CN110793926A - Method for measuring adsorption capacity of montmorillonite - Google Patents
Method for measuring adsorption capacity of montmorillonite Download PDFInfo
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- 238000001179 sorption measurement Methods 0.000 title claims abstract description 159
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 title claims abstract description 108
- 229910052901 montmorillonite Inorganic materials 0.000 title claims abstract description 107
- 238000000034 method Methods 0.000 title claims abstract description 75
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- GOOCRIHPADOQAS-ZNUXJMJHSA-N (4ar,5as,8ar,13as,15as,15br)-4a,5,5a,7,8,13a,15,15a,15b,16-decahydro-2h-4,6-methanoindolo[3,2,1-ij]oxepino[2,3,4-de]pyrrolo[2,3-h]quinoline-14-one;sulfuric acid Chemical compound OS(O)(=O)=O.O([C@H]1CC(N([C@H]2[C@H]1[C@H]1C3)C=4C5=CC=CC=4)=O)CC=C1CN1[C@@H]3[C@]25CC1.O([C@H]1CC(N([C@H]2[C@H]1[C@H]1C3)C=4C5=CC=CC=4)=O)CC=C1CN1[C@@H]3[C@]25CC1 GOOCRIHPADOQAS-ZNUXJMJHSA-N 0.000 description 4
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- AKYHKWQPZHDOBW-UHFFFAOYSA-N (5-ethenyl-1-azabicyclo[2.2.2]octan-7-yl)-(6-methoxyquinolin-4-yl)methanol Chemical compound OS(O)(=O)=O.C1C(C(C2)C=C)CCN2C1C(O)C1=CC=NC2=CC=C(OC)C=C21 AKYHKWQPZHDOBW-UHFFFAOYSA-N 0.000 description 1
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 1
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- 231100000699 Bacterial toxin Toxicity 0.000 description 1
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- 241000700605 Viruses Species 0.000 description 1
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- 235000019257 ammonium acetate Nutrition 0.000 description 1
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- ONCZQWJXONKSMM-UHFFFAOYSA-N dialuminum;disodium;oxygen(2-);silicon(4+);hydrate Chemical compound O.[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Na+].[Na+].[Al+3].[Al+3].[Si+4].[Si+4].[Si+4].[Si+4] ONCZQWJXONKSMM-UHFFFAOYSA-N 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
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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Abstract
The invention provides a method for measuring montmorillonite adsorption force by using berberine sulfate, which comprises the following steps: preparing a berberine sulfate standard solution, taking montmorillonite fine powder, quantitatively adding a phosphate buffer solution with the pH value of 6.8, quantitatively adding the berberine sulfate standard solution, controlling the ratio of the sampling amount of the montmorillonite to the adding amount of the berberine sulfate to be a certain proportion, fully adsorbing excessive berberine sulfate by the montmorillonite, measuring the residual berberine sulfate by using an ultraviolet-visible spectrophotometry, and calculating the adsorption capacity of the montmorillonite. The method for measuring the adsorption capacity specificity, linearity, accuracy, precision, durability and the like of the medicinal montmorillonite are good, and the method is safe, non-toxic, convenient to purchase and manage, low in price and low in cost.
Description
Technical Field
The invention relates to a method for measuring the adsorption capacity of medicinal montmorillonite, in particular to a method for measuring the adsorption capacity of the montmorillonite on berberine sulfate by using an ultraviolet-visible spectrophotometry, belonging to the technical field of medicines.
Background
The mineral name of bentonite is montmorillonite (see, Jujiaying, Strin eds., the development and application of bentonite in engineering, 1 st edition of month 07/2003, page 1). Montmorillonite powder is used as an anti-diarrhea drug in the medical field, and is marketed in more than 100 countries and regions around the world. The pharmacological basis of the medicinal montmorillonite is the function of adsorbing pathogenic bacteria, viruses and bacterial toxins, and the magnitude of the adsorption force is a key index of the montmorillonite with low curative effect. Accurate detection of the adsorption force of montmorillonite is a method for controlling the quality of products and ensuring the curative effect.
The method for detecting the montmorillonite adsorption force in the existing national drug standard is to measure the amount of adsorbed strychnine sulfate. The method has the advantages that the adsorption force is measured accurately, but the strychnine sulfate belongs to A-grade organic highly toxic substances, the environment can be polluted when the strychnine sulfate is used, the experimenter can be injured by careless operation in the using process, and great potential safety hazards exist. Moreover, no enterprise produces strychnine sulfate which can meet the experimental requirements in China, and needs to purchase imported reagents, so that the purchase is difficult and the price is high, and the enterprise cost is increased virtually.
In other fields, the content of montmorillonite in the mineral is determined by detecting the methylene blue adsorption capacity of the montmorillonite, which is called blue adsorption amount for short, and the method is widely applied. The method for measuring the blue absorption amount is mainly a halo method in the reported article. The halo method is convenient to operate, simple in instrument and most commonly applied. However, because the liquid drops are taken out from the test paper for multiple times, and the eye is used for observing the green ring to determine the end point, the size of the green ring is greatly different due to human judgment, and the end point judgment is liquid taking observation, the result error is large, and the accuracy and precision of the method are limited.
Zhengxihua notes (see, Zhengxihua main edition, applied technology of bentonite, 1 st edition at 09 month 2001, pages 10 to 11): the adsorption force of bentonite can be divided into three types, namely physical adsorption, chemical adsorption and ion exchange adsorption.
