CN116165289A - Method for measuring hydroxypropyl cellulose content - Google Patents
Method for measuring hydroxypropyl cellulose content Download PDFInfo
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- CN116165289A CN116165289A CN202211634853.1A CN202211634853A CN116165289A CN 116165289 A CN116165289 A CN 116165289A CN 202211634853 A CN202211634853 A CN 202211634853A CN 116165289 A CN116165289 A CN 116165289A
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- hydroxypropyl cellulose
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- 229920002153 Hydroxypropyl cellulose Polymers 0.000 title claims abstract description 61
- 239000001863 hydroxypropyl cellulose Substances 0.000 title claims abstract description 61
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000013353 HPLC-CAD method Methods 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 239000013558 reference substance Substances 0.000 claims abstract description 12
- 239000012488 sample solution Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000005303 weighing Methods 0.000 claims abstract description 8
- 239000003495 polar organic solvent Substances 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 238000007865 diluting Methods 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 4
- 239000000523 sample Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 23
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 238000010828 elution Methods 0.000 claims description 3
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000012074 organic phase Substances 0.000 claims description 3
- 239000012071 phase Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 239000000741 silica gel Substances 0.000 claims description 2
- 229910002027 silica gel Inorganic materials 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 10
- 239000003814 drug Substances 0.000 abstract description 5
- 238000002203 pretreatment Methods 0.000 abstract description 2
- 229940079593 drug Drugs 0.000 abstract 1
- OFQCQIGMURIECL-UHFFFAOYSA-N 2-[2-(diethylamino)ethyl]-2',6'-dimethylspiro[isoquinoline-4,4'-oxane]-1,3-dione;phosphoric acid Chemical compound OP(O)(O)=O.O=C1N(CCN(CC)CC)C(=O)C2=CC=CC=C2C21CC(C)OC(C)C2 OFQCQIGMURIECL-UHFFFAOYSA-N 0.000 description 4
- 238000005259 measurement Methods 0.000 description 3
- 239000012088 reference solution Substances 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 229940071870 hydroiodic acid Drugs 0.000 description 1
- FMKOJHQHASLBPH-UHFFFAOYSA-N isopropyl iodide Chemical compound CC(C)I FMKOJHQHASLBPH-UHFFFAOYSA-N 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000546 pharmaceutical excipient Substances 0.000 description 1
- 229940124531 pharmaceutical excipient Drugs 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 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
-
- 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
- G01N30/64—Electrical 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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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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)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to the technical field of drug detection, in particular to a method for measuring the content of hydroxypropyl cellulose, which comprises the following steps: weighing high-substituted hydroxypropyl cellulose, preparing hydroxypropyl cellulose solution by using water or polar organic solvent as solvent, and diluting to obtain series of hydroxypropyl cellulose reference substance solutions with different concentrations; grinding a preparation sample, weighing fine powder, extracting in water bath, and preparing into corresponding sample solution; detecting a series of hydroxypropyl cellulose reference substance solutions by using an HPLC-CAD method, and drawing a standard curve; and (3) measuring the sample solution with the target concentration by using an HPLC-CAD method, acquiring target peak information, and calculating the content of hydroxypropyl cellulose in the sample solution by using an external standard curve method. The pretreatment method has simple pretreatment steps, can detect the content of the hydroxypropyl cellulose, and can reflect model differences; the detection result has high accuracy and precision and repeatability.
Description
Technical Field
The invention relates to the technical field of medicine detection, in particular to a method for measuring the content of hydroxypropyl cellulose.
Background
In the research and development process of the simulated medicine, detailed research is required to be carried out on the reference preparation, wherein most auxiliary materials have no clinical activity but influence the performance of the medicine product, such as stability, hardness, dissolution rate and the like, so that the reverse analysis of the auxiliary materials in the reference preparation and the determination of the types and the contents of the auxiliary materials have important guiding significance for the research and development of the simulated medicine. Hydroxypropyl cellulose, which is a macromolecular pharmaceutical excipient with a molecular weight ranging from thousands to hundreds of megabits, is a mixture of non-single components, is mainly used as an adhesive and a disintegrating agent, and is widely applied to oral capsules and tablets, and local and transdermal absorption preparations.
The current method for measuring the content of the hydroxypropyl cellulose mainly refers to four general rules of the edition 2020 of Chinese pharmacopoeia, and generally adopts a gas chromatography or a volumetric method to measure the content of the hydroxypropyl radical. Because the pharmaceutical preparation product often has complex components, the sample treatment process has complicated steps, long time consumption and poor accuracy of the measurement result. In the prior art, the measuring method has complex device and strong corrosiveness of reagent hydroiodic acid used in the gas chromatography, and the contrast 2-iodopropane is extremely volatile and easy to be degraded, and the marking needs to be carried out before each measurement. In addition, the prior art can only measure the content of hydroxypropyl cellulose, and cannot compare specific model differences.
