CN113624881A - Method for simultaneously detecting contents of six components in Sanwu capsule - Google Patents
Method for simultaneously detecting contents of six components in Sanwu capsule Download PDFInfo
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- CN113624881A CN113624881A CN202110933602.2A CN202110933602A CN113624881A CN 113624881 A CN113624881 A CN 113624881A CN 202110933602 A CN202110933602 A CN 202110933602A CN 113624881 A CN113624881 A CN 113624881A
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- 239000002775 capsule Substances 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 33
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 70
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 60
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 34
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 18
- 238000000926 separation method Methods 0.000 claims abstract description 16
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- 238000000605 extraction Methods 0.000 claims abstract description 10
- 230000002378 acidificating effect Effects 0.000 claims abstract description 9
- 239000003463 adsorbent Substances 0.000 claims abstract description 9
- 238000000746 purification Methods 0.000 claims abstract description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 8
- 238000009736 wetting Methods 0.000 claims abstract description 7
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- 238000001704 evaporation Methods 0.000 claims abstract description 5
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- 239000006228 supernatant Substances 0.000 claims abstract description 5
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- 239000000243 solution Substances 0.000 claims description 29
- 238000001514 detection method Methods 0.000 claims description 27
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 26
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 22
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 claims description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 16
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 16
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
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- 239000000412 dendrimer Substances 0.000 claims description 8
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- 239000012043 crude product Substances 0.000 claims description 6
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 6
- 229920001721 polyimide Polymers 0.000 claims description 6
- MBYLVOKEDDQJDY-UHFFFAOYSA-N tris(2-aminoethyl)amine Chemical compound NCCN(CCN)CCN MBYLVOKEDDQJDY-UHFFFAOYSA-N 0.000 claims description 6
- 239000004952 Polyamide Substances 0.000 claims description 5
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(II) nitrate Inorganic materials [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 5
- 229920002647 polyamide Polymers 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 3
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- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims description 2
- 229920000768 polyamine Polymers 0.000 claims description 2
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- 239000000523 sample Substances 0.000 description 21
- DHVYLCVNTWPXSI-UHFFFAOYSA-N [11-ethyl-5,8,14-trihydroxy-6,16,18-trimethoxy-13-(methoxymethyl)-11-azahexacyclo[7.7.2.12,5.01,10.03,8.013,17]nonadecan-4-yl] 4-methoxybenzoate Chemical compound CCN1CC(C(CC2OC)O)(COC)C3C(OC)C(C(C45)(O)CC6OC)C1C32C4CC6(O)C5OC(=O)C1=CC=C(OC)C=C1 DHVYLCVNTWPXSI-UHFFFAOYSA-N 0.000 description 17
- 239000012071 phase Substances 0.000 description 12
- PKUBGLYEOAJPEG-UHFFFAOYSA-N physcion Natural products C1=C(C)C=C2C(=O)C3=CC(C)=CC(O)=C3C(=O)C2=C1O PKUBGLYEOAJPEG-UHFFFAOYSA-N 0.000 description 10
- 239000000126 substance Substances 0.000 description 10
- DHJXZSFKLJCHLH-BMTFSNIDSA-N 369u7a6hxd Chemical compound O([C@H]1[C@]2(O)C[C@H]3[C@@]45[C@H]6[C@@H]([C@@]([C@H]31)(O)[C@@H](O)[C@@H]2OC)[C@H](OC)[C@@H]4[C@]([C@@H](C[C@@H]5OC)O)(COC)CN6CC)C(=O)C1=CC=CC=C1 DHJXZSFKLJCHLH-BMTFSNIDSA-N 0.000 description 9
- VWDXGKUTGQJJHJ-UHFFFAOYSA-N Catenarin Natural products C1=C(O)C=C2C(=O)C3=C(O)C(C)=CC(O)=C3C(=O)C2=C1O VWDXGKUTGQJJHJ-UHFFFAOYSA-N 0.000 description 9
- 239000010282 Emodin Substances 0.000 description 9
- RBLJKYCRSCQLRP-UHFFFAOYSA-N Emodin-dianthron Natural products O=C1C2=CC(C)=CC(O)=C2C(=O)C2=C1CC(=O)C=C2O RBLJKYCRSCQLRP-UHFFFAOYSA-N 0.000 description 9
