CN113588807B - Method for measuring gypsum content in traditional Chinese medicine decoction - Google Patents
Method for measuring gypsum content in traditional Chinese medicine decoction Download PDFInfo
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- 239000010440 gypsum Substances 0.000 title claims abstract description 96
- 229910052602 gypsum Inorganic materials 0.000 title claims abstract description 96
- 238000000034 method Methods 0.000 title claims abstract description 49
- 239000003814 drug Substances 0.000 title claims abstract description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 87
- 239000000243 solution Substances 0.000 claims abstract description 79
- 239000011575 calcium Substances 0.000 claims abstract description 49
- 239000012488 sample solution Substances 0.000 claims abstract description 47
- 239000013558 reference substance Substances 0.000 claims abstract description 29
- 239000000523 sample Substances 0.000 claims abstract description 28
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 21
- 238000001514 detection method Methods 0.000 claims abstract description 17
- 239000012088 reference solution Substances 0.000 claims abstract description 14
- 230000035945 sensitivity Effects 0.000 claims abstract description 10
- 238000004255 ion exchange chromatography Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 238000002360 preparation method Methods 0.000 claims description 28
- 239000000706 filtrate Substances 0.000 claims description 19
- 238000001914 filtration Methods 0.000 claims description 17
- 239000000126 substance Substances 0.000 claims description 15
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical group [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 9
- 239000003480 eluent Substances 0.000 claims description 8
- 230000001629 suppression Effects 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 7
- 238000001724 coherent Stokes Raman spectroscopy Methods 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 6
- 208000004371 toothache Diseases 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 239000008187 granular material Substances 0.000 claims description 4
- 239000012085 test solution Substances 0.000 claims description 4
- 230000003110 anti-inflammatory effect Effects 0.000 claims description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 3
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 abstract description 14
- 229910001424 calcium ion Inorganic materials 0.000 abstract description 14
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 37
- 229910021642 ultra pure water Inorganic materials 0.000 description 22
- 239000012498 ultrapure water Substances 0.000 description 22
- 238000005303 weighing Methods 0.000 description 19
- 238000011835 investigation Methods 0.000 description 13
- 238000005259 measurement Methods 0.000 description 12
- 238000011084 recovery Methods 0.000 description 12
- 238000000605 extraction Methods 0.000 description 11
- 239000003153 chemical reaction reagent Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 9
- 239000002904 solvent Substances 0.000 description 9
- 238000009835 boiling Methods 0.000 description 8
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 238000012986 modification Methods 0.000 description 7
- 230000004048 modification Effects 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
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- 150000002500 ions Chemical class 0.000 description 5
- 239000000463 material Substances 0.000 description 5
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- 230000014759 maintenance of location Effects 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- HNSDLXPSAYFUHK-UHFFFAOYSA-N 1,4-bis(2-ethylhexyl) sulfosuccinate Chemical compound CCCCC(CC)COC(=O)CC(S(O)(=O)=O)C(=O)OCC(CC)CCCC HNSDLXPSAYFUHK-UHFFFAOYSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 238000009614 chemical analysis method Methods 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
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- 238000005516 engineering process Methods 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 238000012417 linear regression Methods 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 229940098779 methanesulfonic acid Drugs 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 238000009777 vacuum freeze-drying Methods 0.000 description 2
- 241001061264 Astragalus Species 0.000 description 1
- 235000010110 Astragalus glycyphyllos Nutrition 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- 101100136092 Drosophila melanogaster peng gene Proteins 0.000 description 1
- 208000000059 Dyspnea Diseases 0.000 description 1
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- 208000015220 Febrile disease Diseases 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229930182555 Penicillin Natural products 0.000 description 1
- JGSARLDLIJGVTE-MBNYWOFBSA-N Penicillin G Chemical compound N([C@H]1[C@H]2SC([C@@H](N2C1=O)C(O)=O)(C)C)C(=O)CC1=CC=CC=C1 JGSARLDLIJGVTE-MBNYWOFBSA-N 0.000 description 1
- 208000001431 Psychomotor Agitation Diseases 0.000 description 1
- 206010038743 Restlessness Diseases 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052925 anhydrite Inorganic materials 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 235000006533 astragalus Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- ZHZFKLKREFECML-UHFFFAOYSA-L calcium;sulfate;hydrate Chemical compound O.[Ca+2].[O-]S([O-])(=O)=O ZHZFKLKREFECML-UHFFFAOYSA-L 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000003926 complexometric titration Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 235000008216 herbs Nutrition 0.000 description 1
- 208000021760 high fever Diseases 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 229940049954 penicillin Drugs 0.000 description 1
- 206010036067 polydipsia Diseases 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 229910052600 sulfate mineral Inorganic materials 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- 230000035922 thirst Effects 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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- Physics & Mathematics (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to a method for measuring gypsum content in a traditional Chinese medicine decoction, which comprises the following steps: preparing a reference substance solution and a sample solution respectively, and detecting the reference substance solution and the sample solution by adopting an ion chromatography; the reference solution comprises Ca-containing 2+ Is/are SO-containing and/or reference substance solution of (C) 4 2‑ Is a reference solution; in the process of preparing the sample solution, hydrochloric acid is adopted to dissolve the traditional Chinese medicine decoction to be tested. The invention adopts hydrochloric acid to pretreat the traditional Chinese medicine decoction to be detected, and calcium ions and sulfate ions are in a completely free state in a sample solution obtained by the pretreat, and gypsum content is accurately measured when the sample is loaded to ion chromatography for detection. Meanwhile, the invention has the advantages of simple operation, rapid detection, high sensitivity, good selectivity and good repeatability.
Description
Technical Field
The invention belongs to the technical field of medicines, and particularly relates to a method for measuring gypsum content in a traditional Chinese medicine decoction.
