CN102973621A - Three-gout sandalwood oral liquid and detecting method thereof - Google Patents
Three-gout sandalwood oral liquid and detecting method thereof Download PDFInfo
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- CN102973621A CN102973621A CN2012105704859A CN201210570485A CN102973621A CN 102973621 A CN102973621 A CN 102973621A CN 2012105704859 A CN2012105704859 A CN 2012105704859A CN 201210570485 A CN201210570485 A CN 201210570485A CN 102973621 A CN102973621 A CN 102973621A
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- lignum santali
- santali albi
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- 238000000034 method Methods 0.000 title claims abstract description 41
- 241000221035 Santalaceae Species 0.000 title abstract 5
- 235000008632 Santalum album Nutrition 0.000 title abstract 5
- 201000005569 Gout Diseases 0.000 title abstract 4
- 239000000341 volatile oil Substances 0.000 claims abstract description 69
- YQUVCSBJEUQKSH-UHFFFAOYSA-N 3,4-dihydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C(O)=C1 YQUVCSBJEUQKSH-UHFFFAOYSA-N 0.000 claims abstract description 38
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims abstract description 38
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Abstract
The invention relates to three-gout sandalwood oral liquid and a detecting method thereof. The three-gout sandalwood oral liquid is prepared by extracting active ingredients from three gouts of Chinese medicinal materials, namely sandalwood, myristica fragrans and fructus choerospondiatis. The detecting method comprises the following steps of: performing thin-layer chromatography identification on the sandalwood and the myristica fragrans; and measuring the content of protocatechuic acid and the content of gallic acid, wherein the content measuring method comprises high performance liquid chromatography and measurement of total volatile oil quantity.
Description
Technical field
The invention belongs to pharmaceutical field, be specifically related to a kind of heat clearing away effect be particularly useful for clearing away heart-fire preparation and method of quality control thereof of three flavor Lignum Santali Albi oral liquids of heat that have.
Background technology
Three flavor Lignum Santali Albi compound recipes are comprised of Lignum Santali Albi, Fructus Choerospondiatis and Semen Myristicae three flavor medical materials, and its function cures mainly and is heat clearing away, and reinforcing the heart is used for heat in the heart cardiopalmus, and the heart diseases such as dysphoria are very remarkable to treatment heart disease such as the curative effects such as coronary heart disease, pulmonary heart disease.Present three flavor Lignum Santali Albi compound recipes have a plurality of dosage forms such as powder, capsule and granule, but the deficiency of existing preparation is: powder carries inconvenience, and easily the moisture absorption is rotten, and volatile ingredient can not be preserved for a long time; And the hard capsule softgel shell dissolves slowly, causes drug effect slow; The easy moisture absorption of granule is rotten, contains the volatile-type composition and stores that content descends easily when more of a specified duration.The advantage of oral liquid is not need disintegrate, directly enters gastrointestinal tract, is beneficial to absorption, and bioavailability is good, is specially adapted to cardiovascular disease.Therefore, be necessary to develop a kind of three flavor Lignum Santali Albi oral liquids.
Three flavor Lignum Santali Albi oral liquids are in the market continued to use traditional method because of its preparation method, the difficult quality control of its oral liquid, need preparation technology is improved for this reason, make the oral liquid that obtains be not less than conventional art in effect, can control its quality simultaneously, the quality that is conducive to product improves.
For effectively controlling the quality of product, we have set up three flavor Lignum Santali Albi oral liquid method of quality control, the method adopts thin layer chromatography that Lignum Santali Albi, Semen Myristicae are differentiated, adopt high performance liquid chromatography that protocatechuic acid and gallic acid are carried out assay, the volatile oil of Semen Myristicae and Lignum Santali Albi is measured.This method of quality control specificity, stability, accuracy are all better, can guarantee the safety and stability of product quality, effectively controlled.
Summary of the invention
The object of the present invention is to provide a kind of heat clearing away effect be particularly useful for clearing away heart-fire three flavor Lignum Santali Albi oral liquid formulations and new preparation methoies of heat that have, a kind of detection method is provided simultaneously.
