AU2021101503A4 - Method for detecting the content of constants and impurity elements in montmorillonite, powders and tablets thereof - Google Patents
Method for detecting the content of constants and impurity elements in montmorillonite, powders and tablets thereof Download PDFInfo
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Abstract
The present disclosure belongs to the technical field of analytical chemistry, and particularly
relates to a method for detecting constants and impurity elements in montmorillonite, powders
and tablets thereof. The detection method specifically includes the following steps of:
preparation of a test solution: precisely weighing and taking the fine powder of a test sample,
adding nitric acid and water, sealing and soaking overnight, and adding hydrofluoric acid for
microwave digestion; cooling and adding a saturated boric acid solution for secondary
microwave digestion; then, cooling after the digestion, and shaking uniformly after diluting;
preparation of a standard curve solution: respectively taking a standard curve solution, an
internal standard solution and a test solution for irradiation by inductively coupled plasma mass
spectrometry and measurement by an internal-calibration standard curve method. In the present
disclosure, the sample is pretreated by microwave digestion for two times; and inductively
coupled plasma mass spectrometer (ICP-MS) is combined to measure the content of magnesium
and aluminum simultaneously. Further, the method of the present disclosure is simple, precise,
highly reproducible, highly sensitive and the like; and achieves the simultaneous measurement of
the magnesium and aluminum content.
1/1
Fig. 1
Description
1/1
Fig. 1
Field of the Invention
The present disclosure belongs to the technical field of analytical chemistry, and particularly relates to a method for detecting constants and impurity elements in montmorillonite, powders and tablets thereof.
Background of the Invention
Montmorillonite is a kind of layered mineral composed of ultra-finely granular hydrous aluminum silicates, and is a major component of bentonite which is formed by the alteration of volcanic ignimbrite and other igneous rocks in an alkaline environment. Montmorillonite is mainly used for treating acute and chronic diarrhea of adults and children and for adjusting intestinal flora, and has the function of protecting gastrointestinal mucosa. The pharmacological action of montmorillonite is from the charging property and ion exchange property thereof, so that montmorillonite has fixation and inhibition effects on digestive tract viruses, germs and toxins produced thereby. Therefore, the content of metal ions in the montmorillonite and the content of montmorillonite has a significant impact on the curative effect of the montmorillonite powder. The ratio of magnesium to aluminum in montmorillonite has a great influence on the adsorption capacity of montmorillonite, and is easy to interfere with the adsorption capacity in the quality standard of montmorillonite. At the same time, the metal residue in medicines is harmful to human health. Therefore, the ratio of magnesium to aluminum and the exceedance of metal contents in montmorillonite have become the foci of attention. Further, it has been found that iron also has a great effect on the efficacy of montmorillonite, and the content of iron is relatively high in montmorillonite; thereby, there are different levels of distinctions in property.
In the prior art, most of the studies are directed to the measurement of the content of aluminum oxide in montmorillonite, montmorillonite powders and tablets thereof; while, there are less studies on the control method of the magnesium content. Based on the quality control standard of the purified bentonite in USP40-NF35, it is explicitly stipulated that the ratio of aluminum content to and magnesium content ranges from 3.5 to 5.5; and the content of magnesium and aluminum is measured by atomic absorption spectrophotometry. Meanwhile, there are shortcomings, such as too long sample pretreatment time, complicated operation, easy introduction of interference, loss and the like, poor detection mode specificity, low sensitivity, and poor stability in the existing methods for measuring the content of macroelements and impurity elements in montmorillonite, montmorillonite powders and tablets at home and abroad currently, especially the measurement for the content of aluminum oxide. At the same time, individual treatment and individual measurement modes are adopted in the existing domestic methods for measuring the content of magnesium and aluminum in montmorillonite, montmorillonite powders and the tablets thereof, and pretreatment methods thereof. Moreover, the sample pretreatment methods are complex and too time-consuming. Therefore, it is an urgent problem to research and develop a detection method which is simple in operation, high in sensitivity, good in accuracy and capable of detecting all elements simultaneously.
Summary of the Invention
Aiming at the problems in the prior art, the present disclosure provides a detection method capable of simultaneously detecting the content of magnesium and aluminum in montmorillonite and powders thereof.