Background
The gypsum is gypsum of sulfate mineral gypsum family, and contains mainly water-containing calcium sulfate (CaSO 4 ·2H 2 O), removing the sundry stones and sediment after digging. Gypsum Fibrosum is a medicinal material in the provincial way of Hubei provincial area, is also a mineral Chinese medicine with characteristics and advantages in clinic, has the effects of clearing heat and purging fire and relieving restlessness and quenching thirst, and is used for treating exogenous febrile disease, high fever and polydipsia, lung heat and dyspnea and cough, excessive stomach fire, headache and toothache. It has been found that gypsum contains abundant trace elements in addition to a large amount of calcium elements, such as: magnesium (Mg), zinc (Zn), manganese (Mn), copper (Cu), iron (Fe), strontium (Sr), and the like. According to regulations, the gypsum contains not less than 95.0% of calcium sulfate (national pharmacopoeia Committee. Pharmacopoeia of the people's republic of China. Beijing: china medical science and technology Press 2015: 248-249).
In the existing method, the method for determining the content of the calcium sulfate hydrate in the gypsum medicinal material provided in Chinese pharmacopoeia of 2020 edition is a titration method. At present, besides the methods in the pharmacopoeia, the method for measuring the content of the hydrous calcium sulfate in the gypsum mainly comprises the following steps: measurement of sulfur trioxide recorded in a barium sulfate gravimetric method, namely a standard method, GBT 5484-2000, gypsum chemical analysis method; ion exchange method for measuring sulfur trioxide, the ion exchange method for measuring sulfur trioxide described in GB/T5484-1985 chemical analysis method for gypsum and anhydrite; the content of the water-containing calcium sulfate can be indirectly measured by measuring the calcium ions in the water-containing calcium sulfate by a complexometric titration method and GB 1892-1980 food additive calcium sulfate; ion chromatography to determine sulfate ions in gypsum involves the following technical literature: zhou Qiaoli, lu Lijun, kingdom, plasma chromatography to determine sulfate in calcium sulfate samples. Chemometrics, 2014, 23 (Z1): 19-21; milkvetch, yao Yating, he Peng, plasma chromatography to determine sulfur trioxide in gypsum. Physicochemical test-chemical division, 2015, 51 (11): 1566-1568; the method for measuring the mutual interference of the sulfite and the sulfide can be established by CN103063781A, realizes the respective measurement of the sulfite content and the sulfide content, and can be used for gypsum and building materials such as gypsum products, cement, sand and the like.
However, the inventor finds that when the traditional detection technology is applied to the gypsum detection of the traditional Chinese medicine decoction, the defect of inaccurate detection results exists.
Disclosure of Invention
Based on the above, the main purpose of the invention is to provide a method for measuring the gypsum content in the traditional Chinese medicine decoction, which is necessary to solve the problem of inaccurate gypsum detection in the traditional Chinese medicine decoction.
The technical scheme of the invention comprises the following steps:
a method for measuring the gypsum content in a traditional Chinese medicine decoction comprises the following steps:
preparing a reference substance solution and a sample solution respectively, and detecting the reference substance solution and the sample solution by adopting an ion chromatography;
the reference solution comprises Ca-containing 2+ Is/are SO-containing and/or reference substance solution of (C) 4 2- Is a reference solution;
preparing the sample solutionThe step of extracting Ca from the Chinese medicinal decoction to be detected by hydrochloric acid 2+ Or/and SO 4 2- 。
In one embodiment, the hydrochloric acid contains 1.35-1.65% of hydrogen chloride by mass.
In one embodiment, the control solution is Ca-containing solution 2+ The conditions for detection include:
protective column: ionPac CG12A (4X 50mm,8 μm);
analytical column: ionPac CS12A (4X 250mm,8 μm);
a suppressor: CSRS 4mm;
eluent: methane sulfonic acid solution with the concentration of 15 mmol/L-25 mmol/L;
flow rate: 0.5-0.9 mL/min;
column temperature: 25-35 ℃;
detecting the temperature of the cell: 30-40 ℃;
suppression current: 45mA to 49mA.
In one embodiment, the detected condition further comprises:
sensitivity of the detector: 4.5 mu S/cm-5.5 mu S/cm;
sample injection volume: 4.5 mu L to 5.5 mu L.
In one embodiment, the control solution is SO-containing 4 2- The conditions for detection include:
protective column: ionPac AG14 (4X 50mm,9 μm);
analytical column: ionPac AS14 (4X 250mm,9 μm);
a suppressor: ASRS 4mm;
eluent: na (Na) 2 CO 3 The concentration is 4 mmol/L-5 mmol/L, naHCO 3 1 mmol/L-1.8 mmol/L aqueous solution;
flow rate: 1 mL/min-1.5 mL/min;
column temperature: 25-35 ℃;
detecting the temperature of the cell: 30-40 ℃;
suppression current: 25 mA-35 mA.
In one embodiment, the detected condition further comprises:
sensitivity of the detector: 4.5 mu S/cm-5.5 mu S/cm;
sample injection volume: 4.5 mu L to 5.5 mu L.
In one embodiment, the dosage of the hydrochloric acid corresponding to each 1g of the traditional Chinese medicine decoction to be tested is 250 mL-350 mL.
In one embodiment, the step of preparing the test solution comprises: mixing the hydrochloric acid with the Chinese medicinal decoction to be tested, fixing volume, filtering, and collecting filtrate.
In one embodiment, each 1mL of the Ca-containing solution 2+ In the reference solution of (2), ca 2+ The mass of (C) is 8-12 mug.
In one embodiment, the Ca-containing gas is 2+ The preparation steps of the reference substance solution comprise: mixing standard substances of the calcium unit element solution and water.
In one embodiment, every 1mL of the SO-containing agent 4 2- In the reference solution of (2), SO 4 2- The mass of (C) is 10-15 mug.
In one embodiment, the SO-containing agent 4 2- The preparation steps of the reference substance solution comprise: mixing sulfate solution standard substance and water.