Three flavor Lignum Santali Albi oral liquids of the present invention comprise following raw material of Chinese medicine medicine:
Lignum Santali Albi 100-300 part Semen Myristicae 100-300 part Fructus Choerospondiatis 100-300 part
Preferred optimum formula consists of:
130 parts of 130 portions of Fructus Choerospondiatis of 130 parts of Semen Myristicaes of Lignum Santali Albi
In more than forming, the weight of each medicine of distinguishing the flavor of is calculated with crude drug, if per 1 part in grams, above-mentioned prescription forms and can be made into 1000ml.
More than form to be by weight as proportioning, when producing, can to increase or dwindle by corresponding proportion, can be take kilogram as unit such as large-scale production, or take ton as unit; Small-scale production also can be take milligram as unit, the constant rate of the Chinese crude drug weight proportion that each forms.
The Fructus Choerospondiatis extraction can be alcohol reflux among the present invention, also can be that percolation extracts.
Correctives among the present invention includes but not limited to maltose, glucose, fructose, dextran, glycosides propylhomoserin, starch, sucrose, lactose, mannitol, stevioside etc., can be wherein one or several combinations.
The antiseptic that the present invention adds includes but not limited to sorbic acid, benzoic acid, oxybenzene esters etc., can be wherein a kind of, also can be two kinds combination.
The present invention's three flavor Lignum Santali Albi oral liquid preparation processes are as follows:
1) it is an amount of to get Fructus Choerospondiatis, is ground into coarse powder, takes by weighing 100-300g, with 6 times of amount 70-80% alcohol reflux 2 times, filters, and medicinal residues are for subsequent use, and Recycled ethanol gets medicinal liquid;
2) get Lignum Santali Albi and Semen Myristicae is an amount of, Lignum Santali Albi medical material wood shavings, Semen Myristicae powder is broken into coarse powder, respectively takes by weighing 100-300g, mixes, and with steam method reflux, extract, volatile oil, separates volatile oil, and sealing is preserved, and medicinal residues are for subsequent use;
3) medicinal residues with three flavor medical materials mix, and decocting in water 1 time filters, and the medicinal liquid hold over night is got supernatant, and is concentrated, places room temperature, and the 50-70% concentration of alcohol stirs precipitate with ethanol, leaves standstill 24-48 hour, filters, and decompression filtrate recycling ethanol gets concentrated solution;
4) with the Fructus Choerospondiatis alcohol extract with merge with the precipitate with ethanol concentrated solution, adding distil water is to the about 1000ml of volume, 4 ℃ of cold preservation 48 hours.Room temperature bacteriological filtration plate sucking filtration, it is 0.2% that filtrate adds sorbic acid to concentration, boil 15 minutes after, adding stevioside to concentration is 0.3%, boiled 1 minute, the volatile oil that extracts and tween 20 with the 1:5-1:6 stirring and evenly mixing, are slowly added into the liquid (70 ℃), strong agitation, be settled to 1000ml with distilled water, fill, sterilization, and get final product.
The preferred three flavor Lignum Santali Albi oral liquid preparation processes of the present invention are as follows:
1) it is an amount of to get Fructus Choerospondiatis, is ground into coarse powder, takes by weighing 130g, with 6 times of amount 70-80% alcohol reflux 2 times, filters, and medicinal residues are for subsequent use, and Recycled ethanol gets medicinal liquid;
2) get Lignum Santali Albi and Semen Myristicae is an amount of, Lignum Santali Albi medical material wood shavings, Semen Myristicae powder is broken into coarse powder, respectively takes by weighing 130g, mixes, and with steam method reflux, extract, volatile oil 3h, separates volatile oil, and sealing is preserved, and medicinal residues are for subsequent use;
3) medicinal residues with three flavor medical materials mix, and 10 times of water gagings boil 1 time, filter, and the medicinal liquid hold over night is got supernatant, and are concentrated, place room temperature, and 60% concentration of alcohol stirs precipitate with ethanol, leave standstill 24 hours, filter, and decompression filtrate recycling ethanol gets concentrated solution;
4) with the Fructus Choerospondiatis alcohol extract with merge with the precipitate with ethanol concentrated solution, adding distil water is to the about 1000ml of volume, 4 ℃ of cold preservation 48 hours.Room temperature bacteriological filtration plate sucking filtration, it is 0.2% that filtrate adds sorbic acid to concentration, boil 15 minutes after, adding stevioside to concentration is 0.3%, boiled 1 minute, the volatile oil that extracts and tween 20 with the 1:5-1:6 stirring and evenly mixing, are slowly added into the liquid (70 ℃), strong agitation, be settled to 1000ml with distilled water, fill, sterilization, and get final product.