- YOOXNSPYGCZLAX-UHFFFAOYSA-N Helminthosporin Natural products C1=CC(O)=C2C(=O)C3=CC(C)=CC(O)=C3C(=O)C2=C1O YOOXNSPYGCZLAX-UHFFFAOYSA-N 0.000 description 9
- NTGIIKCGBNGQAR-UHFFFAOYSA-N Rheoemodin Natural products C1=C(O)C=C2C(=O)C3=CC(O)=CC(O)=C3C(=O)C2=C1O NTGIIKCGBNGQAR-UHFFFAOYSA-N 0.000 description 9
- PULWZCUZNRVAHT-LOCDBSKESA-N benzoylmesaconine Chemical compound O([C@H]1[C@]2(O)C[C@H]3[C@]45[C@@H]6[C@@H](OC)[C@H]([C@@]([C@H]31)(O)[C@@H](O)[C@@H]2OC)[C@H]4N(C)C[C@@]6([C@@H](C[C@@H]5OC)O)COC)C(=O)C1=CC=CC=C1 PULWZCUZNRVAHT-LOCDBSKESA-N 0.000 description 9
- PULWZCUZNRVAHT-UHFFFAOYSA-N benzoylmesaconine Natural products COC1CC(O)C2(COC)CN(C)C3C(C(C45)(O)C(O)C6OC)C(OC)C2C31C4CC6(O)C5OC(=O)C1=CC=CC=C1 PULWZCUZNRVAHT-UHFFFAOYSA-N 0.000 description 9
- RHMXXJGYXNZAPX-UHFFFAOYSA-N emodin Chemical compound C1=C(O)C=C2C(=O)C3=CC(C)=CC(O)=C3C(=O)C2=C1O RHMXXJGYXNZAPX-UHFFFAOYSA-N 0.000 description 9
- VASFLQKDXBAWEL-UHFFFAOYSA-N emodin Natural products OC1=C(OC2=C(C=CC(=C2C1=O)O)O)C1=CC=C(C=C1)O VASFLQKDXBAWEL-UHFFFAOYSA-N 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- YRECILNLFWZVRM-XTNYDWJGSA-N bulleyaconitine a Chemical compound O=C([C@H]1[C@]2(O)C[C@H]3[C@]45[C@H](OC)CC[C@@]6(COC)CN([C@@H]5[C@H]([C@H](OC)[C@H]64)[C@](C[C@@H]2OC)(OC(C)=O)[C@H]31)CC)C1=CC=C(OC)C=C1 YRECILNLFWZVRM-XTNYDWJGSA-N 0.000 description 6
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- 229930013930 alkaloid Natural products 0.000 description 4
- DHJXZSFKLJCHLH-UHFFFAOYSA-N benzoylaconine Natural products CCN1CC(C(CC2OC)O)(COC)C3C(OC)C(C(C45)(O)C(O)C6OC)C1C32C4CC6(O)C5OC(=O)C1=CC=CC=C1 DHJXZSFKLJCHLH-UHFFFAOYSA-N 0.000 description 4
- -1 diester alkaloid Chemical class 0.000 description 4
- 238000005259 measurement Methods 0.000 description 3
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- 238000012360 testing method Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 241000227129 Aconitum Species 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 241000717739 Boswellia sacra Species 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000004863 Frankincense Substances 0.000 description 2
- 235000018167 Reynoutria japonica Nutrition 0.000 description 2
- 240000001341 Reynoutria japonica Species 0.000 description 2
- MDFCJNFOINXVSU-ZEDVMUKVSA-N benzoylhypaconine Chemical compound O([C@H]1[C@]2(O)C[C@H]3[C@]45[C@@H](OC)CC[C@@]6([C@H]4[C@@H](OC)[C@H]([C@](O)([C@H]31)[C@@H](O)[C@@H]2OC)[C@H]5N(C)C6)COC)C(=O)C1=CC=CC=C1 MDFCJNFOINXVSU-ZEDVMUKVSA-N 0.000 description 2
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- FFWOKTFYGVYKIR-UHFFFAOYSA-N physcion Chemical compound C1=C(C)C=C2C(=O)C3=CC(OC)=CC(O)=C3C(=O)C2=C1O FFWOKTFYGVYKIR-UHFFFAOYSA-N 0.000 description 2
- 239000012521 purified sample Substances 0.000 description 2
- 239000012088 reference solution Substances 0.000 description 2
- 239000007901 soft capsule Substances 0.000 description 2
- JAYVHSBYKLLDJC-DSNJPTTOSA-N (E)-2,3,5,4'-tetrahydroxystilbene-2-O-beta-D-glucoside Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=C(O)C=C(O)C=C1\C=C\C1=CC=C(O)C=C1 JAYVHSBYKLLDJC-DSNJPTTOSA-N 0.000 description 1
- 241000826247 Aconitum flavum Species 0.000 description 1
- 235000003717 Boswellia sacra Nutrition 0.000 description 1
- 235000012035 Boswellia serrata Nutrition 0.000 description 1
- 206010008190 Cerebrovascular accident Diseases 0.000 description 1
- 241001289529 Fallopia multiflora Species 0.000 description 1
- UGNZSMZSJYOGNX-UHFFFAOYSA-N Isoviocristine Natural products O=C1C=C(C)C(=O)C2=CC3=CC(OC)=CC(O)=C3C(O)=C21 UGNZSMZSJYOGNX-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 208000006011 Stroke Diseases 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- WLXGUTUUWXVZNM-UHFFFAOYSA-N anthraglycoside A Natural products C1=C(C)C=C2C(=O)C3=CC(OC)=CC(O)=C3C(=O)C2=C1OC1OC(CO)C(O)C(O)C1O WLXGUTUUWXVZNM-UHFFFAOYSA-N 0.000 description 1
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- 229910021641 deionized water Inorganic materials 0.000 description 1
- 150000005690 diesters Chemical class 0.000 description 1
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- 229940044631 ferric chloride hexahydrate Drugs 0.000 description 1
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- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
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- 229920001155 polypropylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
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- 239000001632 sodium acetate Substances 0.000 description 1
