CN115219630A - Method for determining related substances of berberine trimethoprim capsule - Google Patents
Method for determining related substances of berberine trimethoprim capsule Download PDFInfo
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- CN115219630A CN115219630A CN202210879004.6A CN202210879004A CN115219630A CN 115219630 A CN115219630 A CN 115219630A CN 202210879004 A CN202210879004 A CN 202210879004A CN 115219630 A CN115219630 A CN 115219630A
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- 238000000034 method Methods 0.000 title claims abstract description 50
- IEDVJHCEMCRBQM-UHFFFAOYSA-N trimethoprim Chemical compound COC1=C(OC)C(OC)=CC(CC=2C(=NC(N)=NC=2)N)=C1 IEDVJHCEMCRBQM-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229960001082 trimethoprim Drugs 0.000 title claims abstract description 41
- 239000002775 capsule Substances 0.000 title claims abstract description 40
- YBHILYKTIRIUTE-UHFFFAOYSA-N berberine Chemical compound C1=C2CC[N+]3=CC4=C(OC)C(OC)=CC=C4C=C3C2=CC2=C1OCO2 YBHILYKTIRIUTE-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229940093265 berberine Drugs 0.000 title claims abstract description 38
- QISXPYZVZJBNDM-UHFFFAOYSA-N berberine Natural products COc1ccc2C=C3N(Cc2c1OC)C=Cc4cc5OCOc5cc34 QISXPYZVZJBNDM-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 239000000126 substance Substances 0.000 title claims abstract description 32
- 239000012535 impurity Substances 0.000 claims abstract description 29
- 238000010828 elution Methods 0.000 claims abstract description 14
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001514 detection method Methods 0.000 claims abstract description 11
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 8
- WGZCUXZFISUUPR-UHFFFAOYSA-N acetonitrile;oxolane Chemical compound CC#N.C1CCOC1 WGZCUXZFISUUPR-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims abstract description 4
- 235000019796 monopotassium phosphate Nutrition 0.000 claims abstract description 4
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims abstract description 4
- VKJGBAJNNALVAV-UHFFFAOYSA-M Berberine chloride (TN) Chemical compound [Cl-].C1=C2CC[N+]3=CC4=C(OC)C(OC)=CC=C4C=C3C2=CC2=C1OCO2 VKJGBAJNNALVAV-UHFFFAOYSA-M 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 20
- 239000012085 test solution Substances 0.000 claims description 18
- 239000000047 product Substances 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 7
- 239000012088 reference solution Substances 0.000 claims description 7
- 239000012488 sample solution Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 239000013558 reference substance Substances 0.000 claims description 5
- 239000000523 sample Substances 0.000 claims description 5
- 238000007865 diluting Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000010812 external standard method Methods 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000008187 granular material Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
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- 238000002474 experimental method Methods 0.000 description 6
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- 238000003908 quality control method Methods 0.000 description 4
- 230000006378 damage Effects 0.000 description 3
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- 238000012360 testing method Methods 0.000 description 3
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- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000011002 quantification Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- 206010067484 Adverse reaction Diseases 0.000 description 1
- 208000004429 Bacillary Dysentery Diseases 0.000 description 1
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- 208000019872 Drug Eruptions Diseases 0.000 description 1
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- 206010017915 Gastroenteritis shigella Diseases 0.000 description 1
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- 201000010099 disease Diseases 0.000 description 1
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- 238000004090 dissolution Methods 0.000 description 1
- 229940088679 drug related substance Drugs 0.000 description 1
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- 230000002195 synergetic effect Effects 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 230000008673 vomiting Effects 0.000 description 1
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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
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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
- G01N30/26—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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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Abstract
The invention discloses a method for determining related substances of a berberine trimethoprim capsule, which adopts a gradient elution HPLC method, adopts a KROMASIL-C18 chromatographic column, takes 0.05mol/L potassium dihydrogen phosphate solution containing 0.1 percent triethylamine as a mobile phase A, and takes acetonitrile-tetrahydrofuran with the volume ratio of 4; an ultraviolet detector is adopted to detect the related substances of the berberine trimethoprim capsule with the detection wavelength of 280nm, belonging to the technical field of medicine detection. The method for measuring related substances of the berberine trimethoprim capsule is simple and convenient to operate, high in sensitivity, good in specificity and accurate in result, can quickly and simultaneously measure a plurality of impurities of the berberine trimethoprim capsule, makes up for the quality standard defect of the variety, can further effectively control the medicine quality of the berberine trimethoprim capsule, improves the quality level of the medicine, and ensures the clinical medication safety.
Description
Technical Field
The invention belongs to the technical field of medicine detection, and particularly relates to a method for determining related substances of a berberine trimethoprim capsule.