Compared with the prior art, the invention has the following beneficial effects:
the invention adopts hydrochloric acid to pretreat the traditional Chinese medicine decoction to be detected, and calcium ions and sulfate ions are in a completely free state in a sample solution obtained by the pretreat, and gypsum content is accurately measured when the sample is loaded to ion chromatography for detection. Meanwhile, the invention has the advantages of simple operation, rapid detection, high sensitivity, good selectivity and good repeatability.
Drawings
FIG. 1 is a graph of a linear investigation result of calcium ion content measurement of a gypsum standard decoction in one embodiment of the invention;
FIG. 2 is a graph of a linear investigation result of sulfate ion content measurement of gypsum standard decoction in one embodiment of the invention;
FIG. 3 is a diagram showing the results of a specific investigation of calcium ion content measurement of a gypsum standard decoction in one embodiment of the invention;
FIG. 4 is a graph showing the results of a specific study of sulfate ion content determination of gypsum standard decoction in one embodiment of the invention.
FIG. 5 is a graph showing the results of sulfate ion and calcium ion content determination of gypsum standard decoction in accordance with one embodiment of the present invention.
FIG. 6 is a graph showing the results of sulfate ion and calcium ion content determination of gypsum standard decoction in accordance with one embodiment of the present invention.
FIG. 7 is a graph showing the results of measuring the sulfate ion and calcium ion contents of the granule for treating odontalgia and inflammation according to one embodiment of the present invention.
FIG. 8 is a graph showing the results of the sulfate ion and calcium ion content determination of gypsum standard decoction according to one comparative example of the present invention.
Detailed Description
The present invention will be described more fully hereinafter in order to facilitate an understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
The embodiment of the invention provides a method for measuring gypsum content in a traditional Chinese medicine decoction, which comprises the following steps:
preparing a reference substance solution and a sample solution respectively, and detecting the reference substance solution and the sample solution by adopting an ion chromatography;
the reference substance solutionComprises Ca-containing 2+ Is/are SO-containing and/or reference substance solution of (C) 4 2- Is a reference solution;
the step of preparing the sample solution comprises extracting Ca in the Chinese medicinal decoction to be tested with hydrochloric acid 2+ Or/and SO 4 2- 。
In one example, the mass content of the hydrogen chloride contained in the hydrochloric acid is 1.35% to 1.65%, for example, may be 1.35%, 1.52%, 1.65%, or the like.
In one example, the control solution is Ca-containing 2+ The conditions for detection include:
protective column: ionPac CG12A (4X 50mm,8 μm);
analytical column: ionPac CS12A (4X 250mm,8 μm);
a suppressor: CSRS 4mm;
eluent: methane sulfonic acid solution with the concentration of 15 mmol/L-25 mmol/L;
flow rate: 0.5-0.9 mL/min;
column temperature: 25-35 ℃;
detecting the temperature of the cell: 30-40 ℃;
suppression current: 45mA to 49mA.
In one example, the detected condition further includes:
sensitivity of the detector: 4.5 mu S/cm-5.5 mu S/cm;
sample injection volume: 4.5 mu L to 5.5 mu L.
In one example, the control solution is SO-containing 4 2- The conditions for detection include:
protective column: ionPac AG14 (4X 50mm,9 μm);
analytical column: ionPac AS14 (4X 250mm,9 μm);
a suppressor: ASRS 4mm;
eluent: na (Na) 2 CO 3 The concentration is 4 mmol/L-5 mmol/L, naHCO 3 1 mmol/L-1.8 mmol/L aqueous solution;
flow rate: 1 mL/min-1.5 mL/min;
column temperature: 25-35 ℃;
detecting the temperature of the cell: 30-40 ℃;
suppression current: 25 mA-35 mA.
In one example, the detected condition further includes:
sensitivity of the detector: 4.5 mu S/cm-5.5 mu S/cm;
sample injection volume: 4.5 mu L to 5.5 mu L.
In one example, the dosage of the hydrochloric acid corresponding to each 1g of the traditional Chinese medicine decoction to be tested is 250 mL-350 mL.
In one example, the step of preparing the test solution includes: mixing the hydrochloric acid and the Chinese medicinal decoction to be tested, adding water to fix volume, filtering, and collecting filtrate. Specific operations may include: grinding the Chinese medicinal decoction to be tested, placing in a plastic bottle, adding hydrochloric acid, shaking, adding water to constant volume, and filtering to obtain filtrate.
In one example, each 1mL of the Ca-containing solution 2+ In the reference solution of (2), ca 2+ The mass of (C) is 8-12 mug. For example 8. Mu.g, 10. Mu.g, 12. Mu.g.
In one example, the Ca-containing 2+ The preparation steps of the reference substance solution comprise: mixing standard substances of the calcium unit element solution and water.
In one example, every 1mL of the SO-containing agent 4 2- In the reference solution of (2), SO 4 2- The mass of (C) is 10-15 mug. For example, 10. Mu.g, 13. Mu.g, 15. Mu.g.
In one example, the SO-containing agent 4 2- The preparation steps of the reference substance solution comprise: mixing sulfate solution standard substance and water.
The water used in the examples of the present invention was purified water.
The traditional Chinese medicine decoction according to the embodiment of the invention can be a standard decoction or a compound decoction. The standard decoction provided by the embodiment of the invention is a single Chinese medicinal decoction piece decoction prepared by a standard process based on the Chinese medicinal theory as a guide and clinical application. The compound decoction disclosed by the embodiment of the invention is a liquid preparation prepared by a method of decocting or soaking a plurality of medicines, removing residues and taking the decoction. The standard decoction of the embodiment of the invention is gypsum standard decoction, for example, the compound decoction can be a liquid preparation prepared from gypsum and other medicinal materials.
The following examples of the present invention illustrate the content of the present invention by way of example, but it is understood that this is not a further limitation of the present invention, and the gypsum standard decoction may be prepared by, but is not limited to, the following preparation methods:
decocting Gypsum Fibrosum decoction pieces in water, and drying the decoction.