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Classifications
-
- 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
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for simultaneously detecting the content of six components in a Sanwu capsule, which comprises the steps of adding petroleum ether into Sanwu capsule powder for ultrasonic treatment, standing, volatilizing the petroleum ether, adding ammonia water for wetting, adding ether or chloroform for ultrasonic extraction, complementing weight loss in the extraction process with ether or chloroform, carrying out solid-liquid separation, adding ether or chloroform into residues for extraction, complementing weight loss with ether or chloroform, carrying out solid-liquid separation, combining extracting solutions, evaporating the extracting solutions to dryness, and redissolving the residues with acidic methanol; adding a magnetic graphene-based adsorbent into the redissolved solution for purification, centrifuging, filtering the supernatant with a membrane, and detecting by using a high performance liquid chromatograph; the method can simultaneously detect the contents of 6 index components in the Sanwu capsule, the separation effect of the chromatographic conditions is good, the reproducibility is good, and compared with the existing quality control technology of the Sanwu capsule, the method can comprehensively represent the effective components in the Sanwu capsule, and can better ensure the curative effect and the safety of the Sanwu capsule.
Description
Technical Field
The invention belongs to the technical field of traditional Chinese medicine quality analysis and detection, and relates to a method for simultaneously determining six index components in a Sanwu capsule.
Background
CN102507781A discloses a quality control method for a medicine for treating rheumatism and apoplexy, wherein the trade name of the Chinese patent medicine is Sanwu capsule, wherein high performance liquid chromatography is adopted to measure the content of the index component 2, 3, 5, 4' -tetrahydroxy stilbene-2-O-beta-D-glucoside in fleece-flower root and diester alkaloids in aconitum flavum and monkshood, thin layer identification is carried out to frankincense medicinal material and fleece-flower root medicinal material, volatile alkaline substances are detected, and the product quality of the Sanwu capsule is controlled by two modes of qualitative detection and quantitative detection.
However, the high performance liquid chromatography only performs content measurement on index components of a single medicinal material in the Sanwu capsule, and the thin-layer identification can only be used for qualitative determination and cannot be used for quantitative determination. The diester alkaloid in the Sanwu capsule is a main component source of toxicity, but the prescription process of the Sanwu capsule determines that the content of the diester alkaloid is lower and is often lower than the detection limit of high performance liquid chromatography, so that the material basis of the Sanwu capsule cannot be comprehensively reflected. Only the content of the index components of a single medicinal material in the Sanwu capsule is measured, the operation is complicated, the accuracy is not high due to the fact that the content is lower than the detection limit, the curative effect of the Sanwu capsule cannot be evaluated objectively, and certain potential safety hazard is brought to the administration of the Sanwu capsule. Therefore, there is a need to develop a quality analysis method for more comprehensively and simultaneously measuring aconite-type alkaloids in the Sanwu capsule and the emodin as index components in the Polygonum multiflorum so as to establish a more complete and simple-to-operate quality control system which is more relevant to clinical curative effect.
Disclosure of Invention
The invention provides a method for simultaneously detecting the content of six components in a Sanwu capsule, aiming at controlling the product quality of the Sanwu capsule more efficiently and accurately, wherein the six components are benzoylmesaconine, benzoylaconitine, benzoylmesaconine, 8-deacetylyunaconitine, bulleyaconitine A and emodin;
the Sanwu capsule is prepared from radix Aconiti Kusnezoffii, radix Aconiti, Polygoni Multiflori radix, rhizoma Typhonii, radix Aconiti lateralis Preparata, and Olibanum.
