CN102048990B - Quality control method for Chinese medicinal preparation Qinggong Shoutao pills - Google Patents
Quality control method for Chinese medicinal preparation Qinggong Shoutao pills Download PDFInfo
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Abstract
The invention relates to a quality control method for a Chinese medicinal preparation Qinggong Shoutao pills, which comprises the following steps of: performing microscopical identification; and identifying whether the prescription of the Qinggong Shoutao pills comprises components such as Chinese angelica, medlar and dwarf lilyturf tuber or not by thin layer chromatography. On the basis of the primary standard, the microscopical identification method for the Qinggong Shoutao pills is modified, the descriptions of microscopical characteristics of ginseng and rehmannia root in the primary standard are deleted, the thin layer identification method for the Chinese angelica, the medlar and the dwarf lilyturf tuber is added, so that counterfeit medicines and inferior medicines can be more accurately inspected, the quality control of the medicines is improved, and the method has great significance for the modernization and internationalization of traditional Chinese medicines.
Description
Technical field
The invention belongs to technical field of traditional Chinese medicines, relate to the detection method of Chinese medicine, the method for quality control of especially a kind of Chinese medicine preparation palace of the Qing Dynasty peach offered as a birthday present ball.
Background technology
Palace of the Qing Dynasty peach offered as a birthday present ball is made up of donkey kidney, deer kidney, dog kidney, the fruit of Chinese wolfberry, genseng, asparagus fern, the tuber of dwarf lilyturf, glutinous rehmannia, Radix Angelicae Sinensis, intelligence development (salt system), silkworm excrement, spina date seed (stir-fry), diaphragma juglandis (stir-bake to brown), and its preparation method is: above 13 flavors are ground into fine powder; Sieve, mixing, every 100g powder add refined honey 150~170g and process big honeyed pills and promptly get; Palace of the Qing Dynasty peach offered as a birthday present ball has kidney-tonifying sperm-generating, and benefit unit is strong, and is dizzy tired due to the aging that is used to suffer from a deficiency of the kidney; Be losing one's memory soreness and weakness of waist and knees, Hiccough and deaf; Dim eyesight is shed tears, frequent urination at night, diseases such as dripping urination.
Though still there is not the international standard of plant medicine at present in the world; The trend of Chinese medicine standard but the south east asia of the U.S., European Union, China and tradition outlet Chinese medicine is improved; In the case, the standard that needs to propose to be fit to China's product quality is to adapt to international standard, and it is historical that China has the Chinese medicine in thousands of years to use; Countries in the world are many Chinese medicine standards with reference to China in working out corresponding autonomic drug target level of product quality, so quality standard perfect, that improve Chinese medicine is more extremely urgent.
Peach offered as a birthday present ball existing quality standard in the palace of the Qing Dynasty does not have the concrete authentication method about each composition; Just describe from microstructure; The qualitative and quantitative detection that is unfavorable for so very much this medicine brings very big difficulty for the quality control of this medicine, according to retrieval; Do not have the related patent U.S. Patent No. about the method for quality control of palace of the Qing Dynasty peach offered as a birthday present ball at present, existing patent mainly concentrates on the important prescription and preparation method of palace of the Qing Dynasty peach offered as a birthday present ball.
Summary of the invention
The objective of the invention is to overcome the weak point of prior art, a kind of method of quality control of Chinese medicine preparation palace of the Qing Dynasty peach offered as a birthday present ball that can the qualitative and quantitative analysis drug ingedient is provided.
The objective of the invention is to realize through following technical scheme:
The method of quality control of a kind of Chinese medicine preparation palace of the Qing Dynasty peach offered as a birthday present ball, step is:
(1) microscopical identification;
(2) adopt thin-layered chromatography,, differentiate the Radix Angelicae Sinensis in the prescription with when being classified as control medicinal material;
(3) adopting thin-layered chromatography, is control medicinal material with the fruit of Chinese wolfberry, differentiates the fruit of Chinese wolfberry in the prescription;
(4) adopting thin-layered chromatography, is control medicinal material with the tuber of dwarf lilyturf, differentiates the tuber of dwarf lilyturf in the prescription.
And said microscopical identification step is: put microscopically and observe: plant the faint yellow extremely yellow of skin lithocyte, and wall thickness, wavy bending, cell contains brown thing; Endotesta prothenchyma (of wood) yellowish-brown or rufous, wall is thicker, non-lignify, cell contains siliceous; It is in blocks to plant the skin palisade cells, yellowish-brown or light red brown, and type polygon is arranged closely, norma lateralis long column shape, long 60~145 μ m; Contain numerous tiny calcium oxalate cluster crystals in the indigested mesophyll tissue fragment, diameter 5~20 μ m.