The number of times of the decoction according to the embodiment of the present invention is preferably a plurality of times (e.g., 2 times, 3 times, 4 times, etc.), and if the number of times of the decoction is a plurality of times, the decoctions obtained by the plurality of times of the decoction may be combined and then dried. Preferably, the number of times of decoction is two.
Further, in the first decoction process, the water amount is 7-9 times of that of the gypsum decoction pieces, the gypsum decoction pieces are soaked for 25-35 min before decoction, and the decoction is heated and boiled by strong fire (the power is 450-550W) and then kept slightly boiled by slow fire (the power is 180-220W) for 40-50 min. After the decoction is finished, filtering the decoction while the hot by adopting a screen (namely decoction) to obtain filtrate, wherein the screen can be a 200-mesh screen, and the obtained filtrate can be cooled by cold water. In the step, the water adding amount can be 7 times, 7.5 times, 8 times, 8.5 times and 9 times of that of the gypsum decoction pieces, the time for soaking the gypsum decoction pieces before decoction can be 25min, 30min and 35min, the corresponding power of strong fire can be 450W, 470W, 490W, 500W, 520W and 550W, the corresponding power of slow fire can be 180W, 200W, 210W and 220W, and the time for keeping micro boiling can be controlled to be 40min, 45min and 50min.
Further, in the second decoction process, the water addition amount is 5-6.5 times of that of the gypsum decoction pieces, and the decoction is carried out by boiling with strong fire (the power is 450-550W) and then keeping micro-boiling with slow fire (the power is 180-220W) for 25-35 min. After the decoction is finished, filtering the decoction while the hot by adopting a screen (namely decoction) to obtain filtrate, wherein the screen can be a 200-mesh screen, and the obtained filtrate can be cooled by cold water. In the step, the water adding amount can be 5 times, 5.5 times, 6 times and 6.5 times of that of the gypsum decoction pieces, the corresponding power of the strong fire can be 450W, 470W, 490W, 500W, 520W and 550W, the corresponding power of the slow fire can be 180W, 200W, 210W and 220W, and the duration of keeping micro boiling can be controlled to be 25min, 30min and 35min.
It is understood that the resulting decoction may be concentrated (including but not limited to concentrated under reduced pressure) to a fluid extract prior to drying, including but not limited to vacuum freeze drying.
Example 1 measurement of calcium ion content
1 instrument and reagent
Instrument: ion chromatograph (Dionex ICS-6000, siemens technologies Co., ltd.); cation suppressor (CSRS 300 4mm, siemens technologies Co., ltd.); ionPac CG12A guard column (4X 50mm,8 μm); ionPac CS12A analytical column (4X 250mm,8 μm); one ten-thousandth analytical balance (ME 204E, mertrel-tolidox); ultrapure water systems (Milli-Q Direct, merck Co., ltd.).
Reagent: hydrochloric acid (guangzhou chemical reagent plant, top grade purity); methanesulfonic acid (ala Ding Shiji (Shanghai), 99.5%); the water was ultrapure water (laboratory homemade).
Reagent: standard substances of calcium unit cell solution (China national institute of metrology, concentration: 1000. Mu.g/mL, lot number: GBW (E) 080118); calcium sulfate dihydrate control (lot number: 202004171 source: beijing century Ortaceae Biotechnology Co., ltd.; content: 99.5%); the lot number information of 23 batches of gypsum medicinal materials and standard decoction is shown in Table 1.
Table 1, 23 Gypsum herbs and Standard decoction information Table
The 23 batches of gypsum standard decoction are prepared by taking gypsum decoction pieces in batches shown in Table 1 and processing the gypsum decoction pieces by the following process:
(1) Taking 100g of gypsum decoction pieces, adding water and decocting twice:
adding 8 times of water for the first time, soaking for 30 minutes, heating with strong fire (power 500W), boiling with slow fire (power 200W), keeping slight boiling for 45 minutes, filtering with 200 mesh screen, and cooling the filtrate with cold water;
adding 6 times of water for the second decoction, boiling with strong fire (power 500W), keeping micro-boiling with slow fire (power 200W) for 30min, filtering with 200 mesh screen, and cooling with cold water;
(2) Mixing the filtrates, concentrating under reduced pressure to obtain clear paste with volume of about 100ml, packaging into 10ml penicillin bottles, packaging into 3ml bottles, vacuum freeze drying, taking out, and rolling aluminum cap.
2 methods and results
2.1 chromatographic conditions
IonPac CG12A (4X 50mm,8 μm) guard column, ionPac CS12A (4X 250mm,8 μm) analytical column, CSRS 4mm inhibitor was selected; the solution of 20mmol/L methane sulfonic acid is a eluent; the flow rate is 0.8ml per minute; the column temperature is 30 ℃; the temperature of the detection tank is 35 ℃; the suppression current was 47mA; the detector sensitivity was 5 mus per cm; the sample volume was 5. Mu.l.
2.2 preparation of control solution
Taking appropriate amount of standard substance of calcium unitary element solution, precisely weighing, placing into 30ml plastic vial, adding ultrapure water to obtain solution containing Ca per 1ml 2+ 10 μg of the solution.
2.3 preparation of sample solutions
Taking about 0.1g of gypsum standard decoction, precisely weighing, placing into a 30ml plastic bottle, precisely adding 30ml of 1.52% hydrochloric acid, fully shaking to dissolve, shaking uniformly, precisely sucking 0.1ml of the solution, adding ultrapure water to dilute to 10ml, shaking uniformly, filtering, and taking filtrate to obtain the plaster.
2.4 methodology for measuring calcium ion content
2.4.1 linear relationship investigation
3.5237g of a standard substance of the calcium unit element solution is precisely weighed, placed in a 30ml plastic bottle, added with 30ml of ultrapure water and shaken uniformly to obtain a stock solution of the calcium ion reference substance.
