CN113640406A - Method for detecting content of clindamycin palmitate hydrochloride - Google Patents
Method for detecting content of clindamycin palmitate hydrochloride Download PDFInfo
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- CN113640406A CN113640406A CN202110818169.8A CN202110818169A CN113640406A CN 113640406 A CN113640406 A CN 113640406A CN 202110818169 A CN202110818169 A CN 202110818169A CN 113640406 A CN113640406 A CN 113640406A
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- clindamycin palmitate
- palmitate hydrochloride
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- GTNDZRUWKHDICY-DJHAJVGHSA-N Clindamycin palmitate hydrochloride Chemical compound Cl.O1[C@H](SC)[C@H](OC(=O)CCCCCCCCCCCCCCC)[C@@H](O)[C@@H](O)[C@H]1[C@@H]([C@H](C)Cl)NC(=O)[C@H]1N(C)C[C@H](CCC)C1 GTNDZRUWKHDICY-DJHAJVGHSA-N 0.000 title claims abstract description 65
- 229960000792 clindamycin palmitate hydrochloride Drugs 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000012360 testing method Methods 0.000 claims abstract description 24
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 23
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 238000001514 detection method Methods 0.000 claims abstract description 7
- 238000011084 recovery Methods 0.000 claims abstract description 7
- 239000012085 test solution Substances 0.000 claims description 23
- 239000000243 solution Substances 0.000 claims description 21
- 239000003814 drug Substances 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 14
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Natural products OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 11
- 239000012088 reference solution Substances 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical group N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 7
- 239000005695 Ammonium acetate Substances 0.000 claims description 7
- 229940043376 ammonium acetate Drugs 0.000 claims description 7
- 235000019257 ammonium acetate Nutrition 0.000 claims description 7
- 239000008186 active pharmaceutical agent Substances 0.000 claims description 5
- 235000019329 dioctyl sodium sulphosuccinate Nutrition 0.000 claims description 5
- 229940088679 drug related substance Drugs 0.000 claims description 5
- CDOUZKKFHVEKRI-UHFFFAOYSA-N 3-bromo-n-[(prop-2-enoylamino)methyl]propanamide Chemical compound BrCCC(=O)NCNC(=O)C=C CDOUZKKFHVEKRI-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 230000005526 G1 to G0 transition Effects 0.000 claims description 2
- 238000010829 isocratic elution Methods 0.000 claims description 2
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical group CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 238000007865 diluting Methods 0.000 description 5
- 239000013558 reference substance Substances 0.000 description 5
- KDLRVYVGXIQJDK-AWPVFWJPSA-N clindamycin Chemical class CN1C[C@H](CCC)C[C@H]1C(=O)N[C@H]([C@H](C)Cl)[C@@H]1[C@H](O)[C@H](O)[C@@H](O)[C@@H](SC)O1 KDLRVYVGXIQJDK-AWPVFWJPSA-N 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 229960002227 clindamycin Drugs 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 238000010812 external standard method Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000003908 quality control method Methods 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 206010060968 Arthritis infective Diseases 0.000 description 1
- 241000193830 Bacillus <bacterium> Species 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 241000606161 Chlamydia Species 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- OJMMVQQUTAEWLP-UHFFFAOYSA-N Lincomycin Natural products CN1CC(CCC)CC1C(=O)NC(C(C)O)C1C(O)C(O)C(O)C(SC)O1 OJMMVQQUTAEWLP-UHFFFAOYSA-N 0.000 description 1
- 241000204031 Mycoplasma Species 0.000 description 1
- 208000005141 Otitis Diseases 0.000 description 1
- 206010057190 Respiratory tract infections Diseases 0.000 description 1
- 206010040047 Sepsis Diseases 0.000 description 1
- 206010062255 Soft tissue infection Diseases 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 241001148470 aerobic bacillus Species 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229960001200 clindamycin hydrochloride Drugs 0.000 description 1
- YHAIUSTWZPMYGG-UHFFFAOYSA-L disodium;2,2-dioctyl-3-sulfobutanedioate Chemical compound [Na+].[Na+].CCCCCCCCC(C([O-])=O)(C(C([O-])=O)S(O)(=O)=O)CCCCCCCC YHAIUSTWZPMYGG-UHFFFAOYSA-L 0.000 description 1
