylic acid, acetic acid in ammonia woods, and other unknown degradation impurities, are had
Effect is separated, and the measure of lysine is not disturbed, and this method specificity is good.
Result of the test see the table below 9：
The lysine content assay method specificity of table 9 tests separating degree and peak purity
| Failure condition | The separating degree of main peak and other impurities | Peak purity index |
| Sour water solution | 34.147 | 0.999951 |
| Basic hydrolysis | 32.868 | 0.999899 |
| Oxidative demage | 17.580 | 0.999955 |
| High temperature | 7.190 | 0.999583 |
| High light is destroyed | 36.847 | 0.999868 |
Embodiment 10：Determine embodiment 1
Chromatographic condition：It is filler with sulfonic group cation exchange bonded silica gel, with 20mmol/L potassium dihydrogen phosphates-acetonitrile
(85：15) it is mobile phase, Detection wavelength is 205nm, and flow velocity is 1.0ml/min, and column temperature is 35 DEG C.
The specification of test sample is：0.9g/ branch.5 test samples are taken, the average loading amount for measuring test sample is 0.9102g/ branch.
Precision weighs test sample 82.60mg, puts 50ml measuring bottles, and scale is dissolved and be diluted to diluent, shakes up, as confession
Test sample solution (CSample=82.60/50=1.6520mg/ml)；Precision measures 20 μ l injection liquid chromatographs, records chromatogram, often
Individual need testing solution sample introduction 2 times；Another precision weighs lysine hydrochloride reference substance 50.44mg, puts 50ml measuring bottles, is dissolved with diluent
And scale is diluted to, as reference substance solution (CIt is right=50.44 × 0.999 × 0.8004/50=0.80664mg/ml), surveyed with method
It is fixed.By external standard method with lysine content in calculated by peak area test sample be 44.61%.The chromatogram of test sample and reference substance is shown in figure
2。
ASample：Lysine peak area average in need testing solution；AIt is right：Lysine peak area average in reference substance solution.
Embodiment 11：Determine embodiment 2
Chromatographic condition：It is filler with sulfonic group cation exchange bonded silica gel, with 25mmol/L sodium dihydrogen phosphates-acetonitrile
(80：20) it is mobile phase, Detection wavelength is 208nm, and flow velocity is 0.8ml/min, and column temperature is 30 DEG C.
The specification of test sample is：0.9g/ branch.5 test samples are taken, the average loading amount for measuring test sample is 0.9098g/ branch.
Precision weighs test sample 98.51mg, puts 50ml measuring bottles, and scale is dissolved and be diluted to diluent, shakes up, as confession
Test sample solution (CSample=98.51/50=1.9702mg/ml)；Precision measures 20 μ l injection liquid chromatographs, records chromatogram, often
Individual need testing solution sample introduction 2 times；Another precision weighs lysine hydrochloride reference substance 50.12mg, puts 50ml measuring bottles, is dissolved with diluent
And scale is diluted to, as reference substance solution (CIt is right=50.12 × 0.999 × 0.8004/50=0.80152mg/ml), surveyed with method
It is fixed.By external standard method with lysine content in calculated by peak area test sample be 44.70%.The chromatogram of test sample and reference substance is shown in figure
3。
ASample：Lysine peak area average in need testing solution；AIt is right：Lysine peak area average in reference substance solution.
Claims (9)
1. a kind of high-efficiency liquid chromatography method for detecting of lysine, its chromatographic condition is：With sulfonic group cation exchange bonded silica
Glue is filler, and using the mixed liquor of phosphate solution and acetonitrile as mobile phase, the wherein concentration of phosphate solution is 10-
60mmol/L, the percent by volume of acetonitrile is 5-25%, and Detection wavelength is 200-210nm.
2. detection method according to claim 1, its chromatographic condition is：It is to fill out with sulfonic group cation exchange bonded silica gel
Agent is filled, with 20mmol/L potassium dihydrogen phosphates-acetonitrile (85:15) it is mobile phase, Detection wavelength is 205nm.
3. detection method according to claim 2, its chromatographic condition is：It is to fill out with sulfonic group cation exchange bonded silica gel
Agent is filled, with 20mmol/L potassium dihydrogen phosphates-acetonitrile (85:15) it is mobile phase, Detection wavelength is 205nm, and flow velocity is 1.0ml/
Min, column temperature is 35 DEG C.
4. the detection method according to any one of claim 1-3, its number of theoretical plate is not less than 3000 based on lysine peak.
5. the detection method according to any one of claim 1-3, wherein lysine concentration scope to be detected is 0.2-
2.0058mg/ml。
6. the detection method according to any one of claim 1-3, wherein product to be tested are aspirin-Al-lysine for injection.
