CN103033588A - Comprehensive detection method for cynomorium kidney tonifying capsule - Google Patents
Comprehensive detection method for cynomorium kidney tonifying capsule Download PDFInfo
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Abstract
The invention relates to a detection method for a cynomorium kidney tonifying capsule, and belongs to the field of traditional Chinese medicine modernization. According to the detection method, cistanche, herba epimedii, Chinese angelica, fructus cnidii, schisandra chinensis, cinnamon and liquorice are comprehensively subjected to identification and content determination, and the detection method for the cynomorium kidney tonifying capsule is specified by combining the original microscopic identification. The detection method solves the problem that the inspection only with the microscopic identification is not comprehensive; the components of the capsule can be detected more comprehensively; the content and stability of the capsule can be understood; and the description of a medicinal material basis of the capsule is facilitated.
Description
Technical field
The invention belongs to modern Chinese traditional medicine field, be specifically related to a kind of detection method of cynomorium songaricum capsule for tonifying kidney.
Background technology
Traditional Chinese medicine ingredients is complicated, and particularly Chinese medicine compound prescription often contains multiclass, Multiple components, has consisted of a very complicated system.At present, new active component Chinese medicine preparation and the research and development of modern Chinese traditional compound medicine are on the increase, and new technique and multiple different extracting mode also are used for research and the production of medicine.
Along with the fast development of Modern Testing, equipment and instrument, the assay of Chinese medicine, chromatographic identification become the important means of detection.But assay or the discriminating of at present generally only setting up a certain index chemical composition for the simultaneously applied situation of above-mentioned multiple new technology, are only set up the assay of certain single component or are differentiated to a great extent with larger one-sidedness.
The cynomorium songaricum capsule for tonifying kidney has tonifying kidney and strengthening yang, and the admittedly true effect of replenishing essence is used for the diseases such as impotence that kidney-yang deficiency or kidney-yin deficiency cause, seminal emission, premature ejaculation.
The cynomorium songaricum capsule for tonifying kidney is capsule, and content is that yellowish-brown is to tan particle and powder; The little perfume (or spice) of gas, bitter, suffering, little acid.
Its prescription is: cynomorium songaricum 31g, thizoma curculiginis 31g, Morinda officinalis 31g, Radix Angelicae Sinensis 31g, frutus cnidii 31g, saline cistanche (steaming) 31g, semen allii tuberosi 47g, the fruit of Chinese magnoliavine (steaming) 20g, red ginseng 16g, pizzle (system) 16g, dog kidney (system) 16g, pilose antler 10g, black in sheet 10g, Chinese cassia tree 10g, fennel seeds 10g, actinote (forging) 10g, Chinese prickly ash 10g, seed of Chinese dodder 31g, the bark of eucommia (salt stir-fry) 31g, semen astragali complanati (salt stir-fry) 31g, Radix Codonopsis (honey is processed) 31g, the fruit of medicinal cornel (steaming) 31g, barrenwort 31g, the Radix Astragali (honey is processed) 31g, Chinese yam 31g, prepared rhizome of rehmannia 31g, Psoralea corylifolia (salt stir-fry) 20g, fruit of Chinese wolfberry 20g, raspberry 20g, polygala root 20g, stamen nelumbini 20g, fruit of Cherokee rose 20g, rhizoma alismatis 10g, Radix Glycyrrhizae (honey is processed) 10g, Poria cocos 10g.
Method for making: above 30 five tastes, cynomorium songaricum, thizoma curculiginis, Morinda officinalis, Radix Angelicae Sinensis, frutus cnidii, saline cistanche, semen allii tuberosi, the fruit of Chinese magnoliavine, red ginseng, pizzle, dog kidney, pilose antler, black in sheet, Chinese cassia tree, fennel seeds, actinote, Chinese prickly ash 17 flavors, be ground into fine powder, sieve, mixing; 18 flavors such as all the other seed of Chinese dodders, the boiling secondary, each 3 hours, collecting decoction filtered, and filtrate is condensed into the thick paste shape, adds above-mentioned fine powder, mixing, granulation, drying incapsulates, and makes 1000, and get final product.Oral, one time 3～5,2～3 times on the one.