Below in conjunction with testing to illustrate preparation method of the present invention:
1) Lignum Santali Albi, Semen Myristicae volatile oil extract
Volatile oil is Lignum Santali Albi and the myristic effective constituent that mainly contains, and we have investigated the oil pump capacity of different extraction times, and concrete grammar is that the Lignum Santali Albi medical material is made the wood shavings shape, Semen Myristicae powder is broken into coarse powder, carries out vapor extraction, isolates volatile oil, recirculation water stays for subsequent usely in medicinal residues and the bottle, the results are shown in Table 1.
Table 1 Lignum Santali Albi and Semen Myristicae are put forward oily result
By data in the table as seen, steam reflux, extract, volatile oil refluxed after 3 hours, and oil mass no longer increases basically, and therefore, return time 3 hours was optimum extraction time.
2) the medicinal residues extraction conditions determines
With three kinds of medicinal residues mixing decocting in water, take paste-forming rate as detecting index, further extract active ingredient wherein.The concrete technology condition draws with the positive quadraturing design test method.A-amount of water (multiple), B-decocting in water time (hour), C-decocting in water number of times carries out three factors, three levels are investigated.See Table 2.
Table 2 empirical factor table
The experimental result range analysis shows, factor A, B, C are A＞B＞C on the impact of paste-forming rate, the results of analysis of variance shows, amount of water and decocting time have significant to extracting the result, extraction time is without significant, illustrate that affecting the paste-forming rate principal element is the solvent consumption, and the extraction time impact is little.And can suitably shorten extraction time and reduce extraction time from producing for economic consideration, so production is upward adopted 10 times of water gagings, is decocted for 1 time and be advisable in 2 hours.
3) selection of alcohol precipitation concentration
The decocting in water concentrated solution carries out precipitate with ethanol with 50%, 60%, 70% ethanol respectively, makes oral liquid, and place and observe its situation of change, three batches in each alcohol precipitation concentration sample, it the results are shown in following table 3.
The selection of table 3 alcohol precipitation concentration
"-" expression clarification " ± " expression slightly muddy "+" expression is muddy
Can be drawn by above result, alcohol precipitation concentration be 50% oral liquid after placing certain hour, precipitation slightly, alcohol precipitation concentration be 60%, 70% oral liquid through placing still clarification, alcohol precipitation concentration of the present invention selects 60%.
4) solubilizing agent
In order to guarantee the clarity of oral liquid, stability etc. meets the requirements, and experiment is determined best results in the miscible adding oral liquid of tween 20 and volatile oil by the screening to non-ionic surface active agents such as tween 20, Tween-60, tween 80s.And according to the materialization theories, tween 20 content in medicinal liquid reaches its critical micelle concentration (CMC) just can play solubilization.The present invention adopts the CMC of tween 20 in the By Means of Electrical Conductivity oral liquid for this reason.Its principle is combined and is formed critical micelle concentration (CMC) with being carried volatile oil by: tween 20, learns best proportioning by the catastrophe point of conductivity value and surfactant materials concentration relationship curve.
