CN113049737A - Solvent for determining water content of Jinlong capsule, preparation method and application method thereof - Google Patents
Solvent for determining water content of Jinlong capsule, preparation method and application method thereof Download PDFInfo
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- CN113049737A CN113049737A CN202110267291.0A CN202110267291A CN113049737A CN 113049737 A CN113049737 A CN 113049737A CN 202110267291 A CN202110267291 A CN 202110267291A CN 113049737 A CN113049737 A CN 113049737A
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- water content
- organic solvent
- jinlong
- dimethyl sulfoxide
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- 239000002775 capsule Substances 0.000 title claims abstract description 80
- 239000009731 jinlong Substances 0.000 title claims abstract description 77
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000002904 solvent Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 84
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 72
- 239000003960 organic solvent Substances 0.000 claims abstract description 62
- 238000004448 titration Methods 0.000 claims description 27
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 17
- 239000011259 mixed solution Substances 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 4
- 238000009472 formulation Methods 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 13
- 238000005259 measurement Methods 0.000 description 6
- 239000011265 semifinished product Substances 0.000 description 6
- 241000271039 Agkistrodon Species 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 241000272074 Bungarus Species 0.000 description 2
- 150000001413 amino acids Chemical class 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 150000002772 monosaccharides Chemical class 0.000 description 2
- 229920001282 polysaccharide Polymers 0.000 description 2
- 239000005017 polysaccharide Substances 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 241000271897 Viperidae Species 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 208000026106 cerebrovascular disease Diseases 0.000 description 1
- 230000002526 effect on cardiovascular system Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 229920001184 polypeptide Polymers 0.000 description 1
- 102000004196 processed proteins & peptides Human genes 0.000 description 1
- 108090000765 processed proteins & peptides Proteins 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
- G01N31/168—Determining water content by using Karl Fischer reagent
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Molecular Biology (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention relates to a solvent for determining water content of Jinlongjiao capsules, a preparation method and an application method thereof, wherein the organic solvent comprises absolute methanol and dimethyl sulfoxide; the mass percentage of the anhydrous methanol is 50-80%; the content of dimethyl sulfoxide is 20-50%. 50-80% of absolute ethyl alcohol and 20-50% of dimethyl sulfoxide are mixed and then used as an organic solvent for dissolving the Jinlong capsule, and compared with the method that only absolute ethyl alcohol is used as the organic solvent, the solubility of the Jinlong capsule in the organic solvent is greatly improved, so that the Jinlong capsule is dissolved in the organic solvent as much as possible, and the accuracy of the water content determination result of the Jinlong capsule is improved.
Description
Technical Field
The invention relates to the technical field of water content determination of Jinlong capsules, in particular to a solvent for determining water content of Jinlong capsules, a preparation method and an application method thereof.
Background
A Chinese medicine in the form of capsule for treating cardiovascular and cerebrovascular diseases is prepared from semi-finished product of Jinlong capsule, fresh gecko, fresh Bungarus Parvus and fresh Agkistrodon. It is composed ofThe main components comprise proteins, polypeptides, amino acids, free monosaccharides, polysaccharides, micromolecular substances and the like. The Jinlong capsule is used as a modern fresh medicine, takes animals with medicinal value as raw materials, breaks through the processes of baking, steaming, boiling and the like of the traditional medicine, and greatly reserves the effective components in the extract by utilizing the modern technical means of low-temperature crushing, cell freeze-thaw crushing, molecular fractionation, reverse osmosis concentration and the like, so that the great bioactivity of each effective component and the better natural proportion among the effective components can be reserved. The molecular weight of the Jinlong capsule is less than 1 multiplied by 104The content of the substances reaches more than 98 percent, and the substances are very easy to be absorbed in human bodies.
When the water content of the Jinlong capsule is measured, the Jinlong capsule needs to be dissolved in an organic solvent to prepare a mixed solution, and then the water content of the mixed solution is measured by adopting a Karl Fischer reagent. Wherein, the water content of the organic solvent is extremely low, and the water content of the Jinlong capsule can be obtained by measuring the water content of the mixed solution. However, when the jinlong capsule is dissolved in the existing solvent for measuring the water content of the jinlong capsule, the accuracy of the measurement result of the water content is low.
Disclosure of Invention
The invention provides a solvent for determining water content of Jinlong capsules, a preparation method and an application method thereof, aiming at solving the problem that the accuracy of a determination result of the water content is lower when the Jinlong capsules are dissolved in the existing solvent for determining the water content of the Jinlong capsules.