7. in a kind of aspirin-Al-lysine for injection lysine content detection method, including：
(1) chromatographic condition and system suitability：It is filler with sulfonic group cation exchange bonded silica gel, with 20mmol/L
Potassium dihydrogen phosphate-acetonitrile (85:15) it is mobile phase；Detection wavelength is 205nm, and number of theoretical plate should be not less than based on lysine peak
3000；
(2) determination method：Take aspirin-Al-lysine for injection test sample appropriate, it is accurately weighed, plus the dissolving of 0.02mmol/L hydrochloric acid solutions is simultaneously
The solution containing about lysine 0.8mg is quantitatively diluted in every 1ml as need testing solution, precision measures 20 μ l, injects liquid phase color
Spectrometer, records chromatogram；The another lysine hydrochloride reference substance that takes is appropriate, is measured in the same method；By external standard method with calculated by peak area lysine
Content.
8. in a kind of aspirin-Al-lysine for injection lysine content detection method, including：
Chromatographic condition：It is filler with sulfonic group cation exchange bonded silica gel, with 20mmol/L potassium dihydrogen phosphates-acetonitrile (85:
15) it is mobile phase, Detection wavelength is 205nm, and flow velocity is 1.0ml/min, and column temperature is 35 DEG C；
Determination method：Precision weighs test sample, puts 50ml measuring bottles, is dissolved with 0.02mmol/L hydrochloric acid solutions and is diluted to scale, shakes
It is even, as need testing solution；Precision measures 20 μ l, injects liquid chromatograph, records chromatogram, each need testing solution sample introduction 2
It is secondary；Another precision weighs lysine hydrochloride reference substance, puts 50ml measuring bottles, and quarter is dissolved and be diluted to 0.02mmol/L hydrochloric acid solutions
Degree, as reference substance solution, is measured in the same method；By external standard method with lysine content in calculated by peak area test sample, computing formula is：
Wherein,
ASampleIt is lysine peak area average in need testing solution；AIt is rightIt is lysine peak area average in reference substance solution；CIt is rightIt is defined
The concentration of the reference substance solution for really preparing, CSampleIt is the nominal concentration of the accurate need testing solution for preparing；Average loading amount is every confession
The average equipped amount of content of test product container；Specification is every labelled amount of test sample.
9. the application of the detection method described in claim 1-8 any one, it is characterised in that be for detecting that drug injection is used
Lysine content in di-lysine-aspirin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611215171.1A CN106706787B (en) | 2016-12-26 | 2016-12-26 | The detection method and application of lysine content in a kind of aspirin-Al-lysine for injection |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611215171.1A CN106706787B (en) | 2016-12-26 | 2016-12-26 | The detection method and application of lysine content in a kind of aspirin-Al-lysine for injection |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106706787A true CN106706787A (en) | 2017-05-24 |
| CN106706787B CN106706787B (en) | 2019-01-15 |
Family
ID=58902635
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611215171.1A Active CN106706787B (en) | 2016-12-26 | 2016-12-26 | The detection method and application of lysine content in a kind of aspirin-Al-lysine for injection |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106706787B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2350802A (en) * | 1999-06-08 | 2000-12-13 | Anglia Polytechnic University | Sample pre-treatment |
| CN1865988A (en) * | 2006-06-21 | 2006-11-22 | 广州星群（药业）股份有限公司 | Method for detecting amino acid component in Xiasangju preparation |
| CN101963603A (en) * | 2010-09-30 | 2011-02-02 | 湖北新生源生物工程股份有限公司 | Method for analyzing arginine and arginine hydrochloride raw materials and preparations by using HPLC method |
| CN102440989A (en) * | 2010-10-13 | 2012-05-09 | 四川科伦药物研究有限公司 | Compound amino acid injecta, and preparation method and detection method thereof |
| CN103787904A (en) * | 2012-11-01 | 2014-05-14 | 北京双鹭药业股份有限公司 | Preparation method of novel L-lysine alkaline solution |
| CN104280475A (en) * | 2014-10-30 | 2015-01-14 | 四川科伦药业股份有限公司 | Method for detecting content of amino acids and glycyl glutamine in compound amino acid (15) dipeptide (2) injection solution |
-
2016
- 2016-12-26 CN CN201611215171.1A patent/CN106706787B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2350802A (en) * | 1999-06-08 | 2000-12-13 | Anglia Polytechnic University | Sample pre-treatment |