- 208000019258 ear infection Diseases 0.000 description 1
- IPCSVZSSVZVIGE-UHFFFAOYSA-M hexadecanoate Chemical compound CCCCCCCCCCCCCCCC([O-])=O IPCSVZSSVZVIGE-UHFFFAOYSA-M 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000000338 in vitro Methods 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- OJMMVQQUTAEWLP-KIDUDLJLSA-N lincomycin Chemical compound CN1C[C@H](CCC)C[C@H]1C(=O)N[C@H]([C@@H](C)O)[C@@H]1[C@H](O)[C@H](O)[C@@H](O)[C@@H](SC)O1 OJMMVQQUTAEWLP-KIDUDLJLSA-N 0.000 description 1
- 229960005287 lincomycin Drugs 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- QEVHRUUCFGRFIF-MDEJGZGSSA-N reserpine Chemical compound O([C@H]1[C@@H]([C@H]([C@H]2C[C@@H]3C4=C(C5=CC=C(OC)C=C5N4)CCN3C[C@H]2C1)C(=O)OC)OC)C(=O)C1=CC(OC)=C(OC)C(OC)=C1 QEVHRUUCFGRFIF-MDEJGZGSSA-N 0.000 description 1
- 208000013223 septicemia Diseases 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000011003 system suitability test Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
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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
-
- 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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
-
- 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
- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
- G01N30/8631—Peaks
- G01N30/8634—Peak quality criteria
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
- G01N2030/047—Standards external
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
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- 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)
- Engineering & Computer Science (AREA)
- Quality & Reliability (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for detecting the content of clindamycin palmitate hydrochloride, which adopts a high performance liquid chromatography to detect the content of clindamycin palmitate hydrochloride and comprises the following steps: (1) performing a system adaptability test to determine the theoretical plate number and the separation degree of the chromatogram; (2) determining the linear range of the high performance liquid chromatography detection; (3) performing a repeatability test to determine the precision of the high performance liquid chromatography; (4) performing a recovery test to determine the accuracy of the high performance liquid chromatography; (5) and detecting the content of the clindamycin palmitate hydrochloride. The method provided by the invention has the advantages that the number of theoretical plates is more than 3000, the separation degree is more than 1.89, and the precision and the accuracy are better, so that the method can determine that the content of the clindamycin palmitate hydrochloride can be accurately detected by the high performance liquid chromatography provided by the invention.
Description
Technical Field
The invention relates to the field of quality control of raw material medicines, in particular to a method for detecting the content of clindamycin palmitate hydrochloride.
Background
Clindamycin Palmitate Hydrochloride (CPH) is a derivative of clindamycin, is a novel lincomycin antibiotic, and is a water-soluble hydrochloride of clindamycin and palmitate.
The clindamycin palmitate hydrochloride has no activity in vitro, can be quickly converted into clindamycin with antibacterial activity in vivo, has higher antibacterial action, and has activity on gram-positive aerobic bacteria, anaerobic bacillus, chlamydia and mycoplasma. The traditional Chinese medicine composition is widely used for treating septicemia caused by sensitive bacteria, bacterial intima, respiratory tract infection, soft tissue infection, bone joint infection, ear infection and urogenital infection in clinic.
The clindamycin palmitate hydrochloride raw material medicine is an active ingredient for preparing the clindamycin palmitate hydrochloride medicinal preparation, and for the purpose of controlling the quality of the medicine, the content of the clindamycin palmitate hydrochloride in the raw material medicine needs to be detected.
Disclosure of Invention
In view of the above, the invention provides a method for detecting the content of clindamycin palmitate hydrochloride.