And said thin-layered chromatography differentiates that the method for the Radix Angelicae Sinensis composition in the prescription is:
1. the preparation of need testing solution: get palace of the Qing Dynasty peach offered as a birthday present ball sample 9g, shred, the 20ml that adds diethyl ether, sonicated 15 minutes filters, and filtrating volatilizes, and residue adds methyl alcohol 3ml makes dissolving, as need testing solution;
2. the preparation of control medicinal material solution: get Radix Angelicae Sinensis control medicinal material 0.5g, the 20ml that adds diethyl ether, sonicated 15 minutes filters, and filtrating volatilizes, and residue adds methyl alcohol 3ml makes dissolving, as control medicinal material solution;
3. thin layer condition and result: the thin-layer chromatography test, draw each 2~4 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate; With normal hexane: ethyl acetate=4: 1 is developping agent, launches, and takes out; Dry; Put under the ultraviolet lamp 365nm and inspect, inspect in the test sample chromatogram with the corresponding position of control medicinal material chromatogram on whether show the fluorescence spot of same color, confirm to supply whether to contain the Radix Angelicae Sinensis composition in the test agent.
And said thin-layered chromatography differentiates that the method for the fruit of Chinese wolfberry composition in the prescription is:
1. the preparation of need testing solution: get palace of the Qing Dynasty peach offered as a birthday present ball sample 9g, shred, add water 30ml, heated and boiled 15 minutes; Put coldly, centrifugal 5 minutes of 3000rpm gets supernatant; Extract 2 times each 20ml, combined ethyl acetate liquid with the ethyl acetate jolting; Evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution;
2. the preparation of control medicinal material solution: get fruit of Chinese wolfberry control medicinal material 1g, add water 30ml, heated and boiled 15 minutes; Put coldly, centrifugal 5 minutes of 3000rpm gets supernatant; Extract 2 times each 20ml, combined ethyl acetate liquid with the ethyl acetate jolting; Evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as control medicinal material solution;
3. thin layer condition and result: the thin-layer chromatography test, draw each 4~6 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate; With methenyl choloride: ethyl acetate: formic acid=2: 3: 1 is developping agent, launches, and takes out; Dry; Put under the ultraviolet lamp 365nm and inspect, inspect in the test sample chromatogram with the corresponding position of control medicinal material chromatogram on whether show the fluorescence spot of same color, confirm to supply whether to contain fruit of Chinese wolfberry composition in the test agent.
And, said thin-layered chromatography differentiate in the prescription the tuber of dwarf lilyturf composition method be:
1. the preparation of need testing solution: get palace of the Qing Dynasty peach offered as a birthday present ball sample 9g, add methyl alcohol 30ml, sonicated 30 minutes is put cold; Filter, the filtrating evaporate to dryness, residue adds water 25ml makes dissolving; Extract 2 times with the methenyl choloride jolting, each 20ml merges methenyl choloride; Evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as need testing solution;
2. the preparation of control medicinal material solution: get the control medicinal material 2g tuber of dwarf lilyturf, add methyl alcohol 30ml, sonicated 30 minutes is put cold; Filter, the filtrating evaporate to dryness, residue adds water 25ml makes dissolving; Extract 2 times with the methenyl choloride jolting, each 20ml merges methenyl choloride liquid; Evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as control medicinal material solution;
3. thin layer condition and result: the thin-layer chromatography test, draw each 4~6 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate; With methenyl choloride: acetone=4: 1 is developping agent, launches, and takes out; Dry; Spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the spot colour developing, places daylight and ultraviolet lamp 365nm to detect down; Inspect in the test sample chromatogram with the corresponding position of control medicinal material chromatogram on whether show the spot or the fluorescence spot of same color respectively, confirm to supply whether to contain the composition tuber of dwarf lilyturf in the test agent.
Advantage of the present invention and good effect are:
1, the palace of the Qing Dynasty of the present invention peach offered as a birthday present ball is on the primary standard basis; Revised the microscopical identification method; Radix Angelicae Sinensis, the fruit of Chinese wolfberry, the thin layer discrimination method of the tuber of dwarf lilyturf have been increased; Can check out counterfeit drug and substandard drug more exactly after the modification, the quality control that has improved medicine, the modernization of Chinese medicine and Chinese medicine gone abroad to be significant.