Adopt the kidney-yang nourishing medicines such as barrenwort, pilose antler, actinote, Chinese prickly ash, the seed of Chinese dodder, the bark of eucommia, semen astragali complanati, Psoralea corylifolia in the side, reached nourishing liver and kidney, the effect of strong Jinsuo urine.Monarch drug in a prescription cynomorium songaricum, ministerial drug Morinda officinalis, saline cistanche, barrenwort, semen allii tuberosi tonifying kidney and strengthening yang; Stamen nelumbini supplementing the kidney to control the nocturnal in the adjutant, Chinese yam, Poria cocos, the peaceful heart of rhizoma alismatis invigorating the spleen, eliminating dampness and diuresis, remove kidney channel damp and hot, adopt simultaneously the drugs for nourishing yin such as Radix Codonopsis, the fruit of Chinese wolfberry, prepared rhizome of rehmannia, the bark of eucommia, tonify the liver and kidney, cooperate nourishing, the laxative action of the flavour of a drug such as Radix Angelicae Sinensis, frutus cnidii, the fruit of Chinese magnoliavine, Chinese cassia tree, reach property of medicine gentleness; With Radix Glycyrrhizae with all medicine property of medicine in the side of blending, for making medicine also.According to theory of traditional Chinese medical science, this product is nourishing kidney-yin both, kidney-replenishing again, and tonifying both YIN and YANG, gentle and lasting, regulate equilibrium between yin and yang, make the people reach the state of " yin and yang in equilibrium, life activities being normally maintained ".
Only having micro-discriminating in the original detection method of cynomorium songaricum capsule for tonifying kidney, is to utilize microtechnic that Chinese medicine is carried out microscopic analysis, to determine a kind of authentication method of its kind and quality.Microscopic Identification mainly comprises tissue characterization and powder evaluation, utilize microscope to observe the feature of the histological structure of medicinal material, cell shape and inclusions, the optical characteristics of mineral, with use the microscopic chemistry method, determine the character of cell membrane and cell inclusion or some kind effective constituent distribution in tissue etc., in order to the true and false and purity even the quality of differentiating medicinal material.Such survey detecting method needs to cooperate modern other detection method could more fully reflect the content of the important composition of cynomorium songaricum capsule for tonifying kidney to a great extent with larger one-sidedness.
Summary of the invention
The invention provides a kind of detection method of cynomorium songaricum capsule for tonifying kidney
,The comprehensive not problem of detection that exists to solve present micro-discriminating.
The technical scheme that the present invention takes is to comprise following discrimination method and content assaying method:
(1) discrimination method
(1) get this product, put microscopically and observe: needle-like calcium oxalate crystal is very thin, and bunchy is present in the parenchyma cell brokenly; The needle-like calcium oxalate crystal bundle is neat or be staggered, long 40～150 μ m, and diameter 4 μ m are present in the mucilage cell; The endocarp cell is yellow, makes zyklopisch and arranges, and wall is beaded and thickens.Formation of Endosperm Cell Walls is inhomogeneous to be thickened, and larger circular pit is arranged; Plant epidermis skin lithocyte fallow, the class polygon is seen on the surface, and wall is thicker, and the hole ditch is fine and closely woven, and cell contains the burgundy thing; Calcium oxalate cluster crystal diameter 20～68 μ m, the sharp point of corner angle; Square or the similar round of lithocyte class, wall are simultaneously poor; Colourless crystallization is column or bulk; Endocarp cell staple fibre shape is made zyklopisch arrangement or levels and is intersected vertically;
(2) get this product cynomorium songaricum capsule for tonifying kidney content 6g, the 40ml that adds diethyl ether, ultrasonic processing 10 minutes, power 250W, frequency 40KHz lets cool, and filters, and filtrate is put in 60 ℃ of water-baths and is flung to ether, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Radix Angelicae Sinensis control medicinal material 0.5g, is made in the same way of control medicinal material solution; According to the test of an appendix VI of Chinese Pharmacopoeia version in 2005 B thin-layered chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, take cyclohexane: ethyl acetate=7:1 as developping agent, launch, take out, dry, put under the 365nm ultraviolet lamp and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color;
(3) get this product cynomorium songaricum capsule for tonifying kidney content 6g, add ethanol 80ml, ultrasonic processing 30 minutes, power 250W, frequency 40KHz filters, filtrate evaporate to dryness, residue add water 20ml, and heating makes dissolving, let cool, use extracted by ether 2 times, each 20 ml, merge ether solution, put in 60 ℃ of water-baths and volatilize, residue adds ethanol 1ml makes dissolving, as need testing solution; Other gets the Osthole reference substance, adds ethanol and makes the solution that every lml contains lmg, in contrast product solution; According to the test of an appendix VI of Chinese Pharmacopoeia version in 2005 B thin-layered chromatography, draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, take 60～90 ℃ of sherwood oil: ethyl acetate=4:1 as developping agent, launch, take out, dry, put under the 365nm ultraviolet lamp and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color;