Precisely weighing 0.1g,0.5g,1g,2g and 5g of the calcium ion reference stock solution, respectively placing into 30ml plastic bottles, adding 10ml of ultrapure water, weighing, shaking uniformly, and preparing reference application solution containing 1.243 mug, 6.0074 mug, 11.5940 mug, 23.378 mug and 57.705 mug in each 1 ml.
And respectively precisely sucking the reference substance application liquid and the reference substance stock liquid, sequentially injecting 5 μl according to the chromatographic conditions under the item "2.1", and recording the chromatographic peak area.
The standard curve is drawn with the peak area as the ordinate (y) and the reference substance concentration as the abscissa (x), and the result is shown in fig. 1. The results show that the linear regression equation of calcium ions is: y= 9.5663x-0.1123, correlation coefficient R 2 The concentration of =0.9999 showed good linear relationship between the concentration and the peak area in the range of 1.243 μg/ml to 117.320 μg/ml.
2.4.2 precision test
Preparing sample solution by precisely absorbing Gypsum standard decoction (GT 161022) according to the method under the term "2.3", repeatedly sampling for 6 times according to the chromatographic condition under the term "2.1", and recording Ca 2+ Peak area, RSD value of peak area was calculated.
The results show that the same sample solution is continuously injected into 6 needles, ca 2+ The peak area RSD value is 0.54% and less than 3.0%, which indicates that the instrument precision is good.
2.4.3 stability test
Precisely sucking Gypsum standard decoction (GT 161022), preparing sample solution according to "2.3" method, respectively sampling at 0,3,5,7,9 and 12 hr according to "2.1" chromatographic conditions, and recording Ca 2+ Peak area, RSD value of peak area was calculated.
The results show that after sample solutions are respectively injected at 6 time points, ca 2+ The RSD value of the peak area was 0.81%, indicating that the test sample solution had good stability over 12 hours.
2.4.4 repeatability test
About 0.1g of the same batch of gypsum standard decoction (GT 161022) is taken, precisely weighed, 6 parts are weighed in parallel, and the weight is 2.3", 6 parts of the sample solution is prepared. The Ca was calculated by measurement under the chromatographic conditions under the term "2.1 2+ Content and RSD value thereof.
The results are shown in Table 2, which shows that the same batch of samples was repeatedly assayed 6 times, ca 2+ The RSD value of the content was 1.27% and less than 1.5%, indicating good reproducibility of the assay.
TABLE 2 Standard decoction of Gypsum Fibrosum Ca 2+ Repeatability investigation result table
2.4.5 sample recovery rate investigation
Respectively precisely weighing 25mg, 50mg and 75mg of calcium sulfate dihydrate reference substances (batch number: 202004171 source: beijing century Orchidaceae biotechnology Co., ltd.; content: 99.5%) and placing into 30ml plastic measuring bottles, wherein each group is divided into 3 parts in parallel and 9 parts in total;
grinding appropriate amount of Gypsum Fibrosum standard decoction (batch number: GT 161022), respectively placing about 0.05g into the above 9 plastic bottles, precisely weighing, precisely adding 30ml of 1.52% hydrochloric acid, weighing, shaking sufficiently to dissolve, shaking uniformly, precisely sucking 0.1ml of the above solution, diluting to 10ml with ultrapure water, shaking uniformly, filtering, and collecting subsequent filtrate;
measurement is carried out according to the chromatographic condition under the item "2.1", and Ca in the test sample solution is measured 2+ The content is converted into the content of the hydrous calcium sulfate, and the sample adding recovery rate is calculated.
The results are shown in Table 3, and it is clear from Table 3 that the recovery rate of the aqueous calcium sulfate sample ranges from 95.22% to 101.60%, the average recovery rate is 99.04%, and the RSD value is 2.61%, indicating that the recovery rate is good.
Table 3, table of results of investigation of sample recovery rate of aqueous calcium sulfate of gypsum standard decoction
2.4.6 investigation of specificity (see FIG. 3 for results)
Preparing a sample solution from gypsum standard decoction (GT 161022) according to the item of 2.3; taking a proper amount of standard substances of the calcium unit element solution, and preparing Ca according to the method under the item of 2.2 2+ A control solution; then 0.1ml of 1.52% hydrochloric acid solution was taken and diluted with ultrapure water to 10ml to prepare an empty solvent. Precisely sucking the solution of the sample and Ca 2+ The control solution and the blank solvent were each 5. Mu.l, and the mixture was injected into an ion chromatograph, and analyzed under the chromatographic conditions under item "2.1".
The results are shown in Table 4 and FIG. 3, and the results show that the sample chromatogram has the same chromatographic peak at the retention time corresponding to the control chromatogram, and the blank solvent has the same retention time as the control chromatogram 2+ The chromatographic peak of the reference substance is interfered because certain metal ions exist in the aqueous solution, but Ca in the blank solvent 2+ The response value is far smaller than Ca in the sample of the test sample 2+ Response value, ca of blank solvent 2+ The peak area is only Ca of the sample solution 2+ Peak area 2.20%, indicating solvent vs. Ca 2+ The interference of the content measurement is negligible, and in conclusion, the method has better specificity.
TABLE 4 chromatographic peak separation parameter Table
2.5 results of content determination
Taking gypsum standard decoction sample, preparing sample solution according to the term "2.3", and measuring and analyzing according to the chromatographic condition under the term "2.1" to determine Ca of 23 batches of gypsum standard decoction 2+ The content is as follows.
The results are shown in Table 5, and the results show that Ca in different batches of gypsum standard decoction 2+ The content difference is small, the average value is 232.60mg/g, and the RSD value is 3.31%.
TABLE 5 Gypsum Standard decoction Ca 2+ Content measurement results
Example 2 sulfate ion content determination
1 instrument and reagent
Instrument: ion chromatograph (Dionex ICS-6000, siemens technologies Co., ltd.); cation suppressor (CSRS 300 4mm, siemens technologies Co., ltd.); ionPac AG14 guard column
(4X 50mm,9 μm); ionPac AS14 analytical column (4X 250mm,9 μm); one ten-thousandth analytical balance (ME 204E, mertrel-tolidox); ultrapure water systems (Milli-Q Direct, merck Co., ltd.).