Prepare oral liquid 1000ml(by technique of the present invention and do not contain volatile oil), be divided into 10 equal portions.The volatile oil that extracts is divided into 10 equal portions, make 1:0,1:1,1:2,1:3,1:4,1:5,1:6,1:7,1:8(with tween 20 respectively and all do not add sorbic acid) and 1:0(add 0.2% sorbic acid), after stirring, join respectively in the 100ml oral liquid sample, then measure electrical conductivity at DDS-11A type conductivity meter respectively, the results are shown in Table 4.
The result shows catastrophe point between 1:5-1:6, and for guaranteeing clarity of oral liquid of the present invention, selective volatilization oil of the present invention is 1:6 with the tween 20 proportioning.
Table 4 tween 20 consumption and oral liquid electric conductivity value relation
The present invention also provides the present invention the detection method of three flavor Lignum Santali Albi oral liquids, and described detection method comprises following major part:
1) Lignum Santali Albi, Semen Myristicae in the pharmaceutical preparation of the present invention are differentiated;
2) gallic acid of Fructus Choerospondiatis in the pharmaceutical preparation of the present invention, the content of protocatechuic acid are measured;
3) content of the volatile oil in Lignum Santali Albi, the Semen Myristicae in the pharmaceutical preparation of the present invention is measured.
Above-mentioned part concrete operations are as follows:
1) gets this product 100ml, water-bath is transferred in the separatory funnel after being concentrated into thick paste,, the solution after the extraction is poured into treat in the evaporating dish that solution evaporates into fully without ether and distinguish the flavor of to the complete layering of solution with extracted with diethyl ether, make dissolving to wherein adding chloroform 5ml again, as need testing solution.Other gets Semen Myristicae control medicinal material 10g, decocts with water 1h, filtered while hot, and filtrate is concentrated into thick paste, is made in the same way of control medicinal material solution.Draw each 15 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate take sodium carboxymethyl cellulose as binding agent, take chloroform-methanol (95:5) as developing solvent, launch, take out, dry, spray is with sulphuric acid-methanol (1:1) solution, 105 degrees centigrade of lower bakings 5 minutes, put under the uviol lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, the fluorescence speckle of aobvious same color.
2) get this product 30ml, 20ml extracts at twice with ether, merges ether solution, waves loose ether to 2ml, as need testing solution; Other gets the Lignum Santali Albi control medicinal material, presses determination of volatile oil Division A League Matches of French Football method (Chinese Pharmacopoeia version appendix in 2010 X D) and extracts volatile oil, adds diethyl ether and makes the solution that 1ml contains 0.1ml, in contrast medical material solution.Test according to thin layer chromatography (Chinese Pharmacopoeia version appendix in 2010 VI B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate take sodium carboxymethyl cellulose as binding agent, take petroleum ether (60～90 ℃)-normal hexane-Ethyl formate-formic acid (1:3:1.5:0.1) as developing solvent, launch, take out, dry, spray is with paradime thylaminobenzaldehyde solution, 80～90 ℃ of bakings 5 minutes.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, the speckle of aobvious same color.
3) assay of the present invention:
The mensuration of a protocatechuic acid
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filler; Methanol-water (containing 2.5% acetic acid) (10:90) is mobile phase, and the detection wavelength is 260nm.Number of theoretical plate calculates by the protocatechuic acid peak should be not less than 2500.
It is an amount of that the protocatechuic acid reference substance is got in the preparation of reference substance solution, accurately weighed, adds 70% dissolve with ethanol, makes the solution that every 1ml contains 0.1mg, and get final product.
This product 10.00ml is accurately measured in the preparation of need testing solution, and to evaporating dish, water bath method, residue add 70% dissolve with ethanol and be transferred in the 10ml measuring bottle, add 70% ethanol to scale, shakes up, and filters with microporous filter membrane (0.45 μ m), and get final product.
Algoscopy respectively precision is measured reference substance and each 10 μ l of need testing solution, and the injection liquid chromatography is measured, and be get final product.
Every of this product contains Fructus Choerospondiatis with protocatechuic acid (C
7H
6O
4), must not be less than 0.09mg.