To achieve the above objective, the technical solution adopted in the present disclosure is as follows.
The invention provides a method for detecting the content of constants and impurity elements in montmorillonite, montmorillonite powders and tablets thereof, including the following steps:
(1) preparation of a test solution: precisely weighing and taking the fine powder of a test sample and placing into a digestion tank; adding nitric acid and water; sealing and soaking overnight; then adding hydrofluoric acid for microwave digestion; cooling the digestion tank after the digestion, and adding a saturated boric acid solution for secondary microwave digestion; cooling the digestion tank after the digestion; and then shaking uniformly after diluting to obtain a test solution;
(2) preparation of a standard curve solution: precisely measuring and taking a proper amount of a standard solution containing elements to be measured, and then diluting the solution with a proper amount of solvent to obtain a mixed standard curve solution containing elements to be measured in a proper concentration;
(3) respectively taking the standard curve solution, an internal standard solution and the test solution, and irradiating by inductively coupled plasma mass spectrometry and measuring by an internal standard-corrected curve method.
Further, the step (1) is specifically as follows: precisely weighing and taking a proper amount of the fine powder of a test sample, placing into a digestion tank; adding a proper amount of nitric acid and water; sealing and soaking overnight, adding hydrofluoric acid for microwave digestion; then cooling the digestion tank after the digestion; and adding a saturated boric acid solution for secondary microwave digestion, then cooling the digestion tank after the digestion; transferring the mixed solution into a proper amount of a volumetric flask by water, shaking uniformly after keeping a constant volume by water; and diluting the above solution by an acid solution to prepare the product.
Further, in step (1), the solid-liquid ratio of the test sample to nitric acid is 0.1-0.5 g:1-22 mL; the volume ratio of the water to the total volume ranges from 0 to 3/5; and the solid-liquid ratio of the test sample to hydrofluoric acid is 0.5-1 g:3-22 mL; and the volume ratio of the hydrofluoric acid to the saturated boric acid solution is 1:6.
Further, the acid solution for dilution is a nitric acid solution or a hydrochloric acid solution; the concentration of the nitric acid solution ranges from 0.1% to 10%; and the concentration of the hydrochloric acid solution ranges from 0.02 mol/L to 1 mol/L.
Further, in step (1), the microwave digestion conditions are:
Heating-up time (min) Temperature (°C) Holding time (min) 5 120 3 6 150 2 6 180 20 70 13 or
Heating-up time (min) Power (W) Holding time (min) 10 450 5 10 800 5 10 1300 20 70 13
Further, in step (2), when the elements to be measured are magnesium and aluminum, the specific operation is as follows: respectively precisely measuring and taking a proper amount of Mg/Al standard solution respectively; and diluting the Mg/Al standard solution into a mixed standard solution by using a nitric acid solution having a consistent concentration with the nitric acid for the preparation of the test solution, where the Mg concentration is successively 0 ng, 10 ng, 20 ng, 60 ng, 120 ng and 240 ng per1 ml of the mixed standard solution; and Al concentration is successively 0 ng, 25 ng, 50 ng, 150 ng, 300 ng and 500 ng per 1 ml of the mixed standard solution.
Further, in step (3), the internal standard solution is prepared as follows: precisely measuring and taking a proper amount of a standard solution containing a single internal standard element, and diluting the solution with a solvent to obtain an internal standard solution containing rhodium with a concentration of 10-100 ng/ml; and the internal standard element is rhodium, scandium, indium or bismuth.
Further, a collision mode is used for the measurement by inductively coupled plasma mass spectrometry; the collision gas is He gas, the collision gas flow is 3.5 ml/min, and the repetition number is 3.
The present disclosure can be applicable to the detection of all metal impurities in montmorillonite, montmorillonite powders and tablets thereof, for example: lead, arsenic, cadmium, mercury, cobalt, vanadium, nickel, magnesium, titanium, chromium, iron, zinc, barium, tin, antimony, platinum, lithium, copper, sulfur, platinum, molybdenum, palladium and other 22 impurity elements; meanwhile, the present disclosure can be further used for measuring the content of silicon dioxide and iron content; and the present disclosure can achieve the measurement of magnesium and aluminum content simultaneously.