(1) And (4) carrying out physical adsorption. Physical adsorption is produced by intermolecular attraction between the adsorbent and the adsorbate. Physical adsorption is a reversible adsorption process, and the adsorption speed and the desorption speed are in dynamic balance under certain conditions. The main reason for the physical adsorption is that the surface molecules of bentonite have surface energy. The bentonite is highly dispersed in water, so that the physical adsorption phenomenon is very obvious.
(2) And (4) carrying out chemical adsorption. Chemisorption is generated by the chemical bonding forces between the adsorbent and the adsorbate, and chemisorption is generally irreversible.
(3) And (4) ion exchange adsorption. Bentonite mineral crystals are generally negatively charged and adsorb an equivalent amount of oppositely charged cations, which can exchange with cations in solution, a process known as ion exchange adsorption. The ion exchange adsorption is characterized in that: the same numbers are separated from each other, and the isoelectric values are exchanged. The reaction of ion exchange adsorption is reversible, and the rates of adsorption and desorption are influenced by the ion concentration, which follows the law of mass action.
The factors influencing the bentonite mineral adsorption are:
(1) the effect of the bentonite type. The adsorption capacity of the sodium bentonite is obviously stronger than that of other types of bentonite such as calcium bentonite.
(2) The influence of the size of the crushed particle size of the bentonite particles. According to the theory of solid adsorption, the bentonite mineral adsorption capacity after being crushed is obviously improved, and the finer the crushing is, the stronger the adsorption effect is.
(3) Influence of the solution medium. According to the theory of electric double layer, the mineral crystals of bentonite are negatively charged, ion exchange is carried out when the electric double layer is formed, and if the ion concentration in the solution is too high, the electric double layer of bentonite particles is compressed, dispersion and diffusion of bentonite are inhibited, and even the bentonite is coagulated and agglomerated.
In summary, the adsorption force of the montmorillonite comprises three types of physical adsorption, chemical adsorption and ion exchange adsorption, wherein the ion exchange adsorption capacity is not influenced by a set condition and is constant, and the montmorillonite belongs to isoelectric adsorption or stoichiometric reaction; the physical adsorption and chemical adsorption capacity can be determined by measuring the concentration of montmorillonite in the liquid, the dispersion degree of montmorillonite in the liquid, the granularity, the concentration of adsorbed ions, the pH value of the liquid, the temperature of the liquid, the chemical bond force between montmorillonite and adsorbed ions and other factors, and the physical adsorption and chemical adsorption capacity can be changed. An agent is selected to measure the adsorption force of the montmorillonite, and a series of scientific experiments are carried out to determine proper measuring conditions and methods.
The invention patent (CN 102406657 a) discloses (see paragraph 0039 of the specification) that the adsorption force of montmorillonite is derived from its internal charge imbalance. … …, the excess negative charge is compensated by cations adsorbed on the surface of the crystal layer, which are easily exchanged by other cations in the presence of water, known as exchange adsorption. The exchange adsorption has the following characteristics: (1) the same number of ions are exchanged, … … is a stoichiometric reaction, and the mass action law is met; (2) equal electrical quantities (or equal equivalents) are exchanged with each other, … …; (3) the exchange and adsorption of cations is reversible. According to the ion exchange adsorption characteristics of montmorillonite, the adsorbed agent can be a compound capable of dissociating positive ions in water or ethanol solution. These compounds include ammonium acetate, ammonium chloride, methylene blue, quinine sulfate, berberine, betaine, barium chloride, etc., which can dissociate positive ions in water or ethanol solution.
Orefin, norm H, indicates (orefin, usa, lead theory of clay colloid chemistry, 12 months, 1 st edition, 1982, page 169): the adsorption of organic cations is generally not limited by the cation exchange capacity equivalent of the clay. For example, it has been observed that the adsorption of montmorillonite clay to quaternary amine compounds having long chains and three methyl groups is approximately twice and half the cation exchange capacity of the clay.
The invention patent (CN 102406657A) only considers the ion exchange adsorption of montmorillonite, neglects the physical adsorption, the chemical adsorption and other factors influencing the adsorption, and has no general guiding significance. The specification also discloses (see paragraphs 0066 and 0067): experiment seven uses berberine to determine the adsorption force of montmorillonite used in the invention, uses high performance liquid chromatography to determine the adsorption force of montmorillonite to berberine sulfate, calculates the cation exchange capacity of montmorillonite to be 135mmol/100g, namely the adsorption force of montmorillonite used is 135mmol/100 g. The adsorption force of the montmorillonite comprises physical adsorption, chemical adsorption and ion exchange adsorption, and the physical adsorption and the chemical adsorption are influenced by various factors such as the concentration of the montmorillonite in the liquid, the dispersion degree granularity of the montmorillonite in the liquid, the concentration of adsorbed ions, the pH value of the liquid, the temperature of the liquid, the chemical bond force between the montmorillonite and the adsorbed ions and the like when the physical adsorption and the chemical adsorption are measured. The patent only discloses that the adsorption force of montmorillonite can be measured by berberine, and no specific measurement method is disclosed.