(2) content assaying method:
(1) according to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring;
Chromatographic condition and system suitability: be filling agent with octadecylsilane chemically bonded silica; Acetonitrile: water=45:55 is mobile phase; The detection wavelength is 324nm; 30 ℃ of column temperatures, number of theoretical plate calculate by the Osthole peak should be not less than 7000;
The preparation of reference substance solution: it is an amount of that precision takes by weighing the Osthole reference substance, adds methyl alcohol and make the solution that every 1ml contains 40 μ g, and get final product;
The preparation of need testing solution: get the content 1g under this product cynomorium songaricum capsule for tonifying kidney content uniformity item, accurately weighed, put in the tool plug conical flask, accurate methyl alcohol 25ml, close plug, the weighed weight of adding, placed ultrasonic processing 30 minutes, power 250W 2 hours, frequency 40KHz lets cool, more weighed weight, supply less loss weight with methyl alcohol, shake up, filter, get subsequent filtrate, and get final product;
Determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product;
(2) according to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring;
Chromatographic condition and system suitability
:Take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile: water=50:50 as mobile phase; The detection wavelength is 250nm, and number of theoretical plate calculates by the schizandrin peak should be not less than 10000;
The preparation of reference substance solution: get the schizandrin reference substance an amount of, accurately weighed, add methyl alcohol and make the solution that every 1ml contains 20 μ g, and get final product;
The preparation of need testing solution: get the content under the cynomorium songaricum capsule for tonifying kidney content uniformity item, porphyrize is got 1g, and is accurately weighed, put in the tool plug conical flask accurate methyl alcohol 20ml, the close plug of adding, weighed weight, ultrasonic processing 30 minutes, power is 250W, frequency is 30kHz, takes out, and lets cool, weighed weight is again supplied the weight of less loss, mixing with methyl alcohol, filter, get subsequent filtrate, and get final product;
Determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product;
(3) according to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring;
Chromatographic condition and system suitability
:Take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile: water=33:67 as mobile phase; The detection wavelength is 290nm, and number of theoretical plate calculates by the cinnaldehydrum peak should be not less than 3000;
The preparation of reference substance solution
:It is an amount of that precision takes by weighing the cinnaldehydrum reference substance, adds methyl alcohol and make the solution that every 1ml contains 10 μ g, and get final product;
The preparation of need testing solution: get the content under the cynomorium songaricum capsule for tonifying kidney content uniformity item, porphyrize is got 2g, and is accurately weighed, puts in the tool plug conical flask, adds methenyl choloride 50ml, and ultrasonic extraction 30 minutes filters, and discards filtrate; The dregs of a decoction volatilize solvent together with filter paper, accurate methyl alcohol 50ml, the close plug of adding, weighed weight, ultrasonic processing 10 minutes, power is 250W, frequency is 40kHz, and placement is spent the night, with more ultrasonic processing 1 time of method, weighed weight is again supplied the weight of less loss, mixing with methyl alcohol, filter, the accurate subsequent filtrate 5ml that draws puts in the 25ml measuring bottle, add methyl alcohol to scale, shake up, and get final product;
Determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.；
(4) chromatographic condition and system suitability are take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile: methyl alcohol: 1% acetic acid 10:9:81 is as mobile phase; The detection wavelength is 334nm, and theoretical cam curve is calculated by the echinacoside peak should be not less than 3000;
Get the echinacoside reference substance according to the preparation of product solution an amount of, accurately weighed, add 50% methyl alcohol and make the solution that every 1ml contains 0.1mg, and get final product;