The present disclosure has the following beneficial effects: the measurement methods of magnesium and aluminum are integrated; the sample is pretreated by microwave digestion for two times, and the inductively coupled plasma mass spectrometry (ICP-MS) is combined to measure the content of magnesium and aluminum simultaneously. The method is simple, accurate, well reproducible and highly sensitive, and precisely controls the magnesium-aluminum ratio while achieving the simultaneous measurement of magnesium and aluminum content, thus improving working efficiency greatly. Meanwhile, the sample pretreatment method and detection method can also be applied to the inspection of all metal impurities in montmorillonite, montmorillonite powders and tablets, and the measurement of silicon dioxide and metal content of silicate mineral medicines, thus greatly shortening the work task and promoting the working efficiency.
Brief Description of the Drawings
Fig. 1 is a comparison diagram of sample microwave digestion of a bulk drug and a formulation thereof under different conditions.
Detailed Description of the Embodiments
The present disclosure will be further explained and described in details with reference to the embodiments.
Example 1
(1) Preparation of a test solution: 0.1 g fine powder was weighed and taken precisely and placed into a digestion tank; 6 ml nitric acid and 9 ml water were added, and an inner cover was covered well for soaking overnight; then 0.5 ml hydrofluoric acid was added and placed into a microwave digestion instrument for digestion according to a proper microwave digestion procedure; the digestion tank was cooled after the digestion; 3 ml saturated boric acid solution were added and placed into the microwave digestion system for digestion according to the proper microwave digestion procedure; the digestion tank was cooled after the digestion; and the mixed solution was transferred into a 50 ml teflon volumetric flask by water, diluted to the scale, and shaken uniformly; then 5 ml of the solution were precisely measured and placed into a 50 ml volumetric flask; 1% nitric acid was added to dilute to the scale and shaken uniformly; and 0.5 ml solution was precisely measured and placed into a 50 ml volumetric flask, then 1% nitric acid was added to dilute to the scale and shaken uniformly.
The microwave digestion procedure was shown in Table 1:
Table 1
Heating-up time (min) Temperature (°C) Holding time (min) 5 120 3 6 150 2 6 180 20 70 13
(2) Preparation of a standard curve solution: a proper amount of magnesium/aluminum standard solution was weighed and taken respectively and precisely, and then diluted into a mixed standard solution with a 1% nitric acid solution; where the Mg concentration was successively 0 ng, 10 ng, 20 ng, 60 ng, 120 ng and 240 ng per 1 ml of the mixed standard solution; and the Al concentration was successively Ong, 25 ng, 50 ng, 150 ng, 300 ng and 500 ng per 1 ml of the mixed standard solution.
(3) Preparation of an internal standard solution: a proper amount of a rhodium-containing single element standard solution was weighed and taken precisely, and then diluted into an internal standard solution containing 50 ng/ml rhodium by a 1% nitric acid solution.
(4) Blank solution: 1% nitric acid solution.
The blank solution, mixed standard curve solution, internal standard solution and the test solution were respectively taken and irradiated by inductively coupled plasma mass spectrometry (Method One of General Rule 0412 of Chinese Pharmacopoeia(2005 Edition) Volume II) and measured by an internal-calibration standard curve method. A collision mode was used in the instrument; the collision gas flow was 3.5 ml/min; and the repetition number was 3.