The mensuration of b gallic acid
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filler; Methanol-0.2% aqueous formic acid (6:94) is mobile phase, and the detection wavelength is 270nm.Number of theoretical plate calculates by the gallic acid peak should be not less than 3000.
It is an amount of that the gallic acid reference substance is got in the preparation of reference substance solution, accurately weighed, adds 50% dissolve with methanol, makes the solution that every 1ml contains 0.1mg, and get final product.
This product 10.00ml is accurately measured in the preparation of need testing solution, and to evaporating dish, water bath method, residue add 50% dissolve with methanol and be transferred in the 10ml measuring bottle, add methanol to scale, shakes up, and filters with microporous filter membrane (0.45 μ m), and get final product.
Algoscopy respectively precision is measured reference substance and each 5 μ l of need testing solution, and the injection liquid chromatography is measured, and be get final product.
Every of this product contains Fructus Choerospondiatis with gallic acid (C
7H
8O
6), must not be less than 0.07mg.
4) determination of volatile oil:
Get three flavor Lignum Santali Albi sample 100ml(and be equivalent to approximately contain volatile oil 0.5～1.0ml), put in the flask, add water an amount of with bead number, after jolting mixes, connection volatile oil determination apparatus and reflux condensing tube.Autocondensation pipe upper end adds water makes the scale part that is full of volatile oil determination apparatus, and overflow when entering flask till.Put in the electric jacket or slowly be heated to other proper method and boil, and keep little and boiled about 5 hours, oil mass no longer increases to the determinator, stopped heating is placed a moment, opens the piston of determinator lower end, water is slowly emitted, above oil reservoir upper end arrives scale 0 line till the 5mm place.Place more than 1 hour, open again piston and make oil reservoir drop to its upper end just and scale.Line is concordant, reads the volatilization oil mass, and calculates the content (%) of volatile oil in the test sample.
Every of this product contains volatile oil must not be less than 0.05ml.
The invention provides Lignum Santali Albi, myristic thin layer chromatography and differentiate, selected effective ingredient protocatechuic acid in the Fructus Choerospondiatis and gallic acid as the assay index, set up volatile oil standard in the content assaying methods of three flavor Lignum Santali Albis and the three flavor Lignum Santali Albis; Passed through repeated experiment, confirmation method is easy, repeatability is good, can be used as the quality control index of three flavor Lignum Santali Albi oral liquids.
Three flavor Lignum Santali Albi oral liquids of the present invention can be determined usage and dosage according to patient's concrete condition in use.
Three flavor Lignum Santali Albi oral liquids of the present invention have the circulation of qi promoting warming middle-JIAO, and the therapeutic effect of appetizing pain relieving is used for QI stagnated by cold, chest pain, stomachache, stomachache lack of appetite; Coronary heart disease, angina pectoris.
Following examples are used for further specifying three flavor Lignum Santali Albi oral liquid preparation technologies' feasibility, and three flavor Lignum Santali Albi oral liquids of this explained hereafter are stable and controllable for quality.
The specific embodiment
The preparation method of 1: three flavor of specific embodiment Lignum Santali Albi oral liquid
Prescription: Lignum Santali Albi 130g Semen Myristicae 130g Fructus Choerospondiatis 130g
Method for making:
1, medical material pre-treatment: Lignum Santali Albi is dug into the wood shavings shape with electric planer, then pulverize with pulverizer, Semen Myristicae is pulverized (machine temperature can not be too high when noting pulverizing, to prevent the loss of volatile oil) with pulverizer, and the pulverizer that Fructus Choerospondiatis is used is pulverized.
2, the preparation of Fructus Choerospondiatis alcohol extract: get Fructus Choerospondiatis coarse powder 130g with 70%-80% alcohol reflux twice, 2.0h for the first time, 2.0h filters for the second time, and medicinal residues are for subsequent use, and Recycled ethanol gets concentrated medicament.