Background
The berberine trimethoprim capsule is named as a synergistic berberine capsule, is a compound preparation, contains 100 mg of berberine hydrochloride and 50 mg of trimethoprim per capsule, and is mainly used for diseases such as gastroenteritis, bacillary dysentery and the like caused by sensitive bacteria. The adverse reactions include nausea, vomiting, drug eruption, diarrhea, etc. The existing standard of the berberine trimethoprim capsule is the eleventh volume of the national standard which is increased from the local standard of chemical medicines in the national standard, the content determination method of berberine hydrochloride in the national standard is an HPLC method, and the content determination method of trimethoprim is an extraction-ultraviolet spectrophotometry method; the current standard is provided with defects: the related substances are not controlled; dissolution was not controlled; the existing HPLC content determination method for berberine hydrochloride cannot effectively separate main components from impurities; the trimethoprim content measuring method is complex to operate, low in accuracy and large in error.
The related substances refer to starting materials, intermediates, polymers, side reaction products brought in during production, degradation products in storage and the like. Related substances are closely related to the quality, safety and curative effect of the medicine, and the pharmacological activity, metabolic process and toxicity of the chemical medicine containing impurities in a human body have obvious difference; therefore, the control of the drug-related substance is extremely important. Related substances are the items which must be detected by most medicines, and related substance examination items are not included in the current standard of the berberine trimethoprim capsule, which is not beneficial to the quality control of products. Therefore, the method for determining related substances of the berberine trimethoprim capsule is established, the related substances in the berberine trimethoprim capsule are effectively and comprehensively detected, and the method has very important significance for further quality control of the berberine trimethoprim capsule.
Disclosure of Invention
The invention aims to provide a method for measuring related substances of a berberine trimethoprim capsule, which aims at overcoming the defects of the prior art, has the advantages of simple and convenient operation, high sensitivity, good specificity and accurate result, can quickly and simultaneously measure a plurality of impurities of the berberine trimethoprim capsule, is effective and comprehensive, makes up for the quality standard defects of the variety, can further effectively control the medicine quality of the berberine trimethoprim capsule and improve the quality level of the medicine, and has a positive effect on improving the safety of the medicine.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for measuring related substances of a berberine trimethoprim capsule adopts a gradient elution HPLC method to measure the related substances of the berberine trimethoprim capsule, and specifically comprises the following steps:
(1) Chromatographic conditions are as follows: KROMASIL-C18 (250 mm. Times.4.6 mm,5 μm), gradient elution was carried out using a 0.05mol/L potassium dihydrogen phosphate solution containing 0.1% triethylamine as a mobile phase A and acetonitrile-tetrahydrofuran as a mobile phase B in a volume ratio of 4; gradient elution procedure: 0-40 minutes, A85%, 40-42 minutes, A85 → 75, 42-52 minutes, A75%, 52-54 minutes, A75% → 85%,54-70 minutes, A85%; the sample injection amount is 10 mu l; an ultraviolet detector is adopted, and the detection wavelength is 280nm;
(2) Solution preparation:
control solution: taking berberine hydrochloride reference substance, and preparing solution with concentration of 10 μ g/ml with mobile phase;
test solution: taking 10 granules of the product, precisely weighing, grinding, weighing the amount equivalent to 10mg of berberine hydrochloride, placing into a 10ml measuring flask, adding mobile phase for ultrasonic treatment, shaking for dissolving, cooling to room temperature, diluting with mobile phase to scale, shaking, filtering with 0.45 μm filter membrane, and taking the filtrate;
in the preparation of the reference solution and the test solution, the mobile phase is a solution obtained by mixing the mobile phases A and B according to the volume ratio of 85;
(3) And (3) determination: precisely measuring 10 μ L of reference solution and sample solution, respectively injecting into liquid chromatograph, measuring according to the above chromatographic conditions, recording chromatogram, and if impurities are detected in the sample solution, calculating according to reference external standard method, wherein the single impurity can not pass through 0.5% of berberine hydrochloride, and the total amount of impurities can not pass through 1.0% of berberine hydrochloride.
The beneficial effects of the invention are as follows:
the method for determining related substances of the berberine trimethoprim capsule by the gradient elution HPLC method is established for the first time, and a plurality of impurities of the berberine trimethoprim capsule can be sensitively, quickly and simultaneously determined by using the method, so that the method is effective and comprehensive; the method is adopted to detect a brand new impurity, namely impurity 3, of the berberine trimethoprim capsule, and the detection method is sensitive and quick and takes less time to detect. The method for determining related substances of the berberine trimethoprim capsule, which is established by the invention, makes up the deficiency of the quality standard of the variety, is a powerful supplement of the existing quality standard, and has a positive effect on improving the safety of the medicine.