Specific results were shown in Tables 2-6;
Table 2 Statistics on the Method Precision of Magnesium and Aluminum
Aluminum Sample Magnesium Detection Detection value size (g) value (ng/ml) Content (mg/g) (ng/ml) Content (mg/g)
0.1067 52.567 24.633 216.235 101.328
0.1074 51.155 23.815 217.616 101.311
0.1001 48.712 24.331 203.908 101.852
0.1048 50.409 24.050 213.331 101.780 0.1056 52.404 24.812 214.071 101.359
0.1052 51.664 24.555 213.527 101.486
RSD % 1.6 0.3
Table 3 Statistics on the Method Precision of Magnesium
Sample Magnesium Number weight Detection Blank Addition Recovery rate (g) value (ng/ml) size (g) ([tg) (%)
Solution-i 0.1010 79.051 2.46 99.44
Solution-2 0.1012 79.327 2.47 100.03
Solution-3 0.1032 80.066 2.51 99.25 1500 Solution-4 0.1011 79.202 2.46 99.78
Solution-5 0.1048 80.931 2.55 99.53
Solution-6 0.1059 81.443 2.58 99.45
Table 4 Statistics on the Method Precision of Aluminum
Sample Aluminum Number weight Detection Blank Addition Recovery rate (g) value (ng/ml) size (g) ([tg) (%)
Solution-i 0.1010 305.214 10.25 100.14
Solution-2 0.1012 306.694 10.27 101.22
Solution-3 0.1032 309.720 10.48 100.18 5000 Solution-4 0.1011 306.303 10.26 101.03
Solution-5 0.1048 314.616 10.64 101.83
Solution-6 0.1059 316.332 10.75 101.31
Table 5 Statistics on Limit of Detection (LOD) and Limit of Quantitation (LOQ) of Magnesium
Concentration Standard LOD concentration LOQ concentration Number (ng/ml) deviation (ng/ml) (ng/ml)) 1 0.037 2 -0.145 3 -0.068 4 0.120 5 0.151 6 -0.011 0.081 0.242 0.807 7 -0.011 8 0.011 9 0.043 10 -0.013 11 0.014
Remarks: a blank solvent (a blank digestion solvent) was taken and subjected to parallel determination for 11 continuous measurement; the LOD concentration of magnesium was calculated according to C = 3SD (SD: a standard deviation of the 11 concentration values of the blank solution); and then the LOQ concentration of magnesium was calculated according to C= 1OSD.
Table 6 Statistics on LOD and LOQ of Aluminum
Standard LOD concentration LOQ concentration Number Response values (ng/ml) deviation (ng/ml) (ng/ml)) 1 0.763 2 0.270 3 0.248 4 0.765 5 0.486 6 0.316 0.199 0.597 1.990 7 0.484 8 0.460 9 0.156 10 0.353 11 0.311
Remarks: a blank solvent (a blank digestion solvent) was taken and subjected to parallel determination for 11 continuous measurement; the LOD concentration of aluminum was calculated according to C = 3SD (SD: a standard deviation of the 11 concentration values of the blank solution); and then the LOQ concentration of aluminum was calculated according to C = 10SD.
Fig. 1 respectively shows the results of the bulk drug after being subjected to the first microwave digestion without the secondary microwave digestion, and the bulk drug after being subjected to the first microwave digestion with the secondary microwave digestion; the bulk drug after being subjected to the second microwave digestion without the secondary microwave digestion, and the bulk drug after being subjected to the second microwave digestion with the secondary microwave digestion; the formulation after being subjected to the first microwave digestion without the secondary microwave digestion, and the formulation after being subjected to the first microwave digestion with the secondary microwave digestion; and the formulation after being subjected to the second microwave digestion without the secondary microwave digestion, and the formulation after being subjected to the second microwave digestion with the secondary microwave digestion in the following order (from left to right). It can be seen from Fig. 1 that when the bulk drug and the formulation are subjected to microwave digestion only for once, the digestion method is unstable, and causes different degrees of precipitation phenomena; after a certain proportion of saturated boric acid solution is added for secondary microwave digestion, no precipitation occurs. Therefore, the digestion method is relatively stable, and the specific detection results are shown in Table 7.