The method for simultaneously detecting the contents of six components in the Sanwu capsule comprises the steps of adding petroleum ether into 1-2g of Sanwu capsule powder sieved by a 50-mesh sieve, performing ultrasonic treatment at 20-30 ℃ for 4-6min, standing, volatilizing the petroleum ether at the temperature of below 40 ℃, adding ammonia water for wetting, adding ether or chloroform for ultrasonic extraction for 60min after wetting, performing solid-liquid separation, adding ether or chloroform into residues for extraction once again, combining the extracting solutions, evaporating the extracting solution to dryness, and re-dissolving the residues with 1mL of acidic methanol; adding a magnetic graphene-based adsorbent into the redissolved solution for purification, centrifuging, and detecting the supernatant by a high performance liquid chromatograph after passing through a 0.45-micrometer filter membrane.
The acidic methanol is prepared by adding 1-2mL of hydrochloric acid to every 100mL of methanol.
The preparation method of the magnetic graphene-based adsorbent comprises the following steps:
(1) adding methyl acrylate into a methanol solution of tris (2-aminoethyl) amine, reacting for 20-24 h at 30-35 ℃, then adding triethylene diamine, continuing to react for 20-24 h at 30-35 ℃, and performing rotary evaporation to obtain a crude product; dissolving the crude product in a methanol solution, adding methyl acrylate, reacting at 30-35 ℃ for 20-24 h, adding triethylene diamine, and continuing to react at 30-35 ℃ for 20-24 h to prepare the polyamide dendrimer; wherein the mass ratio of the tri (2-aminoethyl) amine to the methyl acrylate is 0.5-1: 4-5, and the mass ratio of the triethylene diamine to the methyl acrylate is 1-2: 2-2.5;
(2) FeCl is added3·6H2O、Ni(NO3)2·6H2O, NaAc and NaOH are added into glycol in sequence for ultrasonic dissolution until the solution is transparent; then adding the polyimide dendrimer prepared in the step (1) and dissolving by ultrasonic; adding carboxylated graphene, stirring at 55-60 ℃ for 30-45 min, transferring to a high-pressure reaction kettle, reacting at 185-200 ℃ for 48h, separating the product by virtue of an external magnetic field, and washing to be neutral to obtain the magnetic graphene-based polyamide, wherein FeCl is used as a material3·6H2O、Ni(NO3)2·6H2O, NaAc and NaOH are in a mass ratio of 1-1.5: 2-3: 0.1-0.5, and the addition amount of the polyimide polyamine dendrimer is FeCl3·6H28-12% of the mass of O, and the addition amount of the carboxylated graphene is FeCl3·6H24-6% of the mass of O.
The addition amount of the magnetic graphene-based adsorbent is 10mg/mL, and the adsorbent has good reusability and mechanical stability.
The high performance liquid chromatograph is provided with an ultraviolet detector, the detection wavelength is set to be 200-300nm, and the stationary phase of the high performance liquid chromatograph is C18Chromatographic column with flowability A of 0.1-1.0% concentration diethylamine solution, phosphoric acid regulated diethylamine solution pH of 3.0-6.0 and flowability B of acetonitrile, and gradient elution at 20-35 deg.c; gradient elution time is 105min, gradient elution (0-15 min, 10% -20% B, 45-55min, 40% -70% B, 70-75 min, 70% -100% B, 85-90min, 100% -10% B, 105min, 10% B)
The invention has the beneficial effects that:
the method can simultaneously detect the contents of six substances in the Sanwu capsule, and the magnetic graphene-based adsorbent is adopted to purify the test solution, so that the interference of impurities such as grease in the test solution and the like on the detection can be effectively eliminated; the detection result has good repeatability and high accuracy, and can comprehensively reflect the material basis of the Sanwu capsule; the invention establishes a quality control system of the Sanwu capsules associated with the drug effect, and the quality of the Sanwu capsules can be effectively controlled by adopting the method.
According to the invention, the chromatographic peaks of 6 components to be detected are well separated by optimizing and screening HPLC conditions, and each substance is correspondingly high at 245nm, so that the accuracy of a detection result is improved, the quality stability of the Sanwu capsule is ensured, and the quality of the Sanwu capsule is more controllable.
Drawings
FIG. 1 is an HPLC chromatogram of a mixed control of 6 components to be tested;
FIG. 2 is an HPLC chromatogram of a sample after purification by methods 1 (b) and 2 (a) in example 1;
FIG. 3 is an HPLC plot of the sample solution after purification at 235nm (a), 255nm (b) detection wavelengths according to method 1 of example 1;
FIG. 4 is an HPLC chromatogram of mobile phases 0.5% aqueous diethylamine solution-acetonitrile (a), 0.2% aqueous diethylamine solution-acetonitrile (b), 0.2% aqueous diethylamine solution (pH 5.0 adjusted with phosphoric acid) -acetonitrile (c), respectively;
FIG. 5 is an HPLC chromatogram of gradient 1 (a), gradient 2 (b) of different gradient elution conditions in example 2;
in the figure: 1 is benzoylmesaconine, 2 is benzoylaconine, 3 is benzoylhypaconine, 4 is 8-deacetylyunaconitine, 5 is bulleyaconitine A, and 6 is emodin;
fig. 6 is an HPLC chromatogram of the pharmacopoeia method for detecting 6 components in the sanwu capsule.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the scope of the present invention, and the methods used in the examples are all conventional methods unless otherwise specified, and reagents used therein are all conventional commercially available reagents or reagents prepared by conventional methods.