Disclosure of Invention
The invention aims to overcome the defects of the existing method for measuring the adsorption capacity of the medicinal montmorillonite and provide a novel method for measuring the adsorption capacity of the medicinal montmorillonite. The method for measuring the adsorption capacity of the medicinal montmorillonite is good in specificity, linearity, accuracy, precision, reproducibility, durability and the like, safe, nontoxic, convenient to purchase and manage, low in price and low in cost.
The purpose of the invention is realized by the following technical scheme.
A method for measuring the adsorption capacity of montmorillonite is characterized by comprising the following steps: the method for measuring the berberine sulfate adsorption amount of montmorillonite by using an ultraviolet-visible spectrophotometry comprises the following steps: preparing a berberine sulfate standard solution with the concentration of 1.5% -2.5%, taking 0.15-0.25 g of montmorillonite fine powder with the granularity of less than 45 mu m, quantitatively adding a phosphate buffer solution with the pH value of 6.8, quantitatively adding the berberine sulfate standard solution, controlling the ratio of the sampling amount of montmorillonite to the adding amount of berberine sulfate to be 0.8-1.2, fully adsorbing excessive berberine sulfate by the montmorillonite, measuring the residual berberine sulfate by using an ultraviolet-visible spectrophotometry, and then calculating the adsorption capacity of the montmorillonite;
the particle size and the measuring method of the montmorillonite fine powder are as follows: taking 10g of montmorillonite, adding 500ml of water, stirring for 15 minutes at 5000 r/min, wetting a 45-micron pore size drug sieve which is dried to constant weight at 105 ℃ with water, pouring the stirred content into the drug sieve, washing the drug sieve with water until no suspension spots exist, drying the drug sieve for 3 hours at 105 ℃, and weighing. The weight of the unscreened granules should not exceed 1%.
The invention relates to a method for measuring the adsorption capacity of montmorillonite, which is characterized by comprising the following steps: the adsorption capacity of montmorillonite was determined using berberine sulphate.
The invention relates to a method for measuring the adsorption capacity of montmorillonite, which is characterized by comprising the following steps: the ratio of montmorillonite sampling amount to berberine sulfate addition amount is 1.
The invention relates to a method for measuring the adsorption capacity of montmorillonite, which is characterized by comprising the following steps: and (3) measuring the residual berberine sulfate by using an ultraviolet-visible spectrophotometry, wherein the wavelength is 200-800 nm.
The invention relates to a method for measuring the adsorption capacity of montmorillonite, which is characterized by comprising the following steps:
1) preparing a standard berberine sulfate solution with the concentration of 2.0 percent:
precisely weighing about 2.0g of berberine sulfate, placing into a 100ml measuring flask, adding appropriate amount of water, heating in water bath to dissolve, cooling, diluting with water to scale, and shaking to obtain standard berberine sulfate solution with concentration of 2.0%;
2) and (3) measuring the adsorption force:
taking 0.2g of montmorillonite fine powder with the granularity of less than 45 mu m, precisely weighing, placing in a conical flask with a plug, precisely adding 10ml of phosphate buffer solution with the pH of 6.8, shaking up, precisely adding 10ml of berberine sulfate standard solution with the concentration of 2.0%, placing in a water bath at 37 ℃, shaking up for 1 hour, filtering, precisely measuring 10ml of subsequent filtrate, placing in a 250ml measuring flask, diluting to scale with phosphate buffer solution with the pH of 6.8, shaking up, precisely measuring 5ml, placing in a 25ml measuring flask, diluting to scale with phosphate buffer solution with the pH of 6.8, shaking up, and measuring absorbance at the wavelength of 420nm according to an ultraviolet-visible spectrophotometry, the general rule 0401 of the national pharmacopoeia 2015 edition, with the pH of 6.8 as a blank; diluting the above 2.0% berberine sulfate standard solution with phosphate buffer solution with pH of 6.8 to obtain solution containing 40 μ g per 1ml, measuring absorbance by the same method, and calculating adsorption force according to the following formula;
adsorption capacity (g/g) = (2A)1-A2）×M1×D2/M2/A1/D1
A1: absorbance of berberine sulfate control solution
A2: absorbance of test solution
M1: weight of berberine sulfate
M2: weight of test article
D1: dilution multiple of berberine sulfate reference solution
D2: dilution factor of test solution
The invention relates to a method for measuring the adsorption capacity of montmorillonite, which is characterized by comprising the following steps: preferably, the measurement wavelength is 420nm, and the absorption peaks of berberine sulfate further include 228nm, 264nm and 345 nm.
The advantageous effects of the present invention are further illustrated by the following experimental examples and methodological studies. Experimental examples and methodological studies are intended to further illustrate the beneficial effects of the present invention and are not intended to limit the invention.
Test example: the determination methodology of the adsorption force of the medicinal montmorillonite is verified
1. Test article and reagent
And (3) testing the sample: montmorillonite (batch number: 1607008, Shandong HongJitang pharmaceutical group GmbH)
Berberine sulfate: (batch No. 36XZM, Taixi Ai-Shanghai Kangcheng Industrial development Co., Ltd.)