Table 7 Comparison of data for samples with and without secondary microwave digestion
Measured value of magnesium Measured value of aluminum (g/g) (g/g) No Presence No Presence Number Conditions secondary of second True secondary of second True microwave microwave value microwave microwave value digestion digestion digestion digestion Microwave 6.41 14.94 37.48 65.42 digestion 1 1 14.02 65.42 Microwave 11.78 14.87 62.27 65.41 digestion 2 Microwave 8.87 15.92 34.59 68.36 2 digestion 1 15.92 68.39 Microwave 13.14 15.93 64.83 68.42 digestion 2 Microwave 101.1 19.35 27.51 54.63 digestioni1 9 3 27.53 9 101.22 Microwave 101.2 25.47 27.39 98.54 digestion 2 4 Microwave 6.32 14.94 21.09 59.87 4 digestion 1 14.89 59.84 Microwave 11.74 14.97 54.32 59.84 digestion 2 Microwave 5 11.38 20.73 20.79 29.36 77.20 77.22 digestion 1
Microwave 17.96 20.83 74.58 77.24 digestion 2 Microwave 8.64 19.32 32.87 76.85 6 digestion 1 19.39 76.82 Microwave 17.97 19.40 72.93 76.84 digestion 2
Remarks: 1. Number denotes the manufacturer's code; No. 1-3 denote the bulk drug, and No. 4-6 denote the formulation;
2. Unit g/g = detection value * dilution factor/sample size, where g/g represents an amount of magnesium or aluminum per 1 g of the sample;
3. The procedure of microwave digestion 1 is the same as that of microwave digestion 2. The data were compared only for the different phenomena after microwave digestion;
It can be seen from Table 7 that the data of the magnesium and aluminum content in the sample without secondary digestion are unstable and have larger deviation from the true value, and the data of the magnesium and aluminum content in the sample with secondary microwave digestion are stable and close to the true value.
Comparative Example 1 Method for measuring the content of aluminum oxide in montmorillonite, powders and tablets in accordance with the Chinese Pharmacopoeia (2020 Edition) Volume II
The specific results were shown in Table 8.
Table 8 Comparison on data of the aluminum content in montmorillonite measured by the method stipulated in Chinese Pharmacopoeia(2020 Edition) and the method of the present disclosure
Chinese Item Pharmacopoeia The present disclosure
Al 2 03 content(%) 21.430% 19.14%
In the Chinese Pharmacopoeia(2020 Edition) Volume II, complexometry was used to judge the titration end point when the indicating liquid changed color. The sensitivity was poorer than that of the method in the present disclosure; the titration value was larger than that of the method in the present disclosure, the EDTA titrating solution can be subjected to complex reaction with 2+ + 2, 2 2+ Zn2, Pb , Hg 2 ', Ca2, and Fe and other ions. Since montmorillonite contains complex element impurities, the method in the pharmacopoeia has poor specificity, while the present disclosure is free from specificity problems.
Comparative Example 2 Method for measuring the content of magnesium and aluminum in purified bentonite in accordance with USP 40-NF 35
Limit specifications: the content ratio of aluminum to magnesium ranged from 3.5 to 5.5.
The specific results were shown in Table 9
Table 9 Comparison on data of the magnesium and aluminum content in montmorillonite measured by the method of the present disclosure and the detection method of the purified bentonite in USP-40-NF 35
Item USP-40-NF35 The present disclosure Magnesium content 25.735 20.633
(mg/g) Aluminum content 101.328 113.522 (mg/g)
Based on the method for measuring the content of aluminum oxide and magnesium in the purified bentonite stipulated in the USP40-NF35, the pretreatment process of the sample is implemented in an open environment; the operation is complex; moreover, there are a large amount of magnesium and aluminum elements in the nature; if the sample is pretreated in an open environment, the measured content of the magnesium and aluminum is to be slightly higher, and has a minor deviation compared with the true value. In the present disclosure, the whole sample is pretreated in a closed environment. Moreover, the method is easy to operate and can achieve the simultaneous measurement of magnesium and aluminum elements; therefore, the method of the disclosure is more superior.
Comparative Example 3 Method for measuring the content of aluminum oxide in montmorillonite powders and tablets thereof in accordance with the Chinese Pharmacopoeia (2020 Edition) Volume II
The specific results were shown in Table 10
Table 10 Comparison on data of the aluminum content in montmorillonite measured by the method stipulated in Chinese Pharmacopoeia(2020 Edition) and the method of the present disclosure
Powder Tablet Item Chinese The present Chinese The present Pharmacopoeia disclosure Pharmacopoeia disclosure A1 2 0 3 22.54% 19.94% 21.17% 19.22% content (%)
The method for measuring the content of aluminum oxide in montmorillonite powders and tablets thereof has the shortcomings of an open environment for the pretreatment method, complicated operation and poor specificity of the detection method.