The solvent for measuring the water content of the Jinlongjiao capsule, which is provided for realizing the aim of the invention, comprises absolute methanol and dimethyl sulfoxide;
the mass percentage of the anhydrous methanol is 50-80%;
the content of dimethyl sulfoxide is 20-50%.
In one embodiment, the anhydrous methanol is 70.58%; the dimethyl sulfoxide content was 29.42%.
In one embodiment, the anhydrous methanol is 78.26%; the content of dimethyl sulfoxide was 21.74%.
The preparation method of the organic solvent provided by any one of the above embodiments based on the same concept comprises the following steps:
placing 50-60ml of anhydrous methanol and 10-40ml of dimethyl sulfoxide into a preparation bottle;
the preparation bottle was sealed and inverted several times.
In one embodiment, the preparation bottle is a volumetric flask.
In one embodiment, the purity of the anhydrous methanol is chromatographically pure.
Based on the same concept, the method for measuring the water content of the Jinlong capsule by using the organic solvent provided by any one of the above embodiments comprises the following steps:
calibrating a titrant: injecting a proper amount of deionized water into a titration bottle of a Karl Fischer moisture tester, and titrating the deionized water by using a Karl Fischer reagent to test the titer of the Karl Fischer reagent;
measuring the water content of the Jinlong capsule: injecting a first preset amount of the organic solvent provided by any one of the above specific embodiments into a titration flask, adding a second preset amount of the Jinlong capsule into the titration flask to form a mixed solution in the titration flask, titrating the mixed solution in the titration flask by using a Karl Fischer reagent, wherein the volume of the consumed Karl Fischer reagent is V1。
In one embodiment, the method further comprises the following steps:
before the water content of the Jinlong capsule is measured, the water content of the organic solvent is measured:
injecting a first preset amount of organic solvent into a titration flask, titrating the organic solvent in the titration flask by using a Karl Fischer reagent, wherein the volume of the consumed Karl Fischer reagent is V2。
In one embodiment, the titration flask is rinsed several times prior to calibrating the titrant.
In one embodiment, the second predetermined amount is less than 7 g.
The invention has the beneficial effects that: the solvent for determining the water content of the Jinlong capsule is prepared by mixing 50-80% of absolute ethyl alcohol by mass percent and 20-50% of dimethyl sulfoxide by mass percent to serve as an organic solvent for dissolving the Jinlong capsule, and compared with the method of only using the absolute ethyl alcohol as the organic solvent, the solvent greatly improves the solubility of the Jinlong capsule in the organic solvent, so that the Jinlong capsule is dissolved in the organic solvent as much as possible, and the accuracy of the determination result of the water content of the Jinlong capsule is improved.
Detailed Description
The invention provides a solvent for determining water content of Jinlongjiao capsule, comprising absolute methanol and dimethyl sulfoxide; the mass percentage of the anhydrous methanol is 50-80%, and the mass percentage of the dimethyl sulfoxide is 20-50%.
In this example, the absolute ethanol is chromatographically pure and of high purity, so that the water content of the organic solvent formed by its mixing with dimethyl sulfoxide is very low. Therefore, the water content of the mixed liquid formed after the Jinlong capsule is dissolved in the organic solvent is the water content of the Jinlong capsule, the interference of the organic solvent on the water content measuring result of the Jinlong capsule is effectively reduced, and the accuracy of the water content measuring result of the Jinlong capsule is further improved. In addition, 50-60ml of absolute ethyl alcohol and 10-40ml of dimethyl sulfoxide are mixed to serve as an organic solvent for dissolving the Jinlong capsule, and compared with the method that only absolute ethyl alcohol is used as the organic solvent, the solubility of the Jinlong capsule in the organic solvent is greatly improved, so that the Jinlong capsule is dissolved in the organic solvent as much as possible, and the accuracy of the water content determination result of the Jinlong capsule is improved. It should be noted that, by analyzing the types and contents of the four raw materials (semi-finished product of jinlong capsule, gecko, bungarus parvus and agkistrodon) that make up the jinlong capsule, 42.47% of the semi-finished product of jinlong capsule can determine the types and contents of the components, 63.03% of the semi-finished product of jinlong-noded pit viper can determine the types and contents of the components, 51.22% of the semi-finished product of agkistrodon can determine the types and contents of the components, and 44.52% of the semi-finished product of agkistrodon can determine the types and contents of the components. The types and contents of the components contained in the raw materials are shown in the following table:
as can be seen from the above table, the free amino acids, proteins, free monosaccharides, and polysaccharides are the main components of the raw material of the jinlong capsule, and these components can be well dissolved in the organic solvent formed by mixing anhydrous ethanol and dimethyl sulfoxide.