The method provided by the invention is verified to prove that the method has a good linear relation in an investigation concentration range, the recovery rate meets the regulations, the method is simple and convenient to operate, high in sensitivity, good in specificity and accurate in result, and the method can be used as a quality control method for related substances of berberine trimethoprim capsules. The method can further effectively control the medicine quality of the berberine trimethoprim capsule, improve the quality level of the berberine trimethoprim capsule, ensure the controllable production process, ensure the safety of clinical medication and provide reliable guarantee for the stable and exact curative effect of the product.
Drawings
FIG. 1 chromatogram of a blank adjuvant solution for a specific experiment;
FIG. 2 chromatogram of berberine hydrochloride reference solution;
FIG. 3 is a chromatogram of a test solution of berberine trimethoprim capsule;
FIG. 4 is a chromatogram of a test solution for specified experimental oxidative damage;
FIG. 5 chromatogram of a specific test acid-breaking test solution;
FIG. 6 chromatogram of a specific test solution for alkali destruction;
FIG. 7 is a chromatogram of a specific test solution subjected to high-temperature destruction;
FIG. 8 is a chromatogram of a test solution destroyed by special experimental sunlight;
FIG. 9 is a chromatogram of a test solution destroyed by ultraviolet light irradiation for a specific experiment.
Detailed Description
The present invention will be further illustrated with reference to the accompanying drawings and specific embodiments, and the following examples are illustrative of experimental methods without specifying specific conditions, and are intended to follow conventional methods and conditions.
1. A method for measuring related substances of a berberine trimethoprim capsule adopts a gradient elution HPLC method to measure the related substances of the berberine trimethoprim capsule, and specifically comprises the following steps:
(1) Chromatographic conditions are as follows: a column, KROMASIL-C18 (250 mm. Times.4.6 mm,5 μm), gradient elution was carried out using 0.05mol/L potassium dihydrogen phosphate solution (containing 0.1% triethylamine) as a mobile phase A and acetonitrile-tetrahydrofuran (4); gradient elution procedure: 0-40 minutes, A85%, 40-42 minutes, A85 → 75, 42-52 minutes, A75%, 52-54 minutes, A75% → 85%,54-70 minutes, A85%; the sample amount is 10 mul; an ultraviolet detector is adopted, and the detection wavelength is 280nm;
(2) Solution preparation:
control solution: taking berberine hydrochloride reference substance, and preparing solution with concentration of 10 μ g/ml with mobile phase;
test solution: taking 10 granules of the product, precisely weighing, grinding, weighing the amount equivalent to 10mg of berberine hydrochloride, placing into a 10ml measuring flask, adding mobile phase ultrasound, shaking at intervals to dissolve, cooling to room temperature, diluting with mobile phase to scale, shaking uniformly, filtering with 0.45 μm filter membrane, and taking the subsequent filtrate;
in the preparation of the reference solution and the test solution, the mobile phase is a solution obtained by mixing the mobile phases A and B according to the volume ratio of 85;
(3) And (3) determination: precisely measuring 10 μ L of each of the reference solution and the sample solution, respectively injecting into a liquid chromatograph, measuring according to the above chromatographic conditions, recording chromatogram, and if impurities are detected in the sample solution, calculating according to the reference external standard method, wherein the amount of the single impurity cannot exceed 0.5% of the labeled amount of berberine hydrochloride, and the total amount of the impurities cannot exceed 1.0% of the labeled amount of berberine hydrochloride.
2. Methodology validation
The method established by the invention is researched by methodology, including special investigation (blank auxiliary materials and destructive experiments), linear relation investigation, sample injection precision, detection limit and stability and the like, and the verification result shows that the method is simple, accurate and sensitive, and can be used for controlling the quality of the product and improving the quality of the product.
2.1 Specificity experiments
A blank auxiliary material solution without main components is prepared according to a prescription, and the product is taken to be respectively subjected to oxidation, acid, alkali, high temperature and illumination damage experiments, so that a negative result sample has no interference on the determination of impurities. The destroyed impurities can be separated from the main peak, which shows that the method has good specificity. The map is shown in figures 1-9.
2.2 wavelength selection
The ultraviolet spectrogram of the main component and each impurity in the test solution is extracted, and has larger absorption at 280nm, so 280nm is selected as the measurement wavelength.
2.3 Investigation of linear relationships
The serial concentration solutions of berberine hydrochloride are prepared, and as a result, the berberine hydrochloride has a good linear relation with the peak area within the concentration range of 1.982-19.82 mug/ml, the linear equation is y = 27.8444 x +0.9530, and the correlation coefficient is 1.000.