The specific technical scheme is as follows:
the invention provides a method for detecting the content of clindamycin palmitate hydrochloride, which adopts a high performance liquid chromatography to detect the content of clindamycin palmitate hydrochloride in a clindamycin palmitate hydrochloride raw material medicine, and comprises the following steps:
(1) performing a system adaptability test to determine the theoretical plate number and the separation degree of the chromatogram;
(2) determining the linear range of the high performance liquid chromatography detection;
(3) performing a repeatability test to determine the precision of the high performance liquid chromatography;
(4) performing a recovery test to determine the accuracy of the high performance liquid chromatography;
(5) under the conditions that the theoretical plate number is more than 3000, the separation degree is more than 1.5, and the RSD of precision and accuracy is less than 2.0, detecting the content of the clindamycin palmitate hydrochloride by adopting the high performance liquid chromatography within a determined linear range;
wherein the stationary phase of the high performance liquid chromatography is octadecylsilane chemically bonded silica, and the mobile phase is ammonium acetate solution-0.21% dioctyl sodium sulfosuccinate methanol solution.
In some embodiments of the invention, the volume ratio of the ammonium acetate solution to the 0.21% sodium dioctyl sulfosuccinate in methanol is 20: 480.
In some embodiments of the invention, the high performance liquid chromatography employs isocratic elution.
In some embodiments of the invention, step (5) comprises
Preparing a test solution of clindamycin palmitate hydrochloride raw material medicine and a reference solution of clindamycin palmitate hydrochloride by using a mobile phase;
respectively injecting the test solution and the reference solution into a liquid chromatograph, and recording a chromatogram;
respectively measuring peak areas A of clindamycin palmitate hydrochloride in chromatogram of test solutionFor supplying toAnd peak area A of clindamycin palmitate hydrochloride in chromatogram of control solutionTo pairDetermining the concentration C of clindamycin palmitate hydrochloride in the test solution according to the following formulaFor supplying to：
CFor supplying to＝(AFor supplying to/ATo pair)*CTo pairWherein, CTo pairThe concentration of the clindamycin palmitate hydrochloride in the reference solution is shown;
according to CFor supplying toDetermining the content of the clindamycin palmitate hydrochloride in the clindamycin palmitate hydrochloride raw material medicine.
In some embodiments of the invention, the concentration of the test solution and the control solution is the same.
In some embodiments of the invention, the concentration of the clindamycin palmitate hydrochloride drug substance in the test solution is 4.517mg/ml to 67.749 mg/ml.
In some embodiments of the invention, the concentration of the clindamycin palmitate hydrochloride drug substance in the test solution is 18 mg/ml.
In some embodiments of the invention, the sample volumes of the test solution and the control solution are 20 μ l each.
Advantageous effects
According to the method, the content of the clindamycin palmitate hydrochloride in the clindamycin palmitate hydrochloride raw material medicine is detected by adopting a high performance liquid chromatography, and according to measurement data, the number of theoretical plates is more than 3000 by calculating the main component clindamycin palmitate hydrochloride peak, the separation degree is more than 1.89, and the good separation of the related material peak and the main component peak is ensured. In addition, the method has better precision and accuracy, so that the content of the clindamycin palmitate hydrochloride in the clindamycin palmitate hydrochloride raw material medicine can be accurately detected by the high performance liquid chromatography provided by the invention, and a basis is provided for quality control of the clindamycin palmitate hydrochloride medicinal preparation.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, the technical solutions of the present application will be clearly and completely described below through specific embodiments.
In the following examples, those not indicated with specific conditions were performed according to conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1 System suitability test
Chromatographic conditions
The instrument comprises the following steps: shimadzu LC-9A high performance liquid chromatograph;
shimadzu RID-10A shows a differential refractive detector; JS-3050 chromatographic work station;
a chromatographic column: HYPERSIL ODS2(4.6 mm. times.200 mm, 5 μm);
mobile phase: ammonium acetate solution-0.21% dioctyl sodium sulfosuccinate methanol solution (20: 480);
flow rate: 1.0 ml/min;
sample introduction amount: 20 mu l of the mixture;
wherein, the ammonium acetate solution is prepared by the following method: 3.85g of ammonium acetate is taken and dissolved by adding 5 percent acetic acid solution and diluted to 100 ml.