3, the extraction of Lignum Santali Albi and Semen Myristicae volatile oil: each 130g coarse powder of Lignum Santali Albi and Semen Myristicae mixes, and with steam method reflux, extract, volatile oil, tells volatile oil, and sealing is preserved, and medicinal residues are for subsequent use.
4, mix the preparation of medical material water cooking liquid: the medicinal residues of three flavor medical materials are mixed, and decocting in water filters, and merges medicinal liquid, hold over night is got supernatant, and is concentrated, leaves standstill room temperature, precipitate with ethanol (regulating the concentration 60% of precipitate with ethanol) stirs and left standstill 24 hours, filters, and decompression filtrate recycling ethanol gets concentrated solution.
5, batching: with the Fructus Choerospondiatis alcohol extract with merge with the decocting in water concentrated solution, adding distil water is to the about 800ml of volume, 4 ℃ of cold preservation 48 hours.It is 0.2% that room temperature board and frame machine sucking filtration, filtrate add sorbic acid to concentration, boil 15 minutes after, adding stevioside to concentration is 0.3%, boiled 1 minute, cool to room temperature, with the volatile oil that extracts and polysorbas20 with the 1:6 stirring and evenly mixing, slowly add into the liquid, stir, be settled to 1000ml with distilled water, fill, sterilization, and get final product.
The preparation method of 2: three flavors of specific embodiment Lignum Santali Albi oral liquid
Prescription: Lignum Santali Albi 130g Semen Myristicae 130g Fructus Choerospondiatis 130g
Method for making:
1, medical material pre-treatment: Lignum Santali Albi is dug into the wood shavings shape with electric planer, then pulverize with pulverizer, Semen Myristicae is pulverized (machine temperature can not be too high when noting pulverizing, to prevent the loss of volatile oil) with pulverizer, and Fructus Choerospondiatis is pulverized with pulverizer.
2, the preparation of Fructus Choerospondiatis alcohol extract: get Fructus Choerospondiatis coarse powder 130g 70%-80% ethanol percolation, soak 24h, with the speed of 3ml/kg/min percolation slowly, collect percolate, Recycled ethanol, being concentrated into proportion is 1.15(60 ℃), medicinal residues are for subsequent use.
3, the extraction of Lignum Santali Albi and Semen Myristicae volatile oil: each 130g coarse powder of Lignum Santali Albi and Semen Myristicae mixes, and with steam method reflux, extract, volatile oil, tells volatile oil, and sealing is preserved, and medicinal residues are for subsequent use.
4, mix the preparation of medical material water cooking liquid: the medicinal residues of three flavor medical materials are mixed, and decocting in water filters, and merges medicinal liquid, and hold over night is got supernatant, and is concentrated, leaves standstill room temperature, and precipitate with ethanol stirs and left standstill 24 hours, filters, and decompression filtrate recycling ethanol gets the decocting in water concentrated solution.
5, batching: with the Fructus Choerospondiatis alcohol extract with merge with the decocting in water concentrated solution, adding distil water is to the about 800ml of volume, 4 degrees centigrade of cold preservation 48 hours.Dosing is centrifugal through centrifuge, and it is 0.2% that the filtrate after centrifugal adds sorbic acid to concentration, after boiling 15 minutes, adding stevioside to concentration is 0.3%, boils 1 minute, the cooling room temperature, with the volatile oil that extracts and polysorbas20 with the 1:6 stirring and evenly mixing, add into the liquid, stirring, be settled to 1000ml with distilled water, fill, sterilization, and get final product.
By the following examples detection method of the present invention is done more detailed explanation, but not as restriction.