2. Test methods and methodological validation
Referring to the downward adsorption force of montmorillonite in the second part of the year 2015 of Chinese pharmacopoeia, the method is tentatively determined as follows:
1) preparing a standard berberine sulfate solution with the concentration of 2.0 percent:
precisely weighing about 2.0g of berberine sulfate, placing into a 100ml measuring flask, adding appropriate amount of water, heating in water bath to dissolve, cooling, diluting with water to scale, and shaking to obtain standard berberine sulfate solution with concentration of 2.0%;
2) and (3) measuring the adsorption force:
taking 0.2g of montmorillonite, precisely weighing, placing in a conical flask with a stopper, precisely adding 10ml of phosphate buffer solution (pH6.8), shaking up, precisely adding 10ml of berberine sulfate standard solution with the concentration of 2.0%, placing in a water bath at 37 ℃, shaking up for 1 hour, filtering, precisely measuring 10ml of subsequent filtrate, placing in a 250ml measuring flask, diluting to scale with phosphate buffer solution (pH6.8), shaking up, precisely measuring 5ml, placing in a 25ml measuring flask, diluting to scale with phosphate buffer solution (pH6.8), shaking up, and measuring absorbance at a wavelength of 420nm by an ultraviolet-visible spectrophotometry (0401 in the book of Chinese pharmacopoeia 2015 edition) with phosphate buffer solution (pH6.8) as a blank; diluting the above 2.0% berberine sulfate standard solution with phosphate buffer solution (pH 6.8) to obtain solution containing 40 μ g per 1ml, measuring absorbance by the same method, and calculating adsorption force according to the following formula;
adsorption capacity (g/g) = (2A)1-A2）×M1×D2/M2/A1/D1
A1: absorbance of berberine sulfate control solution
A2: absorbance of test solution
M1: weight of berberine sulfate
M2: weight of test article
D1: dilution multiple of berberine sulfate reference solution
D2: dilution factor of test solution
2.1 optimization of parameters in the preparation of test articles
2.1.1 adsorption reaction time Curve
Taking 7 parts of sample, testing according to the above method, setting reaction time at 1min, 5min, 10min, 30min, 60min, 90min and 120min, and measuring adsorption time curve, wherein the results are as follows (the adsorption force curve of different reaction times is shown in figure 1):
TABLE 1 results of adsorption force at different reaction times
| Reaction time (min) | 0 | 1 | 5 | 10 | 30 | 60 | 90 | 120 |
| Adsorption capacity (g/g) | 0 | 0.36 | 0.414 | 0.418 | 0.427 | 0.435 | 0.437 | 0.436 |
The results showed that the montmorillonite rapidly adsorbed berberine sulfate to about 95% of the total adsorption within 5min, after which the adsorption rate slowed, slowly increased and finally reached equilibrium, so the tentative reaction time was 60 minutes.
2.1.2 relationship between berberine sulfate concentration and adsorption force
Taking 7 parts of sample, precisely adding 19ml, 18ml, 16ml, 12ml, 10ml, 8ml and 5ml of phosphate buffer solution (pH6.8) and 1ml, 2ml, 4ml, 8ml, 10ml, 12ml and 15ml of berberine sulfate solution (20 mg/ml) according to the test of the measuring method of the adsorption force, and measuring the relation between the adsorption force and the reaction concentration, wherein the results are as follows (the relation curve between the concentration of the berberine sulfate solution and the adsorption force is shown in figure 2):
TABLE 2 relationship between initial reaction concentration and adsorption force
| Initial concentration (mg/ml) | 1 | 2 | 4 | 8 | 10 | 12 | 15 |
| Adsorption force g/g | 0.406 | 0.409 | 0.412 | 0.434 | 0.437 | 0.439 | 0.440 |
The test result shows that the adsorption force result is increased along with the increase of the added amount of the berberine sulfate, and the adsorption force result is balanced when the added amount is 10ml, so the added amount of the tentative berberine sulfate standard solution is 10 ml.
2.1.3 method for measuring adsorption force
From the above examination, the provisional adsorption force measurement method is as follows:
1) preparing a standard berberine sulfate solution with the concentration of 2.0 percent:
precisely weighing about 2.0g of berberine sulfate, placing into a 100ml measuring flask, adding appropriate amount of water, heating in water bath to dissolve, cooling, diluting with water to scale, and shaking to obtain standard berberine sulfate solution with concentration of 2.0%;
2) and (3) measuring the adsorption force:
taking 0.2g of montmorillonite, precisely weighing, placing in a conical flask with a stopper, precisely adding 10ml of phosphate buffer solution (pH6.8), shaking up, precisely adding 10ml of berberine sulfate standard solution with the concentration of 2.0%, placing in a water bath at 37 ℃, shaking up for 1 hour, filtering, precisely measuring 10ml of subsequent filtrate, placing in a 250ml measuring flask, diluting to scale with phosphate buffer solution (pH6.8), shaking up, precisely measuring 5ml, placing in a 25ml measuring flask, diluting to scale with phosphate buffer solution (pH6.8), shaking up, and measuring absorbance at a wavelength of 420nm by an ultraviolet-visible spectrophotometry (0401 in the book of Chinese pharmacopoeia 2015 edition) with phosphate buffer solution (pH6.8) as a blank; diluting the above 2.0% berberine sulfate standard solution with phosphate buffer solution (pH 6.8) to obtain solution containing 40 μ g per 1ml, measuring absorbance by the same method, and calculating adsorption force according to the following formula;
adsorption capacity (g/g) = (2A)1-A2）×M1×D2/M2/A1/D1
A1: absorbance of berberine sulfate control solution
A2: absorbance of test solution
M1: weight of berberine sulfate
M2: weight of test article
D1: dilution multiple of berberine sulfate reference solution
D2: dilution factor of test solution
2.2 methodological validation
The method is verified by referring to appendix 9101 of the four parts of the year 2015 of Chinese pharmacopoeia.