Reagent testing: sanwu soft capsules (batch No. 190903, pharmaceutical Co., Ltd., Yunan Jinwu Heiyao); the control products of benzoylmesaconine (batch No. wkq20041701 mass fraction: HPLC ≥ 98%), benzoylhypaconine (wkq 20041702 mass fraction: HPLC ≥ 98%), benzoylaconine (wkq 20041505 mass fraction: HPLC ≥ 98%) were purchased from Vickers Biotech, Inc. of Sichuan province. 8-deacetylyunaconitine (batch No. Yz0201221 mass fraction: HPLC ≥ 98%), bulleyaconitine (batch No. Yz042122 mass fraction: HPLC ≥ 98%), emodin (batch No. Yz080920 mass fraction: HPLC ≥ 98%), and physcion (batch No. Yz040122 mass fraction: HPLC ≥ 98%) were purchased from Nanjing-sourced phytoscience and technology Limited.
Acetonitrile (HPLC grade, Sigma ltd), phosphoric acid (HPLC grade, shanghai alatin biochem ltd); diethyl ether, ammonia, diethylamine, ferric chloride hexahydrate (FeCl)3·6H2O), nickel nitrate hexahydrate [ Ni (NO)3)2·6H2O]Sodium hydroxide, sodium acetate, Ethylene Glycol (EG), tris (2-aminoethyl) amine, triethylenediamine and Methyl Acrylate (MA) (analytical, chengdu chemical reagents ltd), carboxylated graphene (chengdu organic chemistry ltd, chinese academy of sciences); the water is ultrapure water;
the instrument comprises the following steps: agilent 1260 type high performance liquid chromatograph; a mertler AL-104 model electronic balance (mertler-toledo instruments shanghai ltd); model KQ5200E ultrasonic cleaner (ultrasonic instruments ltd, kunshan).
Example 1: pretreatment of Sanwu capsule sample
Before HPLC content measurement, a Sanwu capsule sample to be measured is subjected to pretreatment, namely extraction, and the extraction aims are two, so that firstly, detection impurities in a Chinese patent medicine preparation are reduced, and secondly, components to be measured can be separated from the Chinese patent medicine preparation as far as possible, so that the peak area of a characteristic peak is improved, and the accuracy is improved. According to the prescription composition of the Sanwu capsule, the properties such as the solubility of the medicine are combined;
(1) the method comprises the following steps: weighing 1.5g of Sanwu capsule powder (sieved by a 50-mesh sieve), adding 5mL of petroleum ether, performing ultrasonic treatment at 25 ℃ for 5min, standing, and volatilizing the petroleum ether at the temperature below 40 ℃; adding 3mL of ammonia water for wetting; adding 20mL of diethyl ether, weighing, performing ultrasonic extraction at 25 ℃ for 60min, adding diethyl ether to make up the loss, and performing solid-liquid separation; adding ether into the residue, extracting for 60min, adding ether to complement weight loss, and performing solid-liquid separation; mixing the two diethyl ether solutions, evaporating to dryness at 32 deg.C, and dissolving the residue in 1mL of acidic methanol (1 mL of hydrochloric acid in 100mL of methanol);
the method 2 comprises the following steps: precisely weighing 1.5g of Sanwu capsule powder (sieved by a 50-mesh sieve), adding 5mL of petroleum ether, performing ultrasonic treatment at 25 ℃ for 5min, standing, volatilizing the petroleum ether at the temperature of below 40 ℃, and adding 3mL of ammonia water for wetting; adding 20mL of chloroform, weighing, performing ultrasonic treatment at 25 ℃ for 60min, and supplementing the loss with chloroform; solid-liquid separation; adding chloroform into the residue, extracting for 60min, adding chloroform to complement weight loss, performing solid-liquid separation, mixing the two chloroform solutions, evaporating at 32 deg.C, and dissolving the residue in 1mL of acidic methanol (1 mL of hydrochloric acid is added to each 100mL of methanol);
example 2: sample purification and detection
1. Preparation of magnetic graphene-based adsorbent
(1) Weighing tris (2-aminoethyl) amine (0.5 g) in a round-bottom flask, adding 100mL of methanol for dissolving, then adding Methyl Acrylate (MA) (2.4 g) in the round-bottom flask for reacting at 30 ℃ for 24h, adding 2.0g of triethylene diamine, continuing to react at 30 ℃ for 24h, and carrying out rotary evaporation on the reaction product at 30 ℃ to obtain a crude product; dissolving the crude product in a methanol solution, adding 2.4g of methyl acrylate, reacting at 30 ℃ for 24h, adding 2.0g of triethylene diamine, and continuing to react at 30 ℃ for 24h to obtain the polyamide dendrimer;