2, in the peach offered as a birthday present ball primary standard of the palace of the Qing Dynasty, adopt the microscopical identification method that the fruit of Chinese wolfberry, intelligence development, genseng and glutinous rehmannia are described, check discovery; Because genseng, after the special processing of ecliptic longitude; Microscopic features separately are not obvious, cause its characteristic to be not easy to observe, so deleted the description of the microscopic features of genseng, glutinous rehmannia in the primary standard; The present invention revises part microscopic features in the primary standard, has increased the feature description of spina date seed, silkworm excrement in the prescription simultaneously.
Description of drawings
200601), sample 2 (lot number: 200602), sample 3 (lot number: 200603), the Radix Angelicae Sinensis control medicinal material Fig. 1 inspects figure for the present invention supplies in the test agent Radix Angelicae Sinensis to detect thin-layer chromatogram at ultraviolet lamp (365nm), and wherein band is followed successively by from left to right: negative control, sample 1 (lot number:;
200601), sample 2 (lot number: 200602), sample 3 (lot number: 200603), the fruit of Chinese wolfberry control medicinal material Fig. 2 detects chromatogram at ultraviolet lamp (365nm) for the present invention supplies in the test agent fruit of Chinese wolfberry, and wherein band is followed successively by from left to right: negative control, sample 1 (lot number:;
Fig. 3 detects thin-layer chromatogram and under daylight, inspects figure for the present invention supplies tuber of dwarf lilyturf in the test agent; Wherein band is followed successively by from left to right: negative control, sample 1 (lot number: 200601; 6 μ l), sample 2 (lot number: 200602; 6 μ l), sample 3 (lot number: 200603,6 μ l), the tuber of dwarf lilyturf control medicinal material, sample 1 (lot number: 200601,2 μ l);
Fig. 4 inspects under ultraviolet lamp (365nm) for the present invention supplies in the test agent detect thin-layer chromatogram the tuber of dwarf lilyturf; Wherein, 200601,6 μ l), sample 2 (lot number: 200602,6 μ l), sample 3 (lot number: 200603 wherein band is followed successively by from left to right: negative control, sample 1 (lot number:; 6 μ l), the tuber of dwarf lilyturf control medicinal material, sample 1 (lot number: 200601,2 μ l).
Embodiment
Below in conjunction with embodiment, the present invention is further specified, following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
The method of quality control of Chinese medicine preparation palace of the Qing Dynasty peach offered as a birthday present ball, the step of its method is:
(1) microscopical identification:
Putting microscopically observes: plant the faint yellow extremely yellow of skin lithocyte, and wall thickness, wavy bending, cell contains brown thing (fruit of Chinese wolfberry).Endotesta prothenchyma (of wood) yellowish-brown or rufous, wall is thicker, non-lignify, cell contains siliceous (intelligence development).It is in blocks to plant the skin palisade cells, yellowish-brown or light red brown, and type polygon is arranged closely, norma lateralis long column shape, long 60~145 μ m (spina date seed).Contain numerous tiny calcium oxalate cluster crystals in the indigested mesophyll tissue fragment, diameter 5~20 μ m (silkworm excrement).
(2) Radix Angelicae Sinensis: with reference to " related content of Chinese pharmacopoeia version in 2005 is worked out.Adopting thin-layered chromatography, is contrast with the Radix Angelicae Sinensis control medicinal material, differentiates the Radix Angelicae Sinensis in the prescription.
1. the preparation of need testing solution: get palace of the Qing Dynasty peach offered as a birthday present ball sample 9g, shred, the 20ml that adds diethyl ether, sonicated 15 minutes filters, and filtrating volatilizes, and residue adds methyl alcohol 3ml makes dissolving, as need testing solution.
2. the preparation of control medicinal material solution: get Radix Angelicae Sinensis control medicinal material 0.5g, the 20ml that adds diethyl ether, sonicated 15 minutes filters, and filtrating volatilizes, and residue adds methyl alcohol 3ml makes dissolving, as control medicinal material solution.
3. the preparation of negative sample solution: by the prescription proportioning, get other flavour of a drug except that Radix Angelicae Sinensis, process pill, make negative sample solution by above-mentioned need testing solution preparation method again by former medicine preparation technology.
4. thin layer condition and result: according to thin-layered chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test; Draw each 2~4 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with normal hexane: ethyl acetate=4: 1 is developping agent; Launch; Take out, dry, put under the ultraviolet lamp 365nm and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color, negative sample solution is noiseless, measures the result and sees Fig. 1.
(3) fruit of Chinese wolfberry: with reference to " related content of Chinese pharmacopoeia version in 2005 is worked out.Adopting thin-layered chromatography, is control medicinal material with the fruit of Chinese wolfberry, differentiates the fruit of Chinese wolfberry in the prescription.