Disclosure of Invention
The present invention is directed to a method for determining the content of hydroxypropyl cellulose, which solves the above-mentioned problems of the prior art.
The invention is realized by the following technical scheme:
a method for determining the content of hydroxypropyl cellulose comprising the steps of:
s1, weighing high-substituted hydroxypropyl cellulose, preparing hydroxypropyl cellulose solution by taking water or a polar organic solvent as a solvent, and diluting to obtain series of hydroxypropyl cellulose reference substance solutions with different concentrations;
s2, taking an auxiliary material containing the preparation sample of the high-substituted hydroxypropyl cellulose in the step S1, grinding, weighing fine powder, extracting in a water bath, and preparing a corresponding sample solution;
s3, detecting the series of hydroxypropyl cellulose reference substance solutions obtained in the step S1 by using an HPLC-CAD method to obtain the peak area of hydroxypropyl cellulose in the reference substance solutions, and performing standard curve fitting with the concentration of the reference substance solutions;
s4, determining a sample solution with target concentration by using an HPLC-CAD method, acquiring target peak information, and calculating the content of hydroxypropyl cellulose in the sample solution by using an external standard curve method;
in the above steps, the HPLC-CAD method employs a column packed with octadecyl-bonded silica gel.
As a further aspect of the present invention, the parameters of the HPLC-CAD method are specifically: and performing gradient elution at the temperature of 40-80 ℃ and the flow rate of 0.3-0.8 mL/min by taking acetonitrile/methanol-water system as mobile phase, wherein the volume percentage of the organic phase is 0-90%, the chromatographic column adopts Presto FF-C18 chromatographic column, CAD is adopted as detector.
In the step S1, the content of the hydroxypropyl cellulose solution before dilution is 5wt.%, and the viscosity of the prepared hydroxypropyl cellulose solution is 500cps, 250cps and 100cps respectively according to the type of the hydroxypropyl cellulose.
As a further aspect of the present invention, in step S1, the concentration of the series of hydroxypropylcellulose control solutions was 3.775. Mu.g/mL, 15.1. Mu.g/mL, 37.75. Mu.g/mL, 75.5. Mu.g/mL, 113.25. Mu.g/mL, 151. Mu.g/mL, respectively.
Preferably, the polar organic solvent comprises at least one of acetonitrile, methanol, ethanol, isopropanol.
Compared with the prior art, the invention has the beneficial effects that:
the HPLC-CAD method can be used for detecting the content of the hydroxypropyl cellulose and reflecting model differences. The method provided by the invention has the advantages of simple pretreatment steps, high accuracy and precision of the detection result and repeatability.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described, and it is possible for a person skilled in the art to obtain other drawings from these drawings without inventive effort.
FIG. 1 is a standard graph of a hydroxypropyl cellulose control solution of the present invention;
FIG. 2 is a graph showing the detection patterns of different types of hydroxypropyl cellulose according to the present invention;
FIG. 3 is a graph showing the detection of hydroxypropyl cellulose in samples of different formulations of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Unless otherwise specified, the reagents used in the examples were all readily available from commercial companies.
Example 1:
the embodiment provides a method for determining the content of hydroxypropyl cellulose, which specifically comprises the following steps:
s1, weighing high-substituted hydroxypropyl cellulose of different types, and preparing into hydroxypropyl cellulose solution with the content of 5wt.% by taking water or a polar organic solvent as a solvent. Since the solvent has a small influence on the measurement method of the embodiment, the polar organic solvent is methanol, ethanol or isopropanol, and the subsequent hydroxypropyl cellulose content measurement is not influenced.