(2) into a 250mL round bottom flask was added 100mL ethylene glycol and 2.0g FeCl3·6H2O、2.0g Ni(NO3)2·6H2O, 6.0g of NaAc and 0.8g of NaOH are sequentially added into ethylene glycol, and ultrasonic dissolution is carried out until the solution is transparent; then adding 200mg of the polyimide dendrimer prepared in the step (1), and ultrasonically dissolving for 10 min; adding 100mg of carboxylated graphene into a round-bottom flask, stirring strongly at 60 ℃ for 40min, transferring the mixture into a stainless steel high-pressure reaction kettle with polytetrafluoroethylene as an inner liner, reacting at 200 ℃ for 48h, separating the synthesized amino functionalized magnetic carbon graphene from the reaction system by virtue of a magnetic field formed by a magnet, then repeatedly washing the synthesized material by deionized water and ethanol in sequence until the pH value of a washing solution is neutral, and drying to obtain the magnetic graphene-based polyimide;
2. purification
Transferring 1mL of the extracting solution prepared in the example 1 into a 2mL polypropylene centrifugal tube, adding 10mg of magnetic graphene-based polyamide, carrying out vortex oscillation for 3min, centrifuging for 5min at 4000r/min, sucking supernatant, filtering the supernatant through a 0.45-micron filter membrane, and then sampling the filtrate into a high performance liquid chromatograph for analysis;
3. liquid phase detection conditions: the instrument comprises the following steps: agilent 1260 type high performance liquid chromatograph; mobile phase: 0.2% diethylamine aqueous solution (pH 4.0 adjusted by phosphoric acid) as mobile phase A, acetonitrile as mobile phase B; gradient elution conditions: 0-15min, 10% -20% B; 45-55min, 40-70% B; 70-75 min, 70% -100% B; 85-90min, 100% -10% B; 105min, 10% B; column temperature: 30 ℃; detection wavelength: 245 nm; flow rate: 1.0 mL/min; sample introduction amount: 10 mu L of the solution;
the results are shown in fig. 2, and fig. 2b shows that the sample solution of the Sanwu capsule extracted and purified by ammonia water and diethyl ether has more peaks, can more comprehensively reflect the main components in the Sanwu capsule, and has larger peak area, better separation degree between the peaks and better peak type.
FIG. 2a shows that the sample solution of SAWU Capsule after extraction and purification with ammonia water and chloroform shows less peak, and the extraction effect of diethyl ether on benzoylmesaconine (1), benzoylaconitine (2), benzoylaconitine (3), and 8-deacetylyunaconitine (4) is much higher than that of chloroform on the above components;
the sample purified by the method 1 is analyzed at the detection wavelengths of 235nm and 255nm at the same time, the result is shown in fig. 3a and 3b, the peak responses of the bulleyaconitine A (5) and the emodin (6) at the detection wavelength of 235nm are not high at the detection wavelength of 245 nm; the responses of the peaks of benzoylmesaconine (1), benzoylaconitine (2), 8-deacetylyunaconitine (4) and emodin (6) at the detection wavelength of 255nm are not high at the detection wavelength of 245nm (fig. 2 b).
In the method 1, the purified sample is simultaneously subjected to detection and analysis under the following 3 liquid phase conditions; mobile phase: a. 0.5% diethylamine aqueous solution is mobile phase A, b.0.2% diethylamine aqueous solution is mobile phase A, c.0.2% diethylamine aqueous solution is mobile phase A (pH 5.0 adjusted by phosphoric acid), mobile phase B is acetonitrile; the results are shown in FIG. 4, where the resolution of the peaks in FIG. 4a is poor, the baseline is unstable and the peak pattern is poor, compared to FIG. 2b (0.2% diethylamine in water (phosphoric acid adjusted pH 4.0)); FIG. 4b shows an improvement in the peak profile, but the separation is still poor and the peaks are not completely separated from each other; c can separate each substance, but the peak shape of the substance has a general tailing phenomenon; in FIG. 2b, the separation between the peaks is good, the baseline is relatively smooth, and the peak pattern is relatively good.