2.2.1 measurement of wavelength and specificity
Preparing a test solution: taking 0.20g of montmorillonite, precisely weighing, and preparing a test solution according to the adsorption force measuring method;
preparation of negative solution: taking 0.20g of montmorillonite, precisely weighing, placing in a conical flask with a stopper, precisely adding 10ml of phosphate buffer solution (pH 6.8), precisely adding 10ml of water, and preparing a negative solution by the same method from 'placing in a water bath at 37 ℃ and shaking for 1 hour' according to the preparation method of the test solution.
The determination method comprises the following steps: scanning in a wavelength range of 200-600 nm by using an ultraviolet-visible spectrophotometry (China pharmacopoeia 2015 edition general rules 0401) and taking a phosphate buffer solution (pH6.8) as a blank; taking appropriate amount of the above 20mg/ml berberine sulfate solution, diluting with phosphate buffer solution (pH 6.8) to obtain solution containing 40 μ g per 1ml, and determining by the same method.
As a result: the absorption spectrum curves of the test solution and the reference solution are consistent, the maximum absorption exists at the wavelengths of 228nm, 264nm, 345nm and 420nm, and the absorption peak does not exist at the wavelength of 200-600 nm in the negative solution, which indicates that the specificity of the method is good.
As can be seen from the scanned graph, the absorption peaks at 228nm, 264nm and 345nm are sharp, the interference factors in the ultraviolet region are more, and the absorption peak at the wavelength of 420nm is relatively flat, so the wavelength measured by the method is tentatively 420 nm.
2.2.2 Linear relationship investigation test
Taking a proper amount of berberine sulfate solution, preparing linear solutions containing 10, 20, 40, 60 and 80 μ g of phosphate buffer solution (pH = 6.8) per 1ml respectively, and measuring absorbance at a wavelength of 420nm by using the phosphate buffer solution (pH 6.8) as a blank, wherein the results are shown in the following table:
TABLE 3 results of the Linear relationship test
| Concentration (μ g/ml) | 80.136 | 64.1088 | 40.068 | 20.034 | 10.017 |
| Absorbance (Abs) | 1.0113 | 0.825 | 0.5222 | 0.2659 | 0.1364 |
Taking the concentration as an abscissa and the absorbance as an ordinate, a linear regression equation y = 0.0125x + 0.0153 and a correlation coefficient r =0.9999 are obtained (the linear relationship is shown in fig. 3).
The result shows that the berberine sulfate concentration is in a good linear relation with the absorbance within the range of 10-80 mug/ml.
2.2.3 precision
2.2.3.1 repeatability
6 parts of test sample are taken, and a repeatability test is carried out according to an adsorption force measuring method, and the result is shown in a table.
TABLE 4 results of the repeatability tests
| | 1 | 2 | 3 | 4 | 5 | 6 | Average | RSD% |
| Adsorption capacity (g/g) | 0.434 | 0.439 | 0.442 | 0.442 | 0.435 | 0.432 | 0.437 | 0.91% |
The result RSD% is less than 2.0%, which shows that the method has good repeatability.
2.2.3.2 different analysts
The test article is taken and tested by different testers, and the results are shown in the table.
TABLE 5 precision of different experimenters
The result RSD% is less than 2.0%, which shows that the precision of different testers is good.
2.2.3.3 different analytical instruments
The test sample is taken and measured by different instruments, and the results are shown in the table.
TABLE 6 precision of different analytical instruments
The result RSD% is less than 2.0%, which shows that the precision of different analytical instruments is good.
2.2.3.4 different dates of analysis
The test article is taken and tested on different dates, and the results are shown in the table.
TABLE 7 results of different dates of analysis
| Date | Date |
| 1 | | Date 3 | Average | RSD% | |
| Adsorption capacity (g/g) | 0.432 | 0.437 | 0.445 | 0.438 | 1.23% |
The result RSD% is less than 2.0%, indicating that the precision is good at different analysis dates.
2.2.4 accuracy
Preparation of 1% berberine sulfate solution: taking 1.0g of berberine sulfate, precisely weighing, and dissolving with water to 100ml to obtain 1% berberine sulfate solution.
Taking 6 parts of conical flask with plug, respectively adding 10ml of phosphate buffer solution (pH6.8) precisely, then adding 10ml of 1% berberine sulfate solution precisely, adding 0.1g of berberine sulfate reference substance precisely, shaking uniformly to dissolve, taking 0.20g of montmorillonite with known adsorption capacity of 0.437g/g, precisely weighing 6 parts, placing in the conical flask, and measuring by the same method according to adsorption capacity measurement method from 'placing in water bath at 37 ℃ and shaking for 1 hour', wherein the results are as follows:
TABLE 8 recovery results
The result shows that the method has good accuracy.