Procedure of the test
Taking a proper amount of clindamycin palmitate hydrochloride reference substance, precisely weighing, dissolving and diluting with a mobile phase to prepare a solution containing about 18mg per 1ml, shaking up, precisely weighing 20 mu l, injecting into a liquid chromatograph, recording a chromatogram, and repeatedly injecting for 5 times; and calculating the number of theoretical plates, the separation degree and the relative standard deviation of repeated sample injection. The results are shown in the following table:
according to the measurement data, the theoretical plate number is more than 3000 calculated by the main component clindamycin hydrochloride palmitate peak, the related substance peak and the main component peak are well separated, the relative standard deviation of repeated sample injection is 0.65%, and the system requirements are met.
EXAMPLE 2 determination of Linear Range
Preparation of stock solutions
2.2583g of clindamycin palmitate hydrochloride reference substance is precisely weighed and placed in a 25ml measuring flask. Dissolving with mobile phase, diluting to scale, and shaking. Each 1ml of the solution contains 90.332mg of clindamycin palmitate hydrochloride control.
Preparation of test solutions
Precisely measuring the stock solutions 0.5 ml, 1.0ml, 2.0 ml, 4.0 ml and 7.5ml, respectively diluting with mobile phase to 10ml measuring flask, shaking up, and preparing into test solution with a series of concentrations. Respectively and precisely measuring 20 mul of the test solution, injecting into a liquid chromatograph, and recording the chromatogram. The test results are given in the following table:
clindamycin palmitate hydrochloride linear range test result
The test result shows that: the clindamycin palmitate hydrochloride has good linear relation in the concentration range of 4.517 mg/ml-67.749 mg/ml.
EXAMPLE 3 repeatability test
Taking a proper amount of clindamycin palmitate hydrochloride reference substance, precisely weighing 6 parts, placing the 6 parts in 10ml measuring flasks, dissolving and diluting the measuring flasks to scales by using the mobile phase, shaking up, precisely weighing 20 mu l, injecting the solution into a liquid chromatograph, and recording a chromatogram; the content of each sample is calculated by peak area according to an external standard method, and the test results are as follows:
results of the repeatability test
| Serial number | 1 | 2 | 3 | 4 | 5 | 6 | Mean value of | RSD％ |
| Content (%) | 58.24 | 58.69 | 58.03 | 57.78 | 58.17 | 58.87 | 58.30 | 0.70 |
As can be seen from the repeatability tests, the precision of the high performance liquid chromatography of the invention meets the relevant requirements.
Example 4 recovery test
1.8262g of a test sample (clindamycin palmitate hydrochloride content: 60.4%) is put into a 10ml measuring flask, dissolved and diluted to the scale by a mobile phase, and 9 parts of 1.0ml of the test sample are precisely weighed and put into the 10ml measuring flask. Another 1.8186g of control was placed in a 10ml measuring flask, dissolved in the mobile phase and diluted to the mark. Then precisely adding the prepared reference substance solutions into the test sample with known content according to three different concentrations, namely low, medium and high, diluting to scale with mobile phase, and shaking up. Measuring 20 μ l of the extract, injecting into a liquid chromatograph, recording chromatogram, taking appropriate amount of reference substance, measuring by the same method, calculating by external standard method according to peak area, and determining recovery rate, with the following results:
recovery rate test meter for low, medium and high concentration
As can be seen from the recovery rate test, the accuracy of the high performance liquid chromatography of the invention meets the relevant requirements.