In an embodiment of the present invention, when the absolute methanol is 51.92% and the dimethyl sulfoxide is 48.08% (i.e. the volume ratio of the absolute methanol to the dimethyl sulfoxide is 60 ml: 40ml), the jinlong capsule can be completely dissolved in the organic solvent, but the measured water content is higher and the deviation of the measurement result is larger. When the absolute methanol is 70.58% and the dimethyl sulfoxide is 21.74% (namely the volume ratio of the absolute methanol to the dimethyl sulfoxide is 50 ml: 15ml), the Jinlong capsule can be completely dissolved in the organic solvent, the deviation of the measurement result is small, the relative value is stable, but the measured water content is still high. When the absolute methanol is 78.26% and the dimethyl sulfoxide is 21.74% (namely the volume ratio of the absolute methanol to the dimethyl sulfoxide is 50 ml: 10ml), the Jinlong capsule can be completely dissolved in the organic solvent, the accuracy of the measured water content is high, and the stability of the measured result is high.
The invention also provides a preparation method of the organic solvent provided by any one of the above embodiments, which comprises the following steps:
first, 50 to 60ml of anhydrous methanol and 10 to 40ml of dimethyl sulfoxide are placed in a formulation bottle, and then, the formulation bottle is sealed and inverted several times, specifically, 3 to 5 times. Therefore, the anhydrous ethanol and the dimethyl sulfoxide are mixed more uniformly, and experimental errors caused by too high or too low local concentration are avoided. Wherein, the preparation bottle is a 1000ml volumetric flask. When the mass percent of the anhydrous methanol is 78.26 percent and the mass percent of the dimethyl sulfoxide is 21.74 percent, the preparation method comprises the following specific steps:
500ml of chromatographically pure absolute ethanol are measured accurately and placed in a 1000ml volumetric flask, and then 100ml of dimethyl sulfoxide is added to the volumetric flask. The flask was sealed and then inverted several times to thoroughly mix the absolute ethanol and dimethyl sulfoxide in the flask.
The invention also provides a method for measuring the water content of the Jinlong capsule by using the organic solvent, which comprises the following steps:
calibrating a titrant:
in this step, 10mg of deionized water was poured into a titration flask of a karl fischer moisture meter, and the deionized water was titrated with a karl fischer reagent to measure the titer T of the karl fischer reagent as 19.6767 mg/ml.
Measuring the water content of the Jinlong capsule:
in the step, a first preset amount of the organic solvent provided by any one of the embodiments is injected into the titration flask, a second preset amount of the Jinlong capsule is added into the titration flask, a mixed solution is formed in the titration flask, the mixed solution in the titration flask is titrated by using a Karl Fischer reagent, and the volume of the consumed Karl Fischer reagent is V1. The first predetermined amount is a liquid level of the organic solvent that is not above the electrode in the titration flask. The second predetermined amount, should be less than 7g to ensure accuracy of the assay. 7g of Jinlong capsule is added into a titration flask for three times to realize the purpose of carrying out three groups of experiments in parallel according to a formula alphaJinlong capsule=19.6767*V1*100%/mJinlong capsuleThe Karl Fischer water content titrator can automatically calculate alphaJinlong capsuleValue (water content of Jinlong capsule). The method is characterized in that anhydrous ethanol with the volume percentage of 60-85% and dimethyl sulfoxide with the volume percentage of 15-40% are mixed and then used as an organic solvent for dissolving the Jinlong capsule, and compared with the method only using the anhydrous ethanol as the organic solvent, the method greatly improves the solubility of the Jinlong capsule in the organic solvent, so that the Jinlong capsule is dissolved in the organic solvent as much as possible, and the accuracy of the water content determination result of the Jinlong capsule is improved. Further, the organic solvent is suitable for use in a Karl Fischer moisture meter.
In an embodiment of the present invention, the method further includes the following steps:
before the water content of the Jinlong capsule is measured, the water content of the organic solvent is measured:
in this step, a first predetermined amount of organic solvent is injected into the titration flask using a cardThe organic solvent in the titration flask is titrated by the Karl Fischer reagent, and the volume consumed by the Karl Fischer reagent is V2. According to the formula alphaOrganic solvent=19.6767*V2*100%/mOrganic solventThe Karl Fischer water content titrator can automatically calculate alphaOrganic solventValue (water content of organic solvent). Since dimethyl sulfoxide has a strong water-absorbing property, it has a certain water-absorbing property with an organic solvent composed of anhydrous methanol. The interference of the water content of the organic solvent on the water content determination result of the Jinlong capsule is eliminated by determining the water content of the organic solvent, and the formula alpha is usedActual Jinlong capsule=αJinlong capsule-αOrganic solventThe Karl Fischer water content titrator can automatically calculate alphaActual Jinlong capsuleThe value (the actual water content of the Jinlong capsule) further improves the accuracy of the determination result of the water content of the Jinlong capsule.