The preparation of need testing solution: get this product cynomorium songaricum capsule for tonifying kidney content under the weight differential item, get 5.0g, accurately weighed, put in the tool plug conical flask accurate 50% methyl alcohol 50ml, the close plug of adding, weighed weight was soaked ultrasonic processing 30 minutes 30 minutes, power 250W, frequency 40kHz lets cool, weighed weight again, supply the weight of less loss with 50% methyl alcohol, shake up, filter; Precision measures subsequent filtrate 10ml, and evaporate to dryness, residue add water 20ml makes dissolving, be transferred in the separating funnel, use extracted by ether 2 times, each 30ml, discard ether solution, and then wash 2 times with water-saturated n-butanol, each 20 ml, merge normal butyl alcohol liquid, evaporate to dryness, residue add 50% methyl alcohol makes dissolving, transfer in the 10ml measuring bottle, add 50% methyl alcohol to scale, filter, get subsequent filtrate, and get final product;
Determination method is accurate reference substance solution and each 10 μ l of need testing solution of drawing respectively, and the injection liquid chromatography is measured, and be get final product;
(5) chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile: 0.05% phosphoric acid=28:72 is as mobile phase; The detection wavelength is 270nm, and theoretical cam curve is calculated by the icariin peak should be not less than 3000;
It is an amount of that the icariin reference substance is got in the preparation of reference substance solution, accurately weighed, adds methyl alcohol and make the solution that every 1ml contains 40 μ g, and get final product;
The preparation of need testing solution: get this product cynomorium songaricum capsule for tonifying kidney content under the weight differential item, get 2.5g, accurately weighed, put in the tool plug conical flask accurate 20% ethanol 50ml, the close plug of adding, weighed weight, ultrasonic processing 30 minutes, power 250W, frequency 33kHz lets cool, more weighed weight, supply the weight of less loss with Diluted Alcohol, shake up, filter, get subsequent filtrate, and get final product;
Determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product;
(6) according to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring;
Chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent; Take methyl alcohol: 0.2mol/L ammonium acetate solution: glacial acetic acid=65:33:2 is as mobile phase; The detection wavelength is 250nm; Number of theoretical plate calculates by the glycyrrhizic acid peak should be not less than 2000;
The preparation of reference substance solution: extracting Radix Glycyrrhizae acid ammonium reference substance 10mg, accurately weighed, the mixed solution that adds 0.5% ammonia solution: methyl alcohol=1:1 is made the solution that every 1ml contains 0.2mg, is equivalent to every 1ml and contains glycyrrhizic acid 0.1959mg, and get final product;
The preparation of need testing solution
:Get this product cynomorium songaricum capsule for tonifying kidney content under the content uniformity item, porphyrize is got 2g, accurately weighed, put in the tool plug conical flask the accurate mixed solution 50ml that adds 0.5% ammonia solution: methyl alcohol=1:1, close plug, weighed weight, ultrasonic processing 30 minutes, power is 250W, and frequency is 20kHz, lets cool, weighed weight is again supplied the weight of less loss with above-mentioned mixed solution, shake up, filter, get subsequent filtrate, and get final product;
Determination method
Precision is drawn reference substance solution and each 20 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
Numerous 30 five tastes that reach of medicine among the side of the present invention, and adopt in a large number barrenwort, pilose antler, actinote, Chinese prickly ash, the seed of Chinese dodder, the bark of eucommia, semen astragali complanati, the kidney-yang nourishing medicines such as Psoralea corylifolia, how to regulate the balance between each medicine, most important, can reach both nourishing kidney-yins, kidney-replenishing then is rareer again, ministerial drug saline cistanche in the side, barrenwort etc. play a major role with the monarch drug in a prescription compatibility, the adjutant frutus cnidii, the fruit of Chinese magnoliavine, Chinese cassia trees etc. are to monarch drug in a prescription, ministerial drug is supervised effect, relaxing the property of medicine, but do not affect the performance curative effect such as monarch-minister drug, with making the medicine Radix Glycyrrhizae with all medicine property of medicine in the side of blending, Each performs its own functions for above-mentioned each medicine, the present invention is just in line with above-mentioned viewpoint, in conjunction with existing micro-discrimination method, under instruction of Chinese Medicine theory, according to present Chinese medicine detection method, draw technical scheme of the present invention through great many of experiments.
Advantage of the present invention is: standard the detection method of cynomorium songaricum capsule for tonifying kidney, solve the incomplete problem of inspection of originally only having micro-discriminating to exist, by saline cistanche, barrenwort, Radix Angelicae Sinensis, frutus cnidii, the fruit of Chinese magnoliavine, Chinese cassia tree, Radix Glycyrrhizae are comprehensively differentiated and assay, can more fully detect the composition of adjutant, understand its content and stability, also help to illustrate the medical substance basis of medicine.
Embodiment
The cynomorium songaricum capsule for tonifying kidney is provided by prescription and explained hereafter in the background technology by JiLin ZiXin Pharmacy Co., Ltd.