Example 5 detection of clindamycin palmitate hydrochloride drug substance
Taking 3 batches of samples of clindamycin palmitate hydrochloride raw material medicine prepared by the company, and carrying out content determination according to the content detection method and conditions prepared in the above embodiment. The specific detection process is as follows:
preparing a test solution of clindamycin palmitate hydrochloride raw material drug with the concentration of 18mg/ml and a reference solution of clindamycin palmitate hydrochloride by using a mobile phase;
injecting 20 μ l of the test solution and the reference solution into a liquid chromatograph, and recording chromatograms;
respectively measuring peak areas A of clindamycin palmitate hydrochloride in chromatogram of test solutionFor supplying toAnd peak area A of clindamycin palmitate hydrochloride in chromatogram of control solutionTo pairDetermining the concentration C of clindamycin palmitate hydrochloride in the test solution according to the following formulaFor supplying to：
CFor supplying to＝(AFor supplying to/ATo pair)*CTo pairWherein, CTo pairThe concentration of the clindamycin palmitate hydrochloride in the reference solution is shown;
according to CFor supplying toDetermining the content of the clindamycin palmitate hydrochloride in the clindamycin palmitate hydrochloride raw material medicine.
The results of the 3 sample runs are shown in the following table:
results of assay of 3 batches of samples
| Sample batch number | 0801 | 0802 | 0803 |
| Content (%) | 58.33 | 57.29 | 57.46 |
Through the tests, the verification of the content determination method and the actual determination of the sample, the result shows that the determination method provided by the invention is feasible and can accurately control the quality of the product.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (8)
1. A method for detecting the content of clindamycin palmitate hydrochloride is characterized in that the content of clindamycin palmitate hydrochloride in a clindamycin palmitate hydrochloride raw material medicine is detected by adopting a high performance liquid chromatography, and the method comprises the following steps:
(1) performing a system adaptability test to determine the theoretical plate number and the separation degree of the chromatogram;
(2) determining the linear range of the high performance liquid chromatography detection;
(3) performing a repeatability test to determine the precision of the high performance liquid chromatography;
(4) performing a recovery test to determine the accuracy of the high performance liquid chromatography;
(5) under the conditions that the theoretical plate number is more than 3000, the separation degree is more than 1.5, and the RSD of precision and accuracy is less than 2.0, detecting the content of the clindamycin palmitate hydrochloride by adopting the high performance liquid chromatography within a determined linear range;
wherein the stationary phase of the high performance liquid chromatography is octadecylsilane chemically bonded silica, and the mobile phase is ammonium acetate solution-0.21% dioctyl sodium sulfosuccinate methanol solution.
2. The content detection method according to claim 1, wherein the volume ratio of the ammonium acetate solution to the 0.21% dioctyl sodium sulfosuccinate methanol solution is 20: 480.
3. The method according to claim 1, wherein the high performance liquid chromatography uses isocratic elution.
4. The content detection method according to any one of claims 1 to 3, wherein the step (5) comprises
Preparing a test solution of clindamycin palmitate hydrochloride raw material medicine and a reference solution of clindamycin palmitate hydrochloride by using a mobile phase;
respectively injecting the test solution and the reference solution into a liquid chromatograph, and recording a chromatogram;
respectively measuring peak areas A of clindamycin palmitate hydrochloride in chromatogram of test solutionFor supplying toAnd peak area A of clindamycin palmitate hydrochloride in chromatogram of control solutionTo pairDetermining the concentration C of clindamycin palmitate hydrochloride in the test solution according to the following formulaFor supplying to：
CFor supplying to＝(AFor supplying to/ATo pair)*CTo pairWherein, CTo pairThe concentration of the clindamycin palmitate hydrochloride in the reference solution is shown;
according to CFor supplying toDetermining the content of the clindamycin palmitate hydrochloride in the clindamycin palmitate hydrochloride raw material medicine.
5. The method of claim 4, wherein the concentrations of the test solution and the control solution are the same.
6. The method of claim 5, wherein the concentration of the clindamycin palmitate hydrochloride drug substance in the test solution is 4.517mg/ml to 67.749 mg/ml.
7. The method of claim 6, wherein the concentration of the clindamycin palmitate hydrochloride drug substance in the test solution is 18 mg/ml.
8. The method of claim 4, wherein the sample volumes of the test solution and the control solution are 20 μ l each.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101062018A (en) * | 2007-05-30 | 2007-10-31 | 西南合成制药股份有限公司 | Hydrochloride clindamycin palmitate soft capsule and the preparing method thereof |
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