Method 1 the purified sample was analyzed simultaneously for the following 2 gradient elution conditions, gradient 1: 0-15min, 40% -45% B; 20-43min, 50% -70% B; 53-58min, 75% -100% B; 68-72min, 100% -40% B; 87min, 40% B; gradient 2: 0-15min, 30% -35% B; 20-43min, 50% -70% B; 53-58min, 75% -100% B; 68-72min, 100% -30% B; 87min, 30% B; the results are shown in FIG. 5, where the peak time of each substance in FIG. 5a is too fast and the substances to be measured are not separated at all; in FIG. 5b, around 6min, peaks are piled up and the separation degree of the substance to be measured is not good; FIG. 2b shows complete separation between the respective substances to be tested.
4. Preparation of standard curve and regression equation
Preparing standard substance of 6 components to be tested with acidic methanol (1 mL hydrochloric acid per 100mL methanol) to obtain solution containing emodin 100 μ g/mL-190 mu g/mL of 8-deacetylyunaconitine-1105 mu g/mL bulleyaconitine A -170 mu g/mL benzoylmesaconine-195. mu.g/mL benzoylmesaconine-165 ug/mL benzoylaconitine-1Mixed reference solution of (1);
mobile phase: 0.2% diethylamine aqueous solution (pH 4.0 adjusted by phosphoric acid) as mobile phase A, acetonitrile as mobile phase B; gradient elution conditions: 0-15min, 10% -20% B; 45-55min, 40-70% B; 70-75 min, 70% -100% B; 85-90min, 100% -10% B; 105min, 10% B; column temperature: 30 ℃; detection wavelength: 245 nm; flow rate: 1.0 mL/min; sample introduction amount: 10 mu L of the solution; the results of the assay are shown in the following table and in FIG. 1; as can also be seen from fig. 1 and fig. 2, the method of the present invention can extract and enrich 6 components to be tested from the sanwu capsule;
diluting the mixed reference substance solution with acidic methanol for 2 times, 4 times, 20 times, 100 times, and 200 times to obtain series mixed reference substance solutions; precisely sucking 10 μ L of the diluted mixed reference solution, analyzing by sample injection according to the chromatographic conditions, and measuring peak area; linear regression of the mass concentration (X) with peak area (Y) is performed on the peak, and the results are shown in the following table;
example 3: repeatability verification
Taking 6 Sanwu capsule samples (batch number: 200903), 1.5g each, extracting by the method 1, purifying by the method of example 2, preparing 6 test sample solutions to be tested, performing liquid phase detection by the conditions of step 3 of example 2, introducing each sample for 2 times, measuring peak areas of 6 components in 6 samples under the detection wavelength of 245nm, then substituting into the regression equation of step 4 of example 2, calculating the content of 6 components to be tested in 6 parallel experiments, wherein the average content of 6 components to be tested in the Sanwu capsule (batch number: 200903) is as follows (in each 1.5 g): 8-deacetylyunaconitine (0.65 mg), bulleyaconitine A (0.14 mg), benzoylmesaconine (0.51 mg), benzoylmesaconine (0.63 mg), benzoylaconitine (0.19 mg), and emodin (0.02 mg); the RSD of the content of the component to be detected is calculated, the result is shown in the table, the RSD of the 6-time content measurement result is not more than 2%, and the result shows that the repeatability of the detection method is good;
example 4: sample application recovery rate test
On the basis of the known content of 6 components in the Sanwu capsule sample (batch number: 200903) measured in example 3, 6 portions of the Sanwu capsule (batch number: 200903) are precisely weighed, 1.5g of each portion is respectively placed in a sample bottle with a plug, after degreasing with petroleum ether and wetting with ammonia water are carried out by adopting the steps in the method 1, 20mL of ether solution containing 8-deacetylyunaconitine 0.65mg, bulleyaconitine A0.14 mg, benzoylmesaconine 0.51mg, benzoylaconine 0.63mg, benzoylaconine 0.19mg and emodin 0.02mg are respectively added into each portion of the sample, and ultrasonic extraction is carried out for 60 min; the subsequent operations are purified by the same method 1 and the same example 2, the liquid phase detection conditions are the same as the step 3 of the example 2, the sample injection analysis is carried out, the content of 6 components of 6 samples is calculated, the standard addition recovery rate is calculated and is expressed by percentage, the average recovery rate result is shown in the following table, and the result shows that the method has better accuracy and precision;
example 5: determination of 6 components of Sanwu capsule pills in different production batches
(1) The extraction method of 5 batches of Sanwu soft capsules with different production batches is the same as the method 1 of the embodiment 1, and the purification method is the same as the steps 1-2 of the embodiment 2;
(2) injecting 10 mu L of sample solution to be detected of 5 batches into a liquid chromatograph respectively, wherein the liquid phase detection conditions are the same as the step 3 in the embodiment 2;
recording peak areas of 6 components to be detected in the Sanwu capsule, calculating the concentration of the components through the standard curve of the step 4 in the example 2, and calculating the content of the 6 components to be detected in the Sanwu capsule through the following formula, wherein the result is shown in the following table;
Mi=Csample (A) 
1000/WSample (A)
MiIs the mass concentration (μ g/g) of the component to be measured
CSample (A)To calculate the sample concentration (mg/mL)
WSample (A)Weighing the sample (g)
The content (mu g/g) of six ingredients in 5 batches of the Sanwu capsule sample
Comparative example: the index components in the Sanwu capsule are determined by referring to a preparation method of a reference substance, a preparation method of a test solution, chromatographic conditions and a system applicability test method in the content determination of monkshood in the 200 th page of the '2020 edition pharmacopoeia'; the result is shown in fig. 6, the chromatographic peak separation degrees of 6 components to be detected in the Sanwu capsule are poor, and the influence of the miscellaneous peak on the result is large;
the results show that the method can simultaneously detect the contents of 6 index components in the Sanwu capsule, has good repeatability and high accuracy, can comprehensively represent the effective components in the Sanwu capsule, and can better ensure the curative effect and the safety of the Sanwu capsule.