| CN1865988A (en) * | 2006-06-21 | 2006-11-22 | 广州星群（药业）股份有限公司 | Method for detecting amino acid component in Xiasangju preparation |
| CN101963603A (en) * | 2010-09-30 | 2011-02-02 | 湖北新生源生物工程股份有限公司 | Method for analyzing arginine and arginine hydrochloride raw materials and preparations by using HPLC method |
| CN102440989A (en) * | 2010-10-13 | 2012-05-09 | 四川科伦药物研究有限公司 | Compound amino acid injecta, and preparation method and detection method thereof |
| CN103787904A (en) * | 2012-11-01 | 2014-05-14 | 北京双鹭药业股份有限公司 | Preparation method of novel L-lysine alkaline solution |
| CN104280475A (en) * | 2014-10-30 | 2015-01-14 | 四川科伦药业股份有限公司 | Method for detecting content of amino acids and glycyl glutamine in compound amino acid (15) dipeptide (2) injection solution |
Non-Patent Citations (3)
| Title |
|---|
| J.R.LARSON 等: "Determination of organic ionic compounds by liquid chromatography with indirect photometric detection", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| 国家药典委员会: "《中华人民共和国药典 2015年版 二部》", 30 June 2015, 北京：中国医药科技出版社 * |
| 李建华 等: "沼液中溶解游离氨基酸的测定——柱前衍生-反相高效液相色谱法", 《中国环境科学》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106706787B (en) | 2019-01-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107907603A (en) | A kind of measure assay method of the amino acids parenteral solution tryptophan in relation to material | |
| CN109870521B (en) | Method for separating oseltamivir phosphate enantiomers by normal phase chromatography | |
| CN105717237B (en) | The detection method of GABA, Glu, DA, 5-HT and Capillary zone electropheresis in a kind of serum | |
| CN104931599A (en) | Determining method of atorvastatin calcium related substance | |
| CN106841408B (en) | The rapid detection method of methionine sulfoxide in a kind of amino acid injection | |
| CN108663448A (en) | Detection method in relation to substance in a kind of Amino Acid Compound Injection | |
| CN106950291A (en) | A kind of detection method of ambroxol hydrochloride injection about material | |
| BHATKAR et al. | " Stability Indicating RP-HPLC Method Development and Validation for the Estimation of Remogliflozin Etabonate in Bulk and Pharmaceutical Dosage Form". | |
| Wang et al. | A liquid chromatographic method for simultaneous determination of amoxicillin sodium and sulbactam sodium in a combination formulation | |
| CN102841170A (en) | Method for detecting impurity phenylhydrazine in edaravone | |
| Nathi et al. | QbD‐based stability‐indicating liquid chromatography (RP‐HPLC) method for the determination of flurbiprofen in cataplasm | |
| CN107991415B (en) | Method for simultaneously separating and measuring pyroglutamic acid and methionine sulfoxide impurities in compound amino acid injection 18AA by liquid chromatography | |
| CN112946099B (en) | Method for detecting related substances in amino acid glucose injection | |
| CN106706789A (en) | Method for detecting related substances in drotaverine hydrochloride injection by high performance liquid chromatography | |
| CN109613128A (en) | The measuring method of drug content in a kind of Famotidine Capsule | |
| Legnerová et al. | Automated sequential injection fluorimetric determination and dissolution studies of ergotamine tartrate in pharmaceuticals | |
| CN109725099A (en) | A kind of efficient liquid phase detection method of valine | |
| CN103543222A (en) | Reduning injection saccharide content detection method | |
| CN106706787B (en) | The detection method and application of lysine content in a kind of aspirin-Al-lysine for injection | |
| CN104535690B (en) | Method for measuring content of cinnarizine in cinnarizine solid preparation | |
| CN101285803A (en) | Qualitative analysis detection method for low polarity sugar-reducing chemical medicament in traditional Chinese medicine | |
| CN109100456A (en) | Method that is a kind of while measuring 3 kinds of liposoluble vitamin contents in multivitamin injection | |
| CN108872406A (en) | HPLC analyzing detecting method in relation to substance in a kind of L-aminobutanedioic acid bulk pharmaceutical chemicals | |
| CN101285802A (en) | Qualitative analysis detection method for high polarity sugar-reducing chemical medicament in traditional Chinese medicine | |
| Tzanavaras et al. | Automated tagging of pharmaceutically active thiols under flow conditions using monobromobimane |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP02 | Change in the address of a patent holder | ||
| CP02 | Change in the address of a patent holder |
Address after: 232000 No.16 Chaoyang East Road, Huainan Economic and Technological Development Zone, Anhui Province Patentee after: CHINA NATIONAL MEDICINES GUORUI PHARMACEUTICAL Co.,Ltd. Address before: 232008 north side of Chaoyang East Road, Huainan Economic and Technological Development Zone, Anhui Province Patentee before: CHINA NATIONAL MEDICINES GUORUI PHARMACEUTICAL Co.,Ltd. |