2.2.5 durability
2.2.5.1 solution stability
The test solution was allowed to stand at room temperature for 8 hours, samples were taken every 2 hours, and the absorbance was measured at a wavelength of 420nm, and the test results are shown in the table:
TABLE 9 stability test results of solutions
| Time of | 0 | 2 | 4 | 6 | 8 hours | Average | RSD% |
| Degree of absorption | 0.559 | 0.558 | 0.560 | 0.558 | 0.555 | 0.558 | 0.28 |
The results show that the solution is stable within 8 hours
2.2.5.2 different analysis wavelengths
Taking a test sample, measuring the adsorption force at different wavelengths, and inspecting the wavelength durability of the test sample, wherein the results are as follows:
TABLE 10 wavelength durability results
| Wavelength of light | 415nm | 418nm | 420nm | 422nm | 425nm | Average | RSD% |
| Adsorption capacity (g/g) | 0.452 | 0.452 | 0.449 | 0.448 | 0.450 | 0.450 | 0.35 |
The result shows that the method has accurate and reliable result when measuring within the wavelength of 420 +/-5 nm.
2.2.6 range
The amount of the test sample in the range of 80-120% of the test amount of the product is taken, and the test is carried out according to the method for measuring the adsorption force, and the result is shown in the table:
TABLE 11 Range of test results
The result shows that the sampling is carried out within the range of +/-20% of the testing amount, and the determination result is reliable.
The result of the above methodology verification shows that the method for determining the adsorption capacity of the medicinal montmorillonite is good in specificity, linearity, accuracy, precision, durability and the like, safe, nontoxic, convenient to purchase and manage, low in price and low in cost.
The method for measuring the adsorption capacity of the medicinal montmorillonite can be used for montmorillonite raw materials and montmorillonite preparations. The montmorillonite preparation comprises clinically acceptable dosage forms such as powder, tablets, capsules, granules, suspension, gels, dispersible tablets and the like.
Drawings
Figure 1, adsorption force versus time curve. It is shown that the montmorillonite rapidly adsorbed berberine sulfate to about 95% of the total adsorption within 5min, after which the adsorption rate slowed, slowly increased and finally reached equilibrium, so the tentative reaction time was 60 min.
FIG. 2 is a graph showing the relationship between the concentration of berberine sulfate solution and the adsorption force. As shown in the figure, the adsorption force results become larger with the increase of the added amount of berberine sulfate, and the adsorption force results tend to be balanced with the added amount of 10ml, so that the added amount of the tentative berberine sulfate standard solution is 10 ml.
Fig. 3, a linear range inspection diagram. The figure shows that the berberine sulfate concentration is in a good linear relation with the absorbance within the range of 10-80 mu g/ml
The invention is further illustrated by the following specific examples.
Detailed Description
Example 1: determination of adsorption force of medicinal montmorillonite
And (3) testing the sample: montmorillonite (batch number: 1611015, Shandong HongJitang pharmaceutical group GmbH)
Berberine sulfate: (batch No. 36XZM, Taixi Ai-Shanghai Kangcheng Industrial development Co., Ltd.)
Measurement method and results:
1) and (3) calibrating berberine sulfate content:
taking 20mg of berberine sulfate, precisely weighing, dissolving with phosphate buffer solution (pH6.8), diluting to 100ml, precisely weighing 10ml from the medium, adding phosphate buffer solution (pH6.8), diluting to 50ml, performing ultraviolet-visible spectrophotometry (0401 in 2015 pharmacopoeia of China), taking phosphate buffer solution (pH6.8) as blank, and measuring absorbance at 420nm wavelength; taking berberine sulfate standard, dissolving with phosphate buffer solution (pH 6.8), quantitatively diluting to obtain solution containing 40 μ g of berberine sulfate per 1ml, and measuring by the same method to calculate berberine sulfate content.
2) Preparing a standard berberine sulfate solution with the concentration of 1.5 percent:
precisely weighing about 1.5g of berberine sulfate, placing into a 100ml measuring flask, adding appropriate amount of water, heating in water bath to dissolve, cooling, diluting with water to scale, and shaking to obtain standard berberine sulfate solution with concentration of 1.5%;
3) and (3) measuring the adsorption force:
taking 0.15g of montmorillonite, precisely weighing, placing in a conical flask with a stopper, precisely adding 10ml of phosphate buffer solution (pH6.8), shaking up, precisely adding 10ml of berberine sulfate standard solution with the concentration of 1.5%, placing in a water bath at 37 ℃, shaking up for 1 hour, filtering, precisely measuring 10ml of subsequent filtrate, placing in a 250ml measuring flask, diluting to scale with phosphate buffer solution (pH6.8), shaking up, precisely measuring 5ml, placing in a 25ml measuring flask, diluting to scale with phosphate buffer solution (pH6.8), shaking up, and measuring absorbance at a wavelength of 420nm by an ultraviolet-visible spectrophotometry (0401 in the book of Chinese pharmacopoeia 2015 edition) with phosphate buffer solution (pH6.8) as a blank; diluting the above 1.5% berberine sulfate standard solution with phosphate buffer solution (pH 6.8) to obtain solution containing 30 μ g per 1ml, measuring absorbance by the same method, and calculating adsorption force according to the following formula;
adsorption capacity (g/g) = (2A)1-A2）×M1×D2/M2/A1/D1
A1: absorbance of berberine sulfate control solution
A2: absorbance of test solution
M1: weight of berberine sulfate
M2: weight of test article
D1: dilution multiple of berberine sulfate reference solution
D2: dilution factor of test solution
As a result: the montmorillonite of the batch adsorbs berberine sulfate 0.425 g/g.