Reagent: hydrochloric acid (guangzhou chemical reagent plant, top grade purity); anhydrous sodium carbonate (ala Ding Shiji (Shanghai) limited, top purity); sodium bicarbonate (ala Ding Shiji (Shanghai), top purity); the water was ultrapure water (laboratory homemade).
Reagent: sulfate solution standard substance (Beijing northern Weijimetric technical institute, concentration: 1000. Mu.g/mL, lot number: BWZ 6783-2016); calcium sulfate dihydrate control (lot number: 202004171; source: beijing century Orchidaceae biotechnology Co., ltd.; content: 99.5%); the lot number information of 23 batches of gypsum medicinal materials and standard decoction is shown in Table 1.
2. Method and results
2.1 Chromatographic conditions
IonPac AG14 (4X 50mm,9 μm) guard column, ionPac AS14 (4X 250mm,9 μm) analytical column, ASRS 4mm inhibitor; eluent Na 2 CO 3 /NaHCO 3 Is (4.5 mmol/L)/(1.4 mmol/L); the flow rate is 1.2ml per minute; the column temperature is 30 ℃; the temperature of the detection tank is 35 ℃; the suppression current was 47mA; the detector sensitivity was 5 mus per cm; the sample volume was 5. Mu.l.
2.2 preparation of control solution
Taking a proper amount of sulfate solution standard substance, precisely weighing, placing into a 30mL plastic vial, adding ultrapure water to prepare each 1mL SO-containing solution 4 2- 13 μg of solution.
2.3 preparation of sample solutions
Taking about 0.1g of gypsum standard decoction, precisely weighing, placing into a 30ml plastic bottle, precisely adding 30ml of 1.52% hydrochloric acid, fully shaking to dissolve, shaking uniformly, precisely sucking 0.1ml of the solution, adding ultrapure water to dilute to 10ml, shaking uniformly, filtering, and taking filtrate to obtain the plaster.
2.4 examination of sulfate ion content determination methodology
2.4.1 linear relationship investigation
3.4622g of sulfate ion solution standard substance is precisely weighed, placed in a 30ml plastic bottle, 20ml of ultrapure water is added, precisely weighed and shaken uniformly, and then the sulfate ion reference stock solution is obtained.
Precisely weighing 0.1g,0.5g,1g,2g and 5g of sulfate ion reference stock solution, respectively placing into 30ml plastic bottles, adding 10ml of ultrapure water, weighing, shaking uniformly, and preparing reference application solution containing 1.874 mug, 9.248 mug, 18.235 mug, 36.134 mug and 89.992 mug in each 1 ml.
And respectively precisely sucking the reference substance application liquid and the reference substance stock liquid, sequentially injecting 5 μl according to the chromatographic conditions under the item "2.1", and recording the chromatographic peak area.
The standard curve is drawn with the peak area as ordinate (y) and the reference substance concentration as abscissa (x), and the result is shown in fig. 2. The results show that the linear regression equation for sulfate ions is: y=0.0254 x-0.052, and the correlation coefficient r=0.9993, shows that the concentration has a good linear relationship with the peak area in the range of 1.874 μg/ml to 180.129 μg/ml.
2.4.2 precision test
Preparing sample solution by precisely absorbing Gypsum standard decoction (GT 1903178) according to the method under the term "2.3", repeatedly sampling for 6 times according to the chromatographic condition under the term "2.1", and recording SO 4 2- Peak area, RSD value of peak area was calculated.
The results show that the same sample solution is continuously injected into 6 needles, SO 4 2- The peak area RSD value is 0.33% and less than 3.0%, which indicates that the instrument precision is good.
2.4.3 stability test
Preparing sample solution by precisely absorbing Gypsum standard decoction (GT 2005079) according to the method under the term "2.3", respectively sampling at 0,2,4,6,8, 10, 12 hr according to the chromatographic conditions under the term "2.1", and recording SO 4 2- Peak area, RSD value of peak area was calculated.
The results show that the sample solution is respectively injected at 7 time points to obtain SO 4 2- The RSD value of the peak area was 0.78%, indicating that the test solution had good stability over 12 hours.
2.4.4 repeatability test
About 0.1g of the same batch of gypsum standard decoction (GT 2005079) is taken, precisely weighed, 6 parts are weighed in parallel, and 6 parts of sample solution are prepared according to the sample solution preparation method determined under the item "2.3". Calculating SO according to the chromatographic condition under the item "2.1 4 2- Content and RSD value thereof.
The results are shown in Table 6, which shows that the same batch of samples was repeatedly assayed 6 times, SO 4 2- The RSD value of the content was 0.41% and less than 1.5%, indicating good reproducibility of the analysis method.
TABLE 6 Standard decoction of Gypsum Fibrosum SO 4 2- Repeatability investigation result table
2.4.5 sample recovery rate investigation
Respectively precisely weighing 25mg, 50mg and 75mg of calcium sulfate dihydrate reference substances (batch number: 202004171 source: beijing century Orchidaceae biotechnology Co., ltd.; content: 99.5%) and placing into 30ml plastic measuring bottles, wherein each group is divided into 3 parts in parallel and 9 parts in total;
grinding appropriate amount of Gypsum Fibrosum standard decoction (GT 2005079), respectively adding about 0.05g into the above 9 plastic bottles, precisely weighing, precisely adding 30ml of 1.52% hydrochloric acid, weighing, shaking sufficiently to dissolve, shaking uniformly, precisely sucking 0.1ml of the above solution, diluting to 10ml with ultrapure water, shaking uniformly, filtering, and collecting the subsequent filtrate;
measuring according to the chromatographic condition under the item "2.1", and measuring SO in the test sample solution 4 2- The content is converted into the content of the hydrous calcium sulfate, and the sample adding recovery rate is calculated.