Comprise following discrimination method and content assaying method:
(1) discrimination method
(1) get this product, put microscopically and observe: needle-like calcium oxalate crystal is very thin, and bunchy is present in the parenchyma cell brokenly; The needle-like calcium oxalate crystal bundle is neat or be staggered, long 40～150 μ m, and diameter 4 μ m are present in the mucilage cell; The endocarp cell is yellow, makes zyklopisch and arranges, and wall is beaded and thickens.Formation of Endosperm Cell Walls is inhomogeneous to be thickened, and larger circular pit is arranged; Plant epidermis skin lithocyte fallow, the class polygon is seen on the surface, and wall is thicker, and the hole ditch is fine and closely woven, and cell contains the burgundy thing; Calcium oxalate cluster crystal diameter 20～68 μ m, the sharp point of corner angle; Square or the similar round of lithocyte class, wall are simultaneously poor; Colourless crystallization is column or bulk; Endocarp cell staple fibre shape is made zyklopisch arrangement or levels and is intersected vertically;
(2) get this product cynomorium songaricum capsule for tonifying kidney content 6g, the 40ml that adds diethyl ether, ultrasonic processing 10 minutes, power 250W, frequency 40KHz lets cool, and filters, and filtrate is put in 60 ℃ of water-baths and is flung to ether, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Radix Angelicae Sinensis control medicinal material 0.5g, is made in the same way of control medicinal material solution; According to the test of an appendix VI of Chinese Pharmacopoeia version in 2005 B thin-layered chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, take cyclohexane: ethyl acetate=7:1 as developping agent, launch, take out, dry, put under the 365nm ultraviolet lamp and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color;
(3) get this product cynomorium songaricum capsule for tonifying kidney content 6g, add ethanol 80ml, ultrasonic processing 30 minutes, power 250W, frequency 40KHz filters, filtrate evaporate to dryness, residue add water 20ml, and heating makes dissolving, let cool, use extracted by ether 2 times, each 20 ml, merge ether solution, put in 60 ℃ of water-baths and volatilize, residue adds ethanol 1ml makes dissolving, as need testing solution; Other gets the Osthole reference substance, adds ethanol and makes the solution that every lml contains lmg, in contrast product solution; According to the test of an appendix VI of Chinese Pharmacopoeia version in 2005 B thin-layered chromatography, draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, take 60～90 ℃ of sherwood oil: ethyl acetate=4:1 as developping agent, launch, take out, dry, put under the 365nm ultraviolet lamp and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color;
(2) content assaying method:
(1) according to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring;
Chromatographic condition and system suitability: be filling agent with octadecylsilane chemically bonded silica; Acetonitrile: water=45:55 is mobile phase; The detection wavelength is 324nm; 30 ℃ of column temperatures, number of theoretical plate calculate by the Osthole peak should be not less than 7000;
The preparation of reference substance solution: it is an amount of that precision takes by weighing the Osthole reference substance, adds methyl alcohol and make the solution that every 1ml contains 40 μ g, and get final product;
The preparation of need testing solution: get the content 1g under this product cynomorium songaricum capsule for tonifying kidney content uniformity item, accurately weighed, put in the tool plug conical flask, accurate methyl alcohol 25ml, close plug, the weighed weight of adding, placed ultrasonic processing 30 minutes, power 250W 2 hours, frequency 40KHz lets cool, more weighed weight, supply less loss weight with methyl alcohol, shake up, filter, get subsequent filtrate, and get final product;
Determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product;
(2) according to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring;
Chromatographic condition and system suitability
:Take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile: water=50:50 as mobile phase; The detection wavelength is 250nm, and number of theoretical plate calculates by the schizandrin peak should be not less than 10000;
The preparation of reference substance solution: get the schizandrin reference substance an amount of, accurately weighed, add methyl alcohol and make the solution that every 1ml contains 20 μ g, and get final product;
The preparation of need testing solution: get the content under the cynomorium songaricum capsule for tonifying kidney content uniformity item, porphyrize is got 1g, and is accurately weighed, put in the tool plug conical flask accurate methyl alcohol 20ml, the close plug of adding, weighed weight, ultrasonic processing 30 minutes, power is 250W, frequency is 30kHz, takes out, and lets cool, weighed weight is again supplied the weight of less loss, mixing with methyl alcohol, filter, get subsequent filtrate, and get final product;
Determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product;
(3) according to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring;
Chromatographic condition and system suitability
:Take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile: water=33:67 as mobile phase; The detection wavelength is 290nm, and number of theoretical plate calculates by the cinnaldehydrum peak should be not less than 3000;