Example 2 method for measuring adsorption force of montmorillonite
Prescription: each bag contains 3g of montmorillonite, 0.749g of glucose, 0.007g of saccharin sodium and 0.004g of vanillin.
Montmorillonite powder: (batch number: 1608004)
Negative preparation: according to the proportion of the prescription, taking 7.49 g of glucose, 0.07 g of saccharin sodium and 0.04g of vanillin as auxiliary materials, and uniformly mixing to obtain the negative preparation.
Method for measuring adsorption force and results:
taking 0.35g of montmorillonite powder (equivalent to 0.25g of montmorillonite), precisely weighing, placing in a conical flask with a plug, precisely adding 10ml of phosphate buffer solution (pH 6.8), shaking up, precisely adding 10ml of berberine sulfate standard solution with the concentration of 2.5%, placing in a water bath at 37 ℃, shaking for 1 hour, filtering, precisely measuring 10ml of subsequent filtrate, placing in a 250ml measuring flask, diluting to scale with phosphate buffer solution (pH 6.8), shaking up, precisely measuring 5ml, placing in a 25ml measuring flask, diluting to scale with phosphate buffer solution (pH 6.8), shaking up, and measuring absorbance at a wavelength of 420nm by ultraviolet-visible spectrophotometry (according to 0401 in 2015 year edition) with phosphate buffer solution (pH 6.8) as blank; diluting the above 2.5% berberine sulfate standard solution with phosphate buffer solution (pH 6.8) to obtain 50 μ g solution per 1ml, measuring absorbance by the same method, and calculating adsorption force according to the following formula;
adsorption capacity (g/g) = (2A)1-A2）×M1×D2×M3/M2/A1/D1/G
A1: absorbance of berberine sulfate control solution
A2: absorbance of test solution
M1: weight of berberine sulfate
M2: weight of test article
M3: average loading
D1: dilution multiple of berberine sulfate reference solution
D2: dilution factor of test solution
G: montmorillonite marker (3 g)
Test of influence of auxiliary materials on adsorption force measurement: 0.05g of negative preparation mixed with auxiliary materials according to the proportion of the prescription is taken and tested according to the method.
As a result: the montmorillonite powder has berberine sulfate adsorption rate of 0.413g/g, and adjuvants do not adsorb berberine sulfate, and has no influence on measurement.
Example 3 method for measuring adsorption force of montmorillonite dispersible tablet
Prescription: each 1000 tablets contains 1000g of montmorillonite, 7g of glucose, 3g of saccharin sodium, 4g of vanillin, 100g of microcrystalline cellulose and 30g of sodium carboxymethyl starch.
Montmorillonite dispersible tablets: (batch number: 1611001)
Negative preparation: according to the proportion of the prescription, taking 7g of glucose, 3g of saccharin sodium, 4g of vanillin, 100g of micro-fine cellulose and 30g of sodium carboxymethyl starch as auxiliary materials, and uniformly mixing to obtain the negative preparation.
Method for measuring adsorption force and results:
grinding montmorillonite dispersible tablet, weighing 0.23g of fine powder (equivalent to 0.20g of montmorillonite), precisely weighing, placing in a conical flask with a plug, precisely adding 10ml of phosphate buffer solution (pH6.8), shaking up, precisely adding 10ml of berberine sulfate standard solution with concentration of 2.0%, placing in a water bath at 37 ℃, shaking up for 1 hour, filtering, precisely measuring to obtain 10ml of subsequent filtrate, placing in a 250ml measuring flask, diluting to scale with phosphate buffer solution (pH6.8), shaking up, precisely measuring 5ml, placing in a 25ml measuring flask, diluting to scale with phosphate buffer solution (pH6.8), shaking up, measuring absorbance at 420nm wavelength according to ultraviolet-visible spectrophotometry (0401 in the 2015 version of Chinese pharmacopoeia), using phosphate buffer solution (pH6.8) as blank; diluting the above 2.0% berberine sulfate standard solution with phosphate buffer solution (pH 6.8) to obtain solution containing 40 μ g per 1ml, measuring absorbance by the same method, and calculating adsorption force according to the following formula;
adsorption capacity (g/g) = (2A)1-A2）×M1×D2×M3/M2/A1/D1/G
A1: absorbance of berberine sulfate control solution
A2: absorbance of test solution
M1: weight of berberine sulfate
M2: weight of test article
M3: average loading
D1: dilution multiple of berberine sulfate reference solution
D2: dilution of test solutionMultiple of
G: montmorillonite marker (3 g)
Test of influence of auxiliary materials on adsorption force measurement: 0.03g of negative preparation mixed with auxiliary materials according to the proportion of the prescription is taken and tested according to the method.
As a result: the montmorillonite dispersible tablets have berberine sulfate adsorption of 0.417g/g, and adjuvants do not adsorb berberine sulfate, and have no influence on measurement.
Example 4 method for measuring adsorption force of montmorillonite suspension
Prescription: each 1000ml of the product contains 150g of montmorillonite and 1g of ethylparaben.
Montmorillonite suspension: (batch number: 1702004)
Negative preparation: according to the proportion of the prescription, 1g of ethylparaben is taken, 1000ml of water is added, and the negative preparation is obtained after uniform mixing.
