CN103018396A - Test method of cynomorium songaricum kidney-tonifying capsule - Google Patents
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- CN103018396A CN103018396A CN2013100002820A CN201310000282A CN103018396A CN 103018396 A CN103018396 A CN 103018396A CN 2013100002820 A CN2013100002820 A CN 2013100002820A CN 201310000282 A CN201310000282 A CN 201310000282A CN 103018396 A CN103018396 A CN 103018396A
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Abstract
The invention relates to a test method of a cynomorium songaricum kidney-tonifying capsule, and belongs to the field of traditional Chinese medicine modernization. According to the invention, through comprehensively performing identification and content determination of Angelica sinensis, fructus cnidii selinum, magnolia vine fruit and cinnamon, in cooperation with the previous micro-identification, the test method of the cynomorium songaricum kidney tonifying capsule is normalized to solve the problem of incomplete testing previously existing only in micro-differentiation, so that the components of the drug can be tested more comprehensively to know the content and stability thereof, which is also beneficial to explaining the pharmaceutical material basis of the drug.
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 constitution 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, it is damp and hot to remove kidney channel, 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 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; It is fallow to plant epidermis skin lithocyte, and 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:
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 with methyl alcohol and to subtract weight loss, 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.
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, adjutant frutus cnidii in the side, Radix Angelicae Sinensis etc. are to monarch drug in a prescription, ministerial drug is supervised effect, to relax the property of medicine, but do not affect the performance curative effects such as monarch drug in a prescription, be even more important so the detection of adjutant among this side just seemed, the present invention is just in line with above-mentioned viewpoint, under instruction of Chinese Medicine theory, according to present Chinese medicine detection method, in conjunction with existing micro-discriminating, 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 to Radix Angelicae Sinensis, frutus cnidii is comprehensively differentiated and assay, can more fully detect the composition of this medicine, 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) 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; It is fallow to plant epidermis skin lithocyte, and 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:
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 with methyl alcohol and to subtract weight loss, 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.
Claims (1)
1. the detection method 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; It is fallow to plant epidermis skin lithocyte, and 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) discrimination 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:
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 with methyl alcohol and to subtract weight loss, 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.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105675750A (en) * | 2016-01-18 | 2016-06-15 | 吉林修正药业新药开发有限公司 | Method for constructing HPLC characteristic chromatogram of Chinese patent medicine 'Yishen Bugu liquid' |
| CN107290442A (en) * | 2017-04-28 | 2017-10-24 | 中国环境科学研究院 | The method for determining four kinds of compositions in cynomorium songaricum simultaneously |
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| CN102038902A (en) * | 2009-10-26 | 2011-05-04 | 天津中新药业集团股份有限公司达仁堂制药厂 | Quality control method of traditional Chinese medicine preparation xiaoerbaishou pill |
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- 2013-01-01 CN CN2013100002820A patent/CN103018396A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102038902A (en) * | 2009-10-26 | 2011-05-04 | 天津中新药业集团股份有限公司达仁堂制药厂 | Quality control method of traditional Chinese medicine preparation xiaoerbaishou pill |
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| 郑立卿等: "薄层扫描法测定蛇床子提取液中蛇床子素的含量", 《河北北方学院学报（医学版）》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105675750A (en) * | 2016-01-18 | 2016-06-15 | 吉林修正药业新药开发有限公司 | Method for constructing HPLC characteristic chromatogram of Chinese patent medicine 'Yishen Bugu liquid' |
| CN107290442A (en) * | 2017-04-28 | 2017-10-24 | 中国环境科学研究院 | The method for determining four kinds of compositions in cynomorium songaricum simultaneously |
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Application publication date: 20130403 |