The preparation of reference substance solution
:It is an amount of that precision takes by weighing the cinnaldehydrum reference substance, adds methyl alcohol and make the solution that every 1ml contains 10 μ g, and get final product;
The preparation of need testing solution: get the content under the cynomorium songaricum capsule for tonifying kidney content uniformity item, porphyrize is got 2g, and is accurately weighed, puts in the tool plug conical flask, adds methenyl choloride 50ml, and ultrasonic extraction 30 minutes filters, and discards filtrate; The dregs of a decoction volatilize solvent together with filter paper, accurate methyl alcohol 50ml, the close plug of adding, weighed weight, ultrasonic processing 10 minutes, power is 250W, frequency is 40kHz, and placement is spent the night, with more ultrasonic processing 1 time of method, weighed weight is again supplied the weight of less loss, mixing with methyl alcohol, filter, the accurate subsequent filtrate 5ml that draws puts in the 25ml measuring bottle, add methyl alcohol to scale, shake up, and get final product;
Determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.；
(4) chromatographic condition and system suitability are take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile: methyl alcohol: 1% acetic acid 10:9:81 is as mobile phase; The detection wavelength is 334nm, and theoretical cam curve is calculated by the echinacoside peak should be not less than 3000;
Get the echinacoside reference substance according to the preparation of product solution an amount of, accurately weighed, add 50% methyl alcohol and make the solution that every 1ml contains 0.1mg, and get final product;
The preparation of need testing solution: get this product cynomorium songaricum capsule for tonifying kidney content under the weight differential item, get 5.0g, accurately weighed, put in the tool plug conical flask accurate 50% methyl alcohol 50ml, the close plug of adding, weighed weight was soaked ultrasonic processing 30 minutes 30 minutes, power 250W, frequency 40kHz lets cool, weighed weight again, supply the weight of less loss with 50% methyl alcohol, shake up, filter; Precision measures subsequent filtrate 10ml, and evaporate to dryness, residue add water 20ml makes dissolving, be transferred in the separating funnel, use extracted by ether 2 times, each 30ml, discard ether solution, and then wash 2 times with water-saturated n-butanol, each 20 ml, merge normal butyl alcohol liquid, evaporate to dryness, residue add 50% methyl alcohol makes dissolving, transfer in the 10ml measuring bottle, add 50% methyl alcohol to scale, filter, get subsequent filtrate, and get final product;
Determination method is accurate reference substance solution and each 10 μ l of need testing solution of drawing respectively, and the injection liquid chromatography is measured, and be get final product;
(5) chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile: 0.05% phosphoric acid=28:72 is as mobile phase; The detection wavelength is 270nm, and theoretical cam curve is calculated by the icariin peak should be not less than 3000;
It is an amount of that the icariin reference substance is got in the preparation of reference substance solution, accurately weighed, adds methyl alcohol and make the solution that every 1ml contains 40 μ g, and get final product;
The preparation of need testing solution: get this product cynomorium songaricum capsule for tonifying kidney content under the weight differential item, get 2.5g, accurately weighed, put in the tool plug conical flask accurate 20% ethanol 50ml, the close plug of adding, weighed weight, ultrasonic processing 30 minutes, power 250W, frequency 33kHz lets cool, more weighed weight, supply the weight of less loss with Diluted Alcohol, shake up, filter, get subsequent filtrate, and get final product;
Determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product;
(6) according to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring;
Chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent; Take methyl alcohol: 0.2mol/L ammonium acetate solution: glacial acetic acid=65:33:2 is as mobile phase; The detection wavelength is 250nm; Number of theoretical plate calculates by the glycyrrhizic acid peak should be not less than 2000;
The preparation of reference substance solution: extracting Radix Glycyrrhizae acid ammonium reference substance 10mg, accurately weighed, the mixed solution that adds 0.5% ammonia solution: methyl alcohol=1:1 is made the solution that every 1ml contains 0.2mg, is equivalent to every 1ml and contains glycyrrhizic acid 0.1959mg, and get final product;
The preparation of need testing solution
:Get this product cynomorium songaricum capsule for tonifying kidney content under the content uniformity item, porphyrize is got 2g, accurately weighed, put in the tool plug conical flask the accurate mixed solution 50ml that adds 0.5% ammonia solution: methyl alcohol=1:1, close plug, weighed weight, ultrasonic processing 30 minutes, power is 250W, and frequency is 20kHz, lets cool, weighed weight is again supplied the weight of less loss with above-mentioned mixed solution, shake up, filter, get subsequent filtrate, and get final product;
Determination method: precision is drawn reference substance solution and each 20 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
Claims (1)
1. the method for comprehensive detection of a cynomorium songaricum capsule for tonifying kidney comprises following discrimination method:
Get this product cynomorium songaricum capsule for tonifying kidney content, put microscopically and observe: needle-like calcium oxalate crystal is very thin, and bunchy is present in the parenchyma cell brokenly; The needle-like calcium oxalate crystal bundle is neat or be staggered, long 40～150 μ m, and diameter 4 μ m are present in the mucilage cell; The endocarp cell is yellow, makes zyklopisch and arranges, and wall is beaded and thickens; Formation of Endosperm Cell Walls is inhomogeneous to be thickened, and larger circular pit is arranged; Plant epidermis skin lithocyte fallow, the class polygon is seen on the surface, and wall is thicker, and the hole ditch is fine and closely woven, and cell contains the burgundy thing; Calcium oxalate cluster crystal diameter 20～68 μ m, the sharp point of corner angle; Square or the similar round of lithocyte class, wall are simultaneously poor; Colourless crystallization is column or bulk; Endocarp cell staple fibre shape is made zyklopisch arrangement or levels and is intersected vertically;
Characterized by further comprising following discrimination method and content assaying method:
(1) get this product cynomorium songaricum capsule for tonifying kidney content 6g, the 40ml that adds diethyl ether, ultrasonic processing 10 minutes, power 250W, frequency 40KHz lets cool, and filters, and filtrate is put in 60 ℃ of water-baths and is flung to ether, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution; Other gets Radix Angelicae Sinensis control medicinal material 0.5g, is made in the same way of control medicinal material solution; According to the test of an appendix VI of Chinese Pharmacopoeia version in 2005 B thin-layered chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, take cyclohexane: ethyl acetate=7:1 as developping agent, launch, take out, dry, put under the 365nm ultraviolet lamp and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color;
(2) get this product cynomorium songaricum capsule for tonifying kidney content 6g, add ethanol 80ml, ultrasonic processing 30 minutes, power 250W, frequency 40KHz filters, filtrate evaporate to dryness, residue add water 20ml, and heating makes dissolving, let cool, use extracted by ether 2 times, each 20 ml, merge ether solution, put in 60 ℃ of water-baths and volatilize, residue adds ethanol 1ml makes dissolving, as need testing solution; Other gets the Osthole reference substance, adds ethanol and makes the solution that every lml contains lmg, in contrast product solution; According to the test of an appendix VI of Chinese Pharmacopoeia version in 2005 B thin-layered chromatography, draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, take 60～90 ℃ of sherwood oil: ethyl acetate=4:1 as developping agent, launch, take out, dry, put under the 365nm ultraviolet lamp and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color;
(2) content assaying method:
(1) according to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring;
Chromatographic condition and system suitability: be filling agent with octadecylsilane chemically bonded silica; Acetonitrile: water=45:55 is mobile phase; The detection wavelength is 324nm; 30 ℃ of column temperatures, number of theoretical plate calculate by the Osthole peak should be not less than 7000;
The preparation of reference substance solution: it is an amount of that precision takes by weighing the Osthole reference substance, adds methyl alcohol and make the solution that every 1ml contains 40 μ g, and get final product;
The preparation of need testing solution: get the content 1g under this product cynomorium songaricum capsule for tonifying kidney content uniformity item, accurately weighed, put in the tool plug conical flask, accurate methyl alcohol 25ml, close plug, the weighed weight of adding, placed ultrasonic processing 30 minutes, power 250W 2 hours, frequency 40KHz lets cool, more weighed weight, supply less loss weight with methyl alcohol, shake up, filter, get subsequent filtrate, and get final product;
Determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product;
(2) according to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring;
Chromatographic condition and system suitability
:Take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile: water=50:50 as mobile phase; The detection wavelength is 250nm, and number of theoretical plate calculates by the schizandrin peak should be not less than 10000;
The preparation of reference substance solution: get the schizandrin reference substance an amount of, accurately weighed, add methyl alcohol and make the solution that every 1ml contains 20 μ g, and get final product;
The preparation of need testing solution: get the content under the cynomorium songaricum capsule for tonifying kidney content uniformity item, porphyrize is got 1g, and is accurately weighed, put in the tool plug conical flask accurate methyl alcohol 20ml, the close plug of adding, weighed weight, ultrasonic processing 30 minutes, power is 250W, frequency is 30kHz, takes out, and lets cool, weighed weight is again supplied the weight of less loss, mixing with methyl alcohol, filter, get subsequent filtrate, and get final product;
Determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product;
(3) according to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring;
Chromatographic condition and system suitability
:Take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile: water=33:67 as mobile phase; The detection wavelength is 290nm, and number of theoretical plate calculates by the cinnaldehydrum peak should be not less than 3000;