Method for measuring adsorption force and results:
taking 10ml of montmorillonite suspension, evaporating to dryness in a water bath, grinding, weighing 0.20g of fine powder, precisely weighing, placing in a conical flask with a stopper, precisely adding 10ml of phosphate buffer solution (pH6.8), shaking up, precisely adding 10ml of berberine sulfate standard solution with the concentration of 2.0%, placing in a water bath at 37 ℃, shaking for 1 hour, filtering, precisely taking 10ml of subsequent filtrate, placing in a 250ml measuring flask, diluting to scale with phosphate buffer solution (pH6.8), shaking up, precisely taking 5ml, placing in a 25ml measuring flask, diluting to scale with phosphate buffer solution (pH6.8), shaking up, measuring absorbance at a wavelength of 420nm by an ultraviolet-visible spectrophotometry (0401 in accordance with the general rules of Chinese pharmacopoeia 2015), using phosphate buffer solution (pH6.8) as blank; diluting the above 2.0% berberine sulfate standard solution with phosphate buffer solution (pH 6.8) to obtain solution containing 40 μ g per 1ml, measuring absorbance by the same method, and calculating adsorption force according to the following formula;
adsorption capacity (g/g) = (2A)1-A2）×M1×D2/M2/A1/D1
A1: absorbance of berberine sulfate control solution
A2: absorbance of test solution
M1: weight of berberine sulfate
M2: weight of test article
D1: dilution multiple of berberine sulfate reference solution
D2: dilution factor of test solution
As a result: the adsorption capacity of the montmorillonite suspension in the batch is 0.408 g/g.
Claims (6)
1. A method for measuring the adsorption capacity of montmorillonite is characterized by comprising the following steps: the method for measuring the berberine sulfate adsorption amount of montmorillonite by using an ultraviolet-visible spectrophotometry comprises the following steps: preparing a berberine sulfate standard solution with the concentration of 1.5% -2.5%, taking 0.15-0.25 g of montmorillonite fine powder with the granularity of less than 45 mu m, quantitatively adding a phosphate buffer solution with the pH value of 6.8, quantitatively adding the berberine sulfate standard solution, controlling the ratio of the sampling amount of montmorillonite to the adding amount of berberine sulfate to be 0.8-1.2, fully adsorbing excessive berberine sulfate by the montmorillonite, measuring the residual berberine sulfate by using an ultraviolet-visible spectrophotometry, and then calculating the adsorption capacity of the montmorillonite.
2. The method for measuring the adsorption ability of montmorillonite according to claim 1, characterized in that: the adsorption capacity of montmorillonite was determined using berberine sulphate.
3. The method for measuring the adsorption ability of montmorillonite according to claim 1, characterized in that: the ratio of montmorillonite sampling amount to berberine sulfate addition amount is 1.
4. The method for measuring the adsorption ability of montmorillonite according to claim 1, characterized in that: and (3) measuring the residual berberine sulfate by using an ultraviolet-visible spectrophotometry, wherein the wavelength is 200-800 nm.
5. The method for measuring the adsorption ability of montmorillonite according to claim 1, characterized in that:
1) preparing a standard berberine sulfate solution with the concentration of 2.0 percent:
precisely weighing about 2.0g of berberine sulfate, placing into a 100ml measuring flask, adding appropriate amount of water, heating in water bath to dissolve, cooling, diluting with water to scale, and shaking to obtain standard berberine sulfate solution with concentration of 2.0%;
2) and (3) measuring the adsorption force:
taking 0.2g of montmorillonite fine powder with the granularity of less than 45 mu m, precisely weighing, placing in a conical flask with a plug, precisely adding 10ml of phosphate buffer solution with the pH of 6.8, shaking up, precisely adding 10ml of berberine sulfate standard solution with the concentration of 2.0%, placing in a water bath at 37 ℃, shaking up for 1 hour, filtering, precisely measuring 10ml of subsequent filtrate, placing in a 250ml measuring flask, diluting to scale with phosphate buffer solution with the pH of 6.8, shaking up, precisely measuring 5ml, placing in a 25ml measuring flask, diluting to scale with phosphate buffer solution with the pH of 6.8, shaking up, and measuring absorbance at the wavelength of 420nm according to an ultraviolet-visible spectrophotometry, the general rule 0401 of the national pharmacopoeia 2015 edition, with the pH of 6.8 as a blank; diluting the above 2.0% berberine sulfate standard solution with phosphate buffer solution with pH of 6.8 to obtain solution containing 40 μ g per 1ml, measuring absorbance by the same method, and calculating adsorption force according to the following formula;
adsorption capacity (g/g) = (2A)1-A2）×M1×D2/M2/A1/D1
A1: absorbance of berberine sulfate control solution
A2: absorbance of test solution
M1: weight of berberine sulfate
M2: weight of test article
D1: dilution multiple of berberine sulfate reference solution
D2: and (4) diluting the test solution by multiple times.
6. The method for measuring the adsorption ability of montmorillonite according to claim 4, characterized in that: preferably, the measurement wavelength is 420nm, and the absorption peaks of berberine sulfate further include 228nm, 264nm and 345 nm.
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| CN113340939A (en) * | 2021-06-23 | 2021-09-03 | 太原理工大学 | Method for measuring dipolar interaction between montmorillonite and organic matter in aqueous solution |
| CN114371212A (en) * | 2022-01-04 | 2022-04-19 | 多多药业有限公司 | Analysis method of montmorillonite powder |
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