2.4 Precision test
Taking the reference substance solution for continuous injection and measuring for 6 times. As a result, the peak area RSD was 1.05%, indicating that the precision was good.
2.5 repeatability test
The same batch of samples are taken, 6 test solutions are prepared in parallel for measurement, the content of each impurity is calculated, and the result is shown in table 1.
2.6 Stability test
A batch of test solution is taken, and peak areas are respectively measured at certain intervals. As a result, no new impurities are generated in the test solution within 24 hours, and the RSD values of the maximum impurities and the total impurity content are 0.82% and 0.51%, respectively, which indicates that the test solution is stable within 24 hours.
2.7 Measurement of detection limit and quantitative limit
Gradually diluting and measuring the berberine hydrochloride reference substance solution, determining the detection limit with S/N & lt 3 & gt and the quantification limit with S/N & lt 10 & gt, wherein the detection limit and the quantification limit are respectively 0.1189 and 0.3963 mu g/ml.
3. Determination of samples
Taking 5 batches of berberine trimethoprim capsule samples, and determining according to the determination method of related substances of the berberine trimethoprim capsule, wherein the content of the related substances is calculated by the percentage content of the marked amount of the berberine hydrochloride. The results are shown in Table 2. The results show that the quality of the samples 1 and 5 is higher than that of the other 3 batches of samples, and the detected impurities are more and the amount of the impurities is larger, and exceeds the set limit. The method can be used for controlling the quality of the berberine trimethoprim capsule.
4. Innovations of the invention
The invention establishes a brand new method for determining related substances of berberine trimethoprim capsules by a gradient elution HPLC method for the first time, detects a brand new impurity (impurity 3, the existing literature does not pay attention to, the existing literature pays more attention to impurity 6), and has the advantages of sensitivity, rapidness, less time consumption and no report in the product literature. The method can effectively control the quality of the product, is a powerful supplement of the existing quality standard, and makes up for the deficiency of the quality standard of the product.
5. Summary of the invention
At present, the content of the berberine hydrochloride trimethoprim capsule is mainly focused on in the literature, the research on related substances is less, and the measurement of the related substances by gradient elution is less common. The gradient elution determination method established for the first time can sensitively and rapidly determine a plurality of impurities of the product at the same time, makes up for the quality standard defect of the product, and has positive effect on improving the safety of the medicine. The method is verified to prove that the method has good linear relation in the range of the inspected concentration, the recovery rate conforms to the regulation, the method is simple and convenient to operate, high in sensitivity, good in specificity and accurate in result, and can be used as a quality control method for related substances of the berberine trimethoprim capsule.
Claims (2)
1. A method for measuring related substances of a berberine trimethoprim capsule is characterized in that the related substances of the berberine trimethoprim capsule are measured by a gradient elution HPLC method, and the method specifically comprises the following steps:
(1) Chromatographic conditions are as follows: a chromatographic column of KROMASIL-C18, 250mm × 4.6mm,5 μm; performing gradient elution by using 0.05mol/L potassium dihydrogen phosphate solution containing 0.1% triethylamine as a mobile phase A and acetonitrile-tetrahydrofuran with the volume ratio of 4 as a mobile phase B; gradient elution procedure: 0-40 minutes, A85%, 40-42 minutes, A85 → 75, 42-52 minutes, A75%, 52-54 minutes, A75% → 85%,54-70 minutes, A85%; the sample amount is 10 mul;
(2) Solution preparation:
control solution: taking berberine hydrochloride reference substance, and preparing solution with concentration of 10 μ g/ml with mobile phase;
test solution: taking 10 granules of the product, precisely weighing, grinding, weighing the amount equivalent to 10mg of berberine hydrochloride, placing into a 10ml measuring flask, adding mobile phase ultrasound, shaking at intervals to dissolve, cooling to room temperature, diluting with mobile phase to scale, shaking uniformly, filtering with 0.45 μm filter membrane, and taking the subsequent filtrate;
in the preparation of the reference solution and the test solution, the mobile phase is a solution obtained by mixing the mobile phases A and B according to the volume ratio of 85;
(3) And (3) determination: precisely measuring 10 μ L of reference solution and sample solution, respectively injecting into liquid chromatograph, measuring according to the above chromatographic conditions, recording chromatogram, and if impurities are detected in the sample solution, calculating according to reference external standard method, wherein the single impurity can not pass through 0.5% of berberine hydrochloride, and the total amount of impurities can not pass through 1.0% of berberine hydrochloride.
2. The method for measuring berberine trimethoprim capsule related substances according to claim 1, wherein an ultraviolet detector is adopted, and the detection wavelength is 280nm.
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