The results are shown in Table 7, and the recovery rate of the aqueous calcium sulfate sample ranges from 97.18% to 101.70%, the average recovery rate is 100.36%, and the RSD value is 1.52%, indicating good recovery rate.
Table 7, table of results of investigation of sample recovery rate of aqueous calcium sulfate of gypsum standard decoction
2.4.6 investigation of specificity (see FIG. 4 for results)
Preparing a sample solution from gypsum standard decoction (GT 1903178) according to the method of '2.3'; taking a proper amount of standard substances of the calcium unit element solution, and preparing SO according to the method under the item of 2.2 4 2- A control solution; then 0.1ml of 1.52% hydrochloric acid solution was taken and diluted with ultrapure water to 10ml to prepare an empty solvent. Precisely sucking the solution of the sample and SO 4 2- The control solution, the blank solvent and ultrapure water were each 5. Mu.l, and the mixture was injected into an ion chromatograph, and analyzed under the chromatographic conditions under the "2.1" item.
The results are shown in Table 8 and FIG. 4, and the results show that the sample chromatogram has the same chromatographic peak at the retention time corresponding to the reference chromatogram, and the blank solvent and the ultrapure water are subjected to SO 4 2- The chromatographic peak of the reference substance has no interference, which proves that the method has better specificity.
TABLE 8 chromatographic peak separation parameter Table
2.5 results of content determination
Taking gypsum standard decoction sample, preparing sample solution according to the term "2.3", performing measurement and analysis according to the chromatographic condition under the term "2.1", and measuring SO of 23 batches of gypsum standard decoction 4 2- The content is as follows.
The results are shown inTable 9, results show that SO in different batches of gypsum standard decoction 4 2- The content difference is not large, the average value is 556.97mg/g, and the RSD value is 1.42%.
Table 9, standard decoction of Gypsum, SO 4 2- Content measurement results
Example 3
This example is a modification of example 2, and the main modification with respect to example 2 is that "preparation of a sample solution of 2.3", specifically, the preparation of a sample solution of this example includes the steps of:
taking about 0.1g of gypsum standard decoction, precisely weighing, placing into a 30ml plastic bottle, precisely adding 25ml of 1.35% hydrochloric acid, fully shaking to dissolve, shaking uniformly, precisely sucking 0.1ml of the solution, adding ultrapure water to dilute to 10ml, shaking uniformly, filtering, and taking filtrate to obtain the plaster.
Results: according to the preparation method of the sample solution, 25ml of 1.35% hydrochloric acid solution is used for extracting Ca in gypsum standard decoction 2+ 、SO 4 2- And measuring the content of the two to obtain Ca 2+ The content of SO is 232.54mg/g 4 2- The content of (C) is 549.32mg/g. See fig. 5.
This example also tested the extraction of Ca from a standard decoction of gypsum with 1.52% hydrochloric acid solution 2+ 、SO 4 2- The content of the two is measured to be 232.95mg/g and 552.53mg/g respectively.
Ca in gypsum measured after two methods of extraction 2+ 、SO 4 2- RSD values of 0.74% and 1.49% respectively, indicating that 1.35% hydrochloric acid solution can achieve the extraction effect of 1.52% hydrochloric acid solution.
Example 4
This example is a modification of example 2, and the main modification with respect to example 2 is that "preparation of a sample solution of 2.3", specifically, the preparation of a sample solution of this example includes the steps of:
taking about 0.1g of gypsum standard decoction, precisely weighing, placing into a 30ml plastic bottle, precisely adding 30ml of 1.65% hydrochloric acid, fully shaking to dissolve, shaking uniformly, precisely sucking 0.1ml of the solution, adding ultrapure water to dilute to 10ml, shaking uniformly, filtering, and taking filtrate to obtain the plaster.
Results: according to the preparation method of the sample, 30ml of 1.65% hydrochloric acid solution is used for extracting Ca in gypsum standard decoction 2+ 、SO 4 2- And measuring the content of the two to obtain Ca 2+ The content of SO is 232.26mg/g 4 2- The content of (C) is 558.48mg/g. See fig. 6.
This example also tested the extraction of Ca from a standard decoction of gypsum with 1.52% hydrochloric acid solution 2+ 、SO 4 2- The content of the two is measured to be 232.95mg/g and 552.53mg/g respectively.
Ca in gypsum measured after two methods of extraction 2+ 、SO 4 2- RSD values of 1.23% and 1.05% respectively, indicating that 1.65% hydrochloric acid solution can achieve the extraction effect of 1.52% hydrochloric acid solution.
Example 5
This example is a modification of example 2, and the main modification with respect to example 2 is that "preparation of a sample solution of 2.3", specifically, the preparation of a sample solution of this example includes the steps of:
taking about 0.1g of gypsum-containing compound decoction (odontalgia anti-inflammatory granule), precisely weighing, placing into a 30ml plastic bottle, precisely adding 1.52% hydrochloric acid 30ml, shaking sufficiently to dissolve, shaking uniformly, precisely sucking 0.1ml of the above solution, diluting to 10ml with ultrapure water, shaking uniformly, filtering, and collecting filtrate.
Results: the method of the embodiment is used for treating Ca in gypsum-containing compound decoction (the toothache anti-inflammatory granule) 2+ 、SO 4 2- The content of two ions can be accurately measured by measuring. See fig. 7.
Comparative example 1
The present comparative example is a comparative example of example 2, and the main difference with respect to example 2 is that "preparation of a sample solution of 2.3", specifically, the preparation of a sample solution of the present comparative example includes the steps of:
taking about 0.1g of gypsum standard decoction, precisely weighing, placing into a 30ml plastic bottle, precisely adding 30ml of water, fully shaking to dissolve, shaking uniformly, precisely sucking 0.1ml of the solution, adding ultrapure water to dilute to 10ml, shaking uniformly, filtering, and taking filtrate to obtain the plaster.