Claims (4)
1. A method for simultaneously detecting the contents of six components in a Sanwu capsule is characterized in that: adding petroleum ether into 1-2g of Sanwu capsule powder sieved by a 50-mesh sieve, performing ultrasonic treatment at 20-30 ℃ for 4-6min, standing, volatilizing the petroleum ether at the temperature below 40 ℃, adding ammonia water for wetting, adding diethyl ether or chloroform for ultrasonic extraction for 60min, supplementing the weight loss in the extraction process with diethyl ether or chloroform, performing solid-liquid separation, adding diethyl ether or chloroform into the residue for extraction for 60min, supplementing the weight loss with diethyl ether or chloroform for solid-liquid separation, combining the extracting solutions, evaporating the extracting solution to dryness, and re-dissolving the residue with 1mL of acidic methanol; adding a magnetic graphene-based adsorbent into the redissolved solution for purification, centrifuging, and detecting the supernatant by a high performance liquid chromatograph after passing through a 0.45-micrometer filter membrane.
2. The method for simultaneously detecting the contents of six ingredients in a Sanwu capsule as claimed in claim 1, wherein the acidic methanol is prepared by adding 1-2mL of hydrochloric acid per 100mL of methanol.
3. The method for simultaneously detecting the contents of six components in a Sanwu capsule according to claim 1, wherein the preparation method of the magnetic graphene-based adsorbent comprises the following steps:
(1) adding methyl acrylate into a methanol solution of tris (2-aminoethyl) amine, reacting for 20-24 h at 30-35 ℃, then adding triethylene diamine, continuing to react for 20-24 h at 30-35 ℃, and performing rotary evaporation on a reaction product to obtain a crude product; dissolving the crude product in a methanol solution, adding methyl acrylate again, reacting at 30-35 ℃ for 20-24 h, adding triethylene diamine, and continuing to react at 30-35 ℃ for 20-24 h to prepare the polyamide dendrimer; wherein the mass ratio of the tri (2-aminoethyl) amine to the methyl acrylate is 0.5-1: 4-5, and the mass ratio of the triethylene diamine to the methyl acrylate is 1-2: 2-2.5;
(2) FeCl is added3·6H2O、Ni(NO3)2·6H2O, NaAc and NaOH are added into glycol in sequence for ultrasonic dissolution until the solution is transparent; then adding the polyimide dendrimer prepared in the step (1) and dissolving by ultrasonic; adding carboxylated graphene, stirring at 55-60 ℃ for 30-45 min, transferring to a high-pressure reaction kettle, reacting at 185-200 ℃ for 48h, separating the product by virtue of an external magnetic field, and washing to be neutral to obtain the magnetic graphene-based polyimideAmines of which FeCl3·6H2O、Ni(NO3)2·6H2O, NaAc and NaOH are in a mass ratio of 1-1.5: 2-3: 0.1-0.5, and the addition amount of the polyimide polyamine dendrimer is FeCl3·6H28-12% of the mass of O, and the addition amount of the carboxylated graphene is FeCl3·6H24-6% of the mass of O.
4. The method for simultaneously detecting the contents of six components in a Sanwu capsule according to claim 1, wherein: the HPLC is equipped with an ultraviolet detector, the detection wavelength is set to 200-300nm, and the stationary phase of the HPLC is C18Chromatographic column with flowability A of 0.1-1.0% concentration diethylamine solution, phosphoric acid regulated diethylamine solution pH of 3.0-6.0 and flowability B of acetonitrile, and gradient elution at 20-35 deg.c.
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