According to different types of the hydroxypropyl cellulose, the prepared hydroxypropyl cellulose solution has the viscosity of 500cps (model 1), 250cps (model 2) and 100cps (model 3) respectively; taking hydroxypropyl cellulose solution with the viscosity of 500cps (model 1), and diluting to obtain a series of hydroxypropyl cellulose reference substance solutions with the concentration of 3.775 mug/mL, 15.1 mug/mL, 37.75 mug/mL, 75.5 mug/mL, 113.25 mug/mL and 151 mug/mL respectively;
s2, taking preparation samples (preparation I and preparation II) from different manufacturers, wherein the preparation I and the preparation II belong to the same variety and all auxiliary materials are the same, grinding the preparation samples, weighing fine powder, extracting in a water bath, and preparing corresponding sample solutions;
s3, setting parameters of an HPLC-CAD method as follows: performing gradient elution by taking acetonitrile/methanol-water system as mobile phase, wherein the volume percentage of the organic phase is 0-90%, and the specific gradient procedure is shown in table 1; the chromatographic column adopts a Presto FF-C18 chromatographic column, adopts CAD as a detector, has the column temperature of 40-80 ℃ and the flow rate of 0.3-0.8 mL/min;
table 1:
| Time | water and its preparation method | Acetonitrile/ |
| 0min | ||
| 100％ | 0％ | |
| |
10％ | 90％ |
| 20.1 |
100％ | 0％ |
| |
100％ | 0％ |
By means ofDetecting the series of hydroxypropyl cellulose (model 1) reference solution obtained in the step S1 by HPLC-CAD method to obtain peak area of hydroxypropyl cellulose in the reference solution, wherein specific data are shown in Table 2, and performing standard curve fitting with concentration of the reference solution to obtain standard curve with formula of y=0.1671x+0.5421, R 2 =0.9985, the fitted standard curve is shown in fig. 1, and the result shows that hydroxypropyl cellulose shows a good linear relationship in the concentration range;
table 2:
s4, respectively measuring the hydroxypropyl cellulose of the model 1-3, the reference substance solution and the sample solutions of the preparation I and the preparation II by using an HPLC-CAD method, obtaining target peak information, and calculating the content of the hydroxypropyl cellulose in the sample solution by using an external standard curve method, wherein the detection result is shown in the figure 2-3. As can be seen from fig. 2-3, the hydroxypropyl cellulose of each model is quite different.
Taking a preparation II with the same model, adding a control solution of hydroxypropyl cellulose (model 1) with a set concentration, detecting the content of the hydroxypropyl cellulose by the method, wherein the detection data are shown in a table 3, and calculating the recovery rate according to the detected data.
Table 3:
the HPLC-CAD pretreatment method provided by the invention has simple steps, can detect the content of hydroxypropyl cellulose, and can reflect model differences. As can be seen from Table 3, the detection method provided by the invention has high accuracy and precision of detection results and repeatability.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (5)
1. A method for determining the content of hydroxypropyl cellulose, comprising the steps of:
s1, weighing high-substituted hydroxypropyl cellulose, preparing hydroxypropyl cellulose solution by taking water or a polar organic solvent as a solvent, and diluting to obtain series of hydroxypropyl cellulose reference substance solutions with different concentrations;
s2, taking an auxiliary material containing the preparation sample of the high-substituted hydroxypropyl cellulose in the step S1, grinding, weighing fine powder, extracting in a water bath, and preparing a corresponding sample solution;
s3, detecting the series of hydroxypropyl cellulose reference substance solutions obtained in the step S1 by using an HPLC-CAD method, obtaining the peak area of hydroxypropyl cellulose in the reference substance solutions, and drawing a reference substance solution standard curve;
s4, determining a sample solution with target concentration by using an HPLC-CAD method, acquiring target peak information, and calculating the content of hydroxypropyl cellulose in the sample solution by using an external standard curve method;
in the above steps, the HPLC-CAD method employs a column packed with octadecyl-bonded silica gel.
2. A method for determining the content of hydroxypropyl cellulose according to claim 1, characterized in that the parameters of the HPLC-CAD method are in particular: and performing gradient elution by taking an acetonitrile/methanol-water system as a mobile phase, wherein the volume percentage of an organic phase is 0-90%, a chromatographic column adopts a Presto FF-C18 chromatographic column, CAD is adopted as a detector, the column temperature is 40-80 ℃, and the flow rate is 0.3-0.8 mL/min.
3. A method for determining the content of hydroxypropyl cellulose according to claim 1, characterized in that in step S1 the content of hydroxypropyl cellulose solution before dilution is 5wt.%.
4. A method for determining the content of hydroxypropyl cellulose according to claim 3, characterized in that in step S1, the concentration of the series of hydroxypropyl cellulose control solutions is 3.775 μg/mL, 15.1 μg/mL, 37.75 μg/mL, 75.5 μg/mL, 113.25 μg/mL, 151 μg/mL, respectively.
5. A method for determining the content of hydroxypropyl cellulose according to any of claims 1-4, characterized in that the polar organic solvent comprises at least one of acetonitrile, methanol, ethanol, isopropanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211634853.1A CN116165289A (en) | 2022-12-19 | 2022-12-19 | Method for measuring hydroxypropyl cellulose content |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211634853.1A CN116165289A (en) | 2022-12-19 | 2022-12-19 | Method for measuring hydroxypropyl cellulose content |
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| Publication Number | Publication Date |
|---|---|
| CN116165289A true CN116165289A (en) | 2023-05-26 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211634853.1A Pending CN116165289A (en) | 2022-12-19 | 2022-12-19 | Method for measuring hydroxypropyl cellulose content |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116165289A (en) |
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2022
- 2022-12-19 CN CN202211634853.1A patent/CN116165289A/en active Pending
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