Results: according to the preparation method of the sample solution, 30ml of water is used for extracting Ca in the gypsum standard decoction 2+ 、SO 4 2- And measuring the content of the two to obtain Ca 2+ The content of SO is 169.62mg/g 4 2- The content of (2) is 432.69mg/g; extracting Ca in gypsum standard decoction with 1.52% hydrochloric acid solution 2+ 、SO 4 2- The content of the two is measured to be 232.95mg/g and 552.53mg/g respectively. Ca in gypsum measured after two methods of extraction 2+ 、SO 4 2- The RSD values of (2) are 16.84% and 13.86%, respectively, and the content difference is large, which indicates that the water can not reach the extraction effect of 1.52% hydrochloric acid solution, and the addition of hydrochloric acid into the pretreatment reagent proves that the extraction effect of gypsum standard decoction can be improved. See fig. 8.
Comparative example 2
The present comparative example is a comparative example of example 2, and the main difference with respect to example 2 is that "preparation of a sample solution of 2.3", specifically, the preparation of a sample solution of the present comparative example includes the steps of:
taking about 0.1g of gypsum standard decoction, precisely weighing, placing into a 30ml plastic bottle, precisely adding 20ml of hydrochloric acid solution and methane sulfonic acid solution with the same concentration respectively, shaking sufficiently to dissolve, shaking uniformly, filtering, and collecting subsequent filtrate.
Results: according to the preparation method of the sample solution, the Ca in the gypsum standard decoction is extracted by hydrochloric acid solution 2+ 、SO 4 2- And measuring the content of the two to obtain Ca 2+ The content of SO is 240.42mg/g 4 2- The content of (2) is 595.59mg/g; extracting Ca from gypsum standard decoction with methanesulfonic acid solution 2+ 、SO 4 2- The content of the two is measured to be 231.07mg/g and 540.70mg/g respectively. Two methodsCa in gypsum measured after extraction 2+ 、SO 4 2- The content of the hydrochloric acid solution is more than that of the methylsulfonic acid solution, which shows that the hydrochloric acid solution has better extraction effect on the gypsum standard decoction.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (7)
1. The method for measuring the gypsum content in the traditional Chinese medicine decoction is characterized by comprising the following steps of:
preparing a reference substance solution and a sample solution respectively, and detecting the reference substance solution and the sample solution by adopting an ion chromatography;
the reference solution comprises Ca-containing 2+ Reference solution of (C) and SO-containing solution 4 2- Is a reference solution;
the step of preparing the sample solution comprises extracting Ca in the Chinese medicinal decoction to be tested with hydrochloric acid 2+ And SO 4 2- ；
The mass content of hydrogen chloride in the hydrochloric acid is 1.35-1.65%;
the dosage of the hydrochloric acid corresponding to each 1g of the traditional Chinese medicine decoction to be detected is 250 mL-350 mL;
the step of preparing the test solution includes: mixing the hydrochloric acid and the Chinese medicinal decoction to be tested, adding water into 0.1mL of the obtained mixture to a volume of 10mL, and filtering to obtain filtrate;
the traditional Chinese medicine decoction to be tested is a compound decoction containing gypsum, and the compound decoction containing gypsum is a odontalgia anti-inflammatory granule;
in the detection of Ca 2+ In the process of (2), the detected conditions include:
protective column: ionPac CG12A, 4X 50mm,8 μm;
analytical column: ionPac CS12A, 4X 250mm,8 μm;
a suppressor: CSRS 4mm;
eluent: methane sulfonic acid solution with the concentration of 15 mmol/L-25 mmol/L;
flow rate: 0.5-0.9 mL/min;
column temperature: 25-35 ℃;
detecting the temperature of the cell: 30-40 ℃;
suppression current: 45 mA-49 mA;
in the detection of SO 4 2- In the process of (2), the detected conditions include:
protective column: ionPac AG14, 4X 50mm,9 μm;
analytical column: ionPac AS14, 4X 250mm,9 μm;
a suppressor: ASRS 4mm;
eluent: na (Na) 2 CO 3 The concentration is 4 mmol/L-5 mmol/L, naHCO 3 1 mmol/L-1.8 mmol/L aqueous solution;
flow rate: 1 mL/min-1.5 mL/min;
column temperature: 25-35 ℃;
detecting the temperature of the cell: 30-40 ℃;
suppression current: 25 mA-35 mA.
2. The method for determining the gypsum content in a Chinese medicinal decoction according to claim 1, wherein the method comprises the steps of 2+ In (2), the detected conditions further include:
sensitivity of the detector: 4.5 mu S/cm-5.5 mu S/cm;
sample injection volume: 4.5 mu L to 5.5 mu L.
3. According toThe method for determining the gypsum content in the Chinese medicinal decoction according to claim 1, wherein in the detection of SO 4 2- In (2), the detected conditions further include:
sensitivity of the detector: 4.5 mu S/cm-5.5 mu S/cm;
sample injection volume: 4.5 mu L to 5.5 mu L.
4. The method for determining the gypsum content in a Chinese medicinal decoction according to any one of claims 1 to 3, wherein each 1mL of the Ca-containing powder 2+ In the reference solution of (2), ca 2+ The mass of (C) is 8-12 mug.
5. The method for determining the gypsum content in a Chinese medicinal decoction according to any one of claims 1 to 3, wherein the Ca-containing extract 2+ The preparation steps of the reference substance solution comprise: mixing standard substances of the calcium unit element solution and water.
6. The method for determining the gypsum content in a Chinese medicinal decoction according to any one of claims 1 to 3, wherein each 1mL of the SO-containing extract 4 2- In the reference solution of (2), SO 4 2- The mass of (C) is 10-15 mug.
7. The method for determining the gypsum content in a Chinese medicinal decoction according to any one of claims 1 to 3, wherein the SO-containing extract 4 2- The preparation steps of the reference substance solution comprise: mixing sulfate solution standard substance and water.
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