The water content of the Jinlong capsules is measured by using organic solvents containing dimethyl sulfoxide with different volume percentages, and the experimental results are shown in the following table:
as can be seen from the above data, when the volume ratio of the anhydrous methanol to the dimethyl sulfoxide is 60 ml: when the water content of the Jinlong capsule is measured at 40ml, the drift value is longer than 10mAV, data reading cannot be carried out, and the experimental efficiency is restricted. The Jinlong capsule can be completely dissolved in an organic solvent, but the measured water content is higher, and the deviation of the measured result is larger.
When the volume ratio of the anhydrous methanol to the dimethyl sulfoxide is 50 ml: when the volume is 15ml, the Jinlong capsule can be completely dissolved in the organic solvent, the deviation of the measurement result is small, the relative value is stable, but the measured water content is still high.
When the volume ratio of the anhydrous methanol to the dimethyl sulfoxide is 50 ml: when the volume is 10ml, the Jinlong capsule can be completely dissolved in the organic solvent, the measured water content is low, and the deviation of the measured result is small. Before the test, the organic solvent was placed in a solvent bottle of a karl fischer moisture meter, and the solvent bottle was rotated several times to remove air bubbles in the organic solvent.
In one embodiment of the invention, the titration flask is rinsed 3-5 times prior to calibrating the titrant. The interference of the residues in the titration flask to the measurement result is effectively reduced, so that the accuracy of the measurement result is further improved.
In the description herein, reference to the description of the terms "one embodiment," "some embodiments," "an example," "a specific example," "one specific embodiment," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, a schematic representation of the term does not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the scope of the present invention by equivalent replacement or change according to the technical solution and the inventive concept of the present invention within the scope of the present disclosure.
Claims (10)
1. The solvent for measuring the water content of the Jinlong capsules is characterized by comprising the following components:
anhydrous methanol and dimethyl sulfoxide;
the anhydrous methanol accounts for 50-80% by mass percent;
the content of dimethyl sulfoxide is 20-50%.
2. The solvent for determining the water content of the Jinlong capsule according to claim 1, wherein the absolute methanol is 70.58%; the dimethyl sulfoxide was 29.42%.
3. The solvent for determining the water content of the Jinlong capsule according to claim 1, wherein the absolute methanol is 78.26%; the dimethyl sulfoxide content was 21.74%.
4. A method for preparing the organic solvent according to any one of claims 1 to 3, comprising the steps of:
placing 50-60ml of anhydrous methanol and 10-40ml of dimethyl sulfoxide into a preparation bottle;
the dispensing vial is sealed and inverted several times.
5. The method of claim 4, wherein the dispensing bottle is a volumetric flask.
6. The formulation process of claim 4, wherein the absolute methanol is chromatographically pure.
7. A method for measuring the water content of Jinlong capsules by using the organic solvent according to any one of claims 1 to 3, which is characterized by comprising the following steps:
calibrating a titrant: injecting a proper amount of deionized water into a titration bottle of a Karl Fischer moisture tester, and titrating the deionized water by using a Karl Fischer reagent to test the titer of the Karl Fischer reagent;
measuring the water content of the Jinlong capsule: injecting a first predetermined amount of the organic solvent according to any one of claims 1 to 3 into the titration flask, adding a second predetermined amount of the Jinlong capsule into the titration flask to form a mixed solution in the titration flask, titrating the mixed solution in the titration flask with the Karl Fischer's reagent, wherein the volume of the consumed Karl Fischer's reagent is V1。
8. The method for measuring the water content of Jinlong capsules by using an organic solvent as claimed in claim 7, further comprising the steps of:
before the determination of the water content of the Jinlong capsule, determining the water content of the organic solvent:
injecting the first preset amount of the organic solvent into the titration flask, titrating the organic solvent in the titration flask by using the Karl Fischer reagent, wherein the volume of the consumed Karl Fischer reagent is V2。
9. The method for measuring the water content of Jinlong capsules using organic solvent as claimed in claim 7, wherein said titration flask is rinsed several times before said titrant is calibrated.
10. The method for measuring moisture content of Jinlong capsules according to claim 7, wherein said second predetermined amount is less than 7 g.
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Cited By (1)
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Application publication date: 20210629 |