The preparation of reference substance solution
:It is an amount of that precision takes by weighing the cinnaldehydrum reference substance, adds methyl alcohol and make the solution that every 1ml contains 10 μ g, and get final product;
The preparation of need testing solution: get the content under the cynomorium songaricum capsule for tonifying kidney content uniformity item, porphyrize is got 2g, and is accurately weighed, puts in the tool plug conical flask, adds methenyl choloride 50ml, and ultrasonic extraction 30 minutes filters, and discards filtrate; The dregs of a decoction volatilize solvent together with filter paper, accurate methyl alcohol 50ml, the close plug of adding, weighed weight, ultrasonic processing 10 minutes, power is 250W, frequency is 40kHz, and placement is spent the night, with more ultrasonic processing 1 time of method, weighed weight is again supplied the weight of less loss, mixing with methyl alcohol, filter, the accurate subsequent filtrate 5ml that draws puts in the 25ml measuring bottle, add methyl alcohol to scale, shake up, and get final product;
Determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product;
(4) chromatographic condition and system suitability are take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile: methyl alcohol: 1% acetic acid 10:9:81 is as mobile phase; The detection wavelength is 334nm, and theoretical cam curve is calculated by the echinacoside peak should be not less than 3000;
Get the echinacoside reference substance according to the preparation of product solution an amount of, accurately weighed, add 50% methyl alcohol and make the solution that every 1ml contains 0.1mg, and get final product;
The preparation of need testing solution: get this product cynomorium songaricum capsule for tonifying kidney content under the weight differential item, get 5.0g, accurately weighed, put in the tool plug conical flask accurate 50% methyl alcohol 50ml, the close plug of adding, weighed weight was soaked ultrasonic processing 30 minutes 30 minutes, power 250W, frequency 40kHz lets cool, weighed weight again, supply the weight of less loss with 50% methyl alcohol, shake up, filter; Precision measures subsequent filtrate 10ml, and evaporate to dryness, residue add water 20ml makes dissolving, be transferred in the separating funnel, use extracted by ether 2 times, each 30ml, discard ether solution, and then wash 2 times with water-saturated n-butanol, each 20 ml, merge normal butyl alcohol liquid, evaporate to dryness, residue add 50% methyl alcohol makes dissolving, transfer in the 10ml measuring bottle, add 50% methyl alcohol to scale, filter, get subsequent filtrate, and get final product;
Determination method is accurate reference substance solution and each 10 μ l of need testing solution of drawing respectively, and the injection liquid chromatography is measured, and be get final product;
(5) chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile: 0.05% phosphoric acid=28:72 is as mobile phase; The detection wavelength is 270nm, and theoretical cam curve is calculated by the icariin peak should be not less than 3000;
It is an amount of that the icariin reference substance is got in the preparation of reference substance solution, accurately weighed, adds methyl alcohol and make the solution that every 1ml contains 40 μ g, and get final product;
The preparation of need testing solution: get this product cynomorium songaricum capsule for tonifying kidney content under the weight differential item, get 2.5g, accurately weighed, put in the tool plug conical flask accurate 20% ethanol 50ml, the close plug of adding, weighed weight, ultrasonic processing 30 minutes, power 250W, frequency 33kHz lets cool, more weighed weight, supply the weight of less loss with Diluted Alcohol, shake up, filter, get subsequent filtrate, and get final product;
Determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product;
(6) according to an appendix VI of Chinese Pharmacopoeia version in 2005 D high effective liquid chromatography for measuring;
Chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent; Take methyl alcohol: 0.2mol/L ammonium acetate solution: glacial acetic acid=65:33:2 is as mobile phase; The detection wavelength is 250nm; Number of theoretical plate calculates by the glycyrrhizic acid peak should be not less than 2000;
The preparation of reference substance solution: extracting Radix Glycyrrhizae acid ammonium reference substance 10mg, accurately weighed, the mixed solution that adds 0.5% ammonia solution: methyl alcohol=1:1 is made the solution that every 1ml contains 0.2mg, is equivalent to every 1ml and contains glycyrrhizic acid 0.1959mg, and get final product;
The preparation of need testing solution
:Get this product cynomorium songaricum capsule for tonifying kidney content under the content uniformity item, porphyrize is got 2g, accurately weighed, put in the tool plug conical flask the accurate mixed solution 50ml that adds 0.5% ammonia solution: methyl alcohol=1:1, close plug, weighed weight, ultrasonic processing 30 minutes, power is 250W, and frequency is 20kHz, lets cool, weighed weight is again supplied the weight of less loss with above-mentioned mixed solution, shake up, filter, get subsequent filtrate, and get final product;
Determination method
Precision is drawn reference substance solution and each 20 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
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Application publication date: 20130410 |