1. the preparation of need testing solution: get palace of the Qing Dynasty peach offered as a birthday present ball sample 9g, shred, add water 30ml, heated and boiled 15 minutes; Put coldly, centrifugal 5 minutes (3000rpm) gets supernatant; Extract 2 times each 20ml, combined ethyl acetate liquid with the ethyl acetate jolting; Evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution.
2. the preparation of control medicinal material solution: get fruit of Chinese wolfberry control medicinal material 1g, add water 30ml, heated and boiled 15 minutes; Put coldly, centrifugal 5 minutes (3000rpm) gets supernatant; Extract 2 times each 20ml, combined ethyl acetate liquid with the ethyl acetate jolting; Evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as control medicinal material solution.
3. the preparation of negative sample solution: by the prescription proportioning, get other flavour of a drug except that the fruit of Chinese wolfberry, process pill, make negative sample solution by above-mentioned need testing solution preparation method again by former medicine preparation technology.
4. thin layer condition and result: according to thin-layered chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test; Drawing each 4~6 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, is developping agent with methenyl choloride-ethyl acetate-formic acid (2: 3: 1); Launch; Take out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color, negative sample solution is noiseless.Measure the result and see Fig. 2.
(4) tuber of dwarf lilyturf: with reference to " related content of Chinese pharmacopoeia version in 2005 is worked out.Adopting thin-layered chromatography, is control medicinal material with the tuber of dwarf lilyturf, differentiates the tuber of dwarf lilyturf in the prescription.
1. the preparation of need testing solution: get palace of the Qing Dynasty peach offered as a birthday present ball sample 9g, add methyl alcohol 30ml, sonicated 30 minutes is put cold; Filter, the filtrating evaporate to dryness, residue adds water 25ml makes dissolving; Extract 2 times with the methenyl choloride jolting, each 20ml merges methenyl choloride; Evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as need testing solution.
2. the preparation of control medicinal material solution: get the control medicinal material 2g tuber of dwarf lilyturf, add methyl alcohol 30ml, sonicated 30 minutes is put cold; Filter, the filtrating evaporate to dryness, residue adds water 25ml makes dissolving; Extract 2 times with the methenyl choloride jolting, each 20ml merges methenyl choloride liquid; Evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as control medicinal material solution.
3. the preparation of negative sample solution: by the prescription proportioning, get other flavour of a drug except that the tuber of dwarf lilyturf, process pill, make negative sample solution by above-mentioned need testing solution preparation method again by former medicine preparation technology.
4. thin layer condition and result: according to thin-layered chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw each 4~6 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate; With methenyl choloride: acetone=4: 1 is developping agent, launches, and takes out; Dry; Spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the spot colour developing, puts respectively under daylight and the ultraviolet lamp (365nm) and inspects.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot or the fluorescence spot of same color respectively.Negative sample solution is noiseless.Measure the result and see Fig. 3, Fig. 4, through finding that relatively inspect under the daylight, effect is better, so the condition of inspecting under the ultraviolet lamp (365nm) is not listed in the standard body.
Claims (1)
1. the detection method of a Chinese medicine preparation palace of the Qing Dynasty peach offered as a birthday present ball, it is characterized in that: the step of its method is:
(1) microscopical identification;
(2) adopt thin-layered chromatography,, differentiate the Radix Angelicae Sinensis in the prescription with when being classified as control medicinal material;
(3) adopting thin-layered chromatography, is control medicinal material with the fruit of Chinese wolfberry, differentiates the fruit of Chinese wolfberry in the prescription;
(4) adopting thin-layered chromatography, is control medicinal material with the tuber of dwarf lilyturf, differentiates the tuber of dwarf lilyturf in the prescription;
Said microscopical identification step is: put microscopically and observe: plant the faint yellow extremely yellow of skin lithocyte, and wall thickness, wavy bending, cell contains brown thing; Endotesta prothenchyma (of wood) yellowish-brown or rufous, wall is thicker, non-lignify, cell contains siliceous; It is in blocks to plant the skin palisade cells, yellowish-brown or light red brown, and type polygon is arranged closely, norma lateralis long column shape, long 60~145 μ m; Contain numerous tiny calcium oxalate cluster crystals in the indigested mesophyll tissue fragment, diameter 5~20 μ m;
Said thin-layered chromatography differentiates that the method for the Radix Angelicae Sinensis composition in the prescription is:
1. the preparation of need testing solution: get palace of the Qing Dynasty peach offered as a birthday present ball sample 9g, shred, the 20ml that adds diethyl ether, sonicated 15 minutes filters, and filtrating volatilizes, and residue adds methyl alcohol 3ml makes dissolving, as need testing solution;
2. the preparation of control medicinal material solution: get Radix Angelicae Sinensis control medicinal material 0.5g, the 20ml that adds diethyl ether, sonicated 15 minutes filters, and filtrating volatilizes, and residue adds methyl alcohol 3ml makes dissolving, as control medicinal material solution;
3. thin layer condition and result: the thin-layer chromatography test, draw each 2~4 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate; With normal hexane: ethyl acetate=4: 1 is developping agent, launches, and takes out; Dry; Put under the ultraviolet lamp 365nm and inspect, inspect in the test sample chromatogram with the corresponding position of control medicinal material chromatogram on whether show the fluorescence spot of same color, confirm to supply whether to contain the Radix Angelicae Sinensis composition in the test agent;
Said thin-layered chromatography differentiates that the method for the fruit of Chinese wolfberry composition in the prescription is:
1. the preparation of need testing solution: get palace of the Qing Dynasty peach offered as a birthday present ball sample 9g, shred, add water 30ml, heated and boiled 15 minutes; Put coldly, centrifugal 5 minutes of 3000rpm gets supernatant; Extract 2 times each 20ml, combined ethyl acetate liquid with the ethyl acetate jolting; Evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution;
2. the preparation of control medicinal material solution: get fruit of Chinese wolfberry control medicinal material 1g, add water 30ml, heated and boiled 15 minutes; Put coldly, centrifugal 5 minutes of 3000rpm gets supernatant; Extract 2 times each 20ml, combined ethyl acetate liquid with the ethyl acetate jolting; Evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as control medicinal material solution;
3. thin layer condition and result: the thin-layer chromatography test, draw each 4~6 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate; With methenyl choloride: ethyl acetate: formic acid=2: 3: 1 is developping agent, launches, and takes out; Dry; Put under the ultraviolet lamp 365nm and inspect, inspect in the test sample chromatogram with the corresponding position of control medicinal material chromatogram on whether show the fluorescence spot of same color, confirm to supply whether to contain fruit of Chinese wolfberry composition in the test agent;
Said thin-layered chromatography differentiate in the prescription the tuber of dwarf lilyturf composition method be:
1. the preparation of need testing solution: get palace of the Qing Dynasty peach offered as a birthday present ball sample 9g, add methyl alcohol 30ml, sonicated 30 minutes is put cold; Filter, the filtrating evaporate to dryness, residue adds water 25ml makes dissolving; Extract 2 times with the methenyl choloride jolting, each 20ml merges methenyl choloride; Evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as need testing solution;
2. the preparation of control medicinal material solution: get the control medicinal material 2g tuber of dwarf lilyturf, add methyl alcohol 30ml, sonicated 30 minutes is put cold; Filter, the filtrating evaporate to dryness, residue adds water 25ml makes dissolving; Extract 2 times with the methenyl choloride jolting, each 20ml merges methenyl choloride liquid; Evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as control medicinal material solution;
3. thin layer condition and result: the thin-layer chromatography test, draw each 4~6 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate; With methenyl choloride: acetone=4: 1 is developping agent, launches, and takes out; Dry; Spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the spot colour developing, places daylight and ultraviolet lamp 365nm to detect down; Inspect in the test sample chromatogram with the corresponding position of control medicinal material chromatogram on whether show the spot or the fluorescence spot of same color respectively, confirm to supply whether to contain the composition tuber of dwarf lilyturf in the test agent;
Said palace of the Qing Dynasty peach offered as a birthday present ball is made up of donkey kidney, deer kidney, dog kidney, the fruit of Chinese wolfberry, genseng, asparagus fern, the tuber of dwarf lilyturf, glutinous rehmannia, Radix Angelicae Sinensis, intelligence development salt system, silkworm excrement, spina date seed stir-fry, diaphragma juglandis stir-bake to brown; Its preparation method is: above 13 flavors; Be ground into fine powder; Sieve, mixing, every 100g powder add refined honey 150~170g and process big honeyed pills and promptly get.
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Address after: No.21, 10th Street, Binhai New Area Development Zone, Tianjin 300457 Patentee after: Jinyao Darentang Group Co., Ltd. Darentang Pharmaceutical Factory Address before: 300457 No. tenth, 21 Avenue, Tianjin economic and Technological Development Zone Patentee before: DARENTANG PHARMACEUTICAL FACTORY, TIANJIN ZHONGXIN PHARMACEUTICAL GROUP Co.,Ltd. |
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