Claims (8)
1. A method for detecting the content of constants and impurity elements in montmorillonite, montmorillonite powders and tablets thereof, characterized by comprising the following steps of: (1) preparation of a test solution: precisely weighing and taking a fine powder of a test sample and placing into a digestion tank; adding nitric acid and water; sealing and soaking overnight; then adding hydrofluoric acid for microwave digestion; cooling the digestion tank after the digestion, and adding a saturated boric acid solution for secondary microwave digestion; cooling the digestion tank after the digestion; and then shaking uniformly after diluting to obtain a test solution; (2) preparation of a standard curve solution: precisely measuring and taking a proper amount of a standard solution containing elements to be measured, and then diluting the solution with a proper amount of a solvent to obtain a mixed standard curve solution containing elements to be measured in a proper concentration; (3) respectively taking the standard curve solution, an internal standard solution and the test solution, and irradiating by inductively coupled plasma mass spectrometry and measuring by an internal standard-calibrated curve method.
2. The detecting method according to claim 1, characterized in that the step (1) is specifically as follows: precisely weighing and taking a proper amount of the fine powder of the test sample, placing into the digestion tank; adding a proper amount of nitric acid and water; sealing and soaking overnight, and adding hydrofluoric acid for microwave digestion; then cooling the digestion tank after the digestion; and adding a saturated boric acid solution for secondary microwave digestion, then cooling the digestion tank after the digestion; transferring the mixed solution into a proper amount of a volumetric flask by water, shaking uniformly after keeping a constant volume by water; and diluting the above solution by an acid solution to prepare the product.
3. The detecting method according to claim 2, characterized in that in step (1), the solid-liquid ratio of the test sample to nitric acid is 0.1-0.5 g:1-22 mL; the volume ratio of the water to the total volume ranges from 0 to 3/5; and the solid-liquid ratio of the test sample to hydrofluoric acid is 0.5-1 g:3-22 mL; and the volume ratio of the hydrofluoric acid to the saturated boric acid solution is 1:6.
4. The detecting method according to claim 3, characterized in that the acid solution for dilution is a nitric acid solution or a hydrochloric acid solution; the concentration of the nitric acid solution ranges from 0.1% to 10%; and the concentration of the hydrochloric acid solution ranges from 0.02 mol/L to 1 mol/L.
5. The detecting method according to any one of claims 1-4, characterized in that in step (1), the microwave digestion conditions are as follows:
Heating-up time (min) Temperature (°C) Holding time (min) 5 120 3 6 150 2 6 180 20 70 13
or
Heating-up time (min) Power (W) Holding time (min) 10 450 5 10 800 5 10 1300 20 70 13
6. The detecting method according to claim 1, characterized in that in step (2), when the elements to be measured are magnesium and aluminum, the specific operation is as follows: precisely measuring and taking a proper amount of Mg/Al standard solution respectively; and diluting the Mg/Al standard solution into a mixed standard solution by using a nitric acid solution having a consistent concentration with the nitric acid for the preparation of the test solution, wherein the Mg concentration is successively 0 ng, 10 ng, 20 ng, 60 ng, 120 ng and 240 ng per 1 ml of the mixed standard solution; and Al concentration is successively 0 ng, 25 ng, 50 ng, 150 ng, 300 ng and 500 ng per1 ml of the mixed standard solution.
7. The detecting method according to claim 1, characterized in that in step (3), the internal standard solution is prepared as follows: precisely measuring and taking a proper amount of a standard solution containing a single internal standard element, and diluting the solution with a solvent to obtain an internal standard solution containing rhodium with a concentration of 10-100 ng/ml; and the internal standard element is rhodium, scandium, indium or bismuth.
8. The detecting method according to any one of claims 1 to 7, characterized in that a collision mode is used for the measurement by inductively coupled plasma mass spectrometry; the collision gas is He gas, the collision gas flow is 3.5 ml/min, and the repetition number is 3.
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| CN114609234B (en) * | 2022-02-24 | 2024-08-30 | 浙江皇马科技股份有限公司 | Method for detecting content of metal element in polyether amine solid catalyst |
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| CN101762632A (en) * | 2009-11-20 | 2010-06-30 | 广东省惠州市石油产品质量监督检验中心 | Method for determining silicon content in naphtha through microwave digestion ICP-MS method |
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| CN118243829B (en) * | 2024-05-29 | 2024-08-30 | 南通大学附属医院 | Method for detecting effective components of montmorillonite medicament for treating diarrhea |
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