Embodiment 3: get the Fructus Choerospondiatis coarse powder with 70% alcohol reflux twice, filter, medicinal residues are for subsequent use, and Recycled ethanol gets medicinal liquid; Each coarse powder of Lignum Santali Albi and Semen Myristicae mixes, and with steam method reflux, extract, volatile oil, tells volatile oil, and sealing is preserved, and medicinal residues are for subsequent use.Medicinal residues are mixed, and decocting in water filters, and merges medicinal liquid, and hold over night is got supernatant, and is concentrated, leaves standstill room temperature, and precipitate with ethanol (regulating the concentration 60% of precipitate with ethanol) stirs, and leaves standstill 24 hours, filters, and decompression filtrate recycling ethanol gets the decocting in water concentrated solution.With the Fructus Choerospondiatis alcohol extract with merge with the decocting in water concentrated solution, adding distil water is to the about 800ml of volume, 4 ℃ of cold preservation 48 hours.Room temperature is filtered with board and frame machine, and it is 0.2% that filtrate adds sorbic acid to concentration, after boiling 15 minutes, adding stevioside to concentration is 0.3%, boils 1 minute, the cooling room temperature, with the volatile oil that extracts and polysorbas20 with the 1:6 stirring and evenly mixing, add into the liquid, stirring, be settled to 1000ml with distilled water, fill, sterilization, and get final product.
Prepare with method in batches, make altogether medicine and amount to 6 batches, be respectively: 20120809,20120827,20120918,20120926,20121011,20121029.
More than 6 batch detection methods comprise following methods:
1) gets this product 100ml, water-bath is transferred in the separatory funnel after being concentrated into thick paste,, the solution after the extraction is poured into treat in the evaporating dish that solution evaporates into fully without ether and distinguish the flavor of to the complete layering of solution with extracted with diethyl ether, make dissolving to wherein adding chloroform 5ml again, as need testing solution.Other gets Semen Myristicae control medicinal material 10g, decocts with water 1h, filtered while hot, and filtrate is concentrated into thick paste, is made in the same way of control medicinal material solution.Test according to thin layer chromatography (Chinese Pharmacopoeia version appendix in 2010 VI B), draw each 15 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate take sodium carboxymethyl cellulose as binding agent, take chloroform-methanol (95:5) as developing solvent, launch, take out, dry, spray, is put under the uviol lamp (365nm) and is inspected 105 degrees centigrade of lower bakings 5 minutes with sulphuric acid-methanol (1:1) solution.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, the fluorescence speckle of aobvious same color.
2) get this product 30ml, 20ml extracts at twice with ether, merges ether solution, waves loose ether to 2ml, as need testing solution.Other gets the Lignum Santali Albi control medicinal material, presses determination of volatile oil Division A League Matches of French Football method (Chinese Pharmacopoeia version appendix in 2010 X D) and extracts volatile oil, adds diethyl ether and makes the solution that 1ml contains 0.1ml, in contrast medical material solution.Test according to thin layer chromatography (Chinese Pharmacopoeia version appendix in 2010 VI B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate take sodium carboxymethyl cellulose as binding agent, take petroleum ether (60～90 ℃)-normal hexane-Ethyl formate-formic acid (1:3:1.5:0.1) as developing solvent, launch, take out, dry, spray is with paradime thylaminobenzaldehyde solution, 80～90 ℃ of bakings 5 minutes.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, the speckle of aobvious same color.
Assay of the present invention is one or both of following method:
Measure according to high performance liquid chromatography (Chinese Pharmacopoeia version appendix in 2010 VI D).
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filler; Methanol-water (containing 2.5% acetic acid) (10:90) is mobile phase, and the detection wavelength is 260nm.Number of theoretical plate calculates by the protocatechuic acid peak should be not less than 2500.
It is an amount of that the protocatechuic acid reference substance is got in the preparation of reference substance solution, accurately weighed, adds 70% dissolve with ethanol, makes the solution that every 1ml contains 0.1mg, and get final product.
This product 10.00ml is accurately measured in the preparation of need testing solution, and to evaporating dish, water bath method, residue add 70% dissolve with ethanol and be transferred in the 10ml measuring bottle, add 70% ethanol to scale, shakes up, and filters with microporous filter membrane (0.45 μ m), and get final product.
Algoscopy respectively precision is measured reference substance and each 10 μ l of need testing solution, and the injection liquid chromatography is measured, and be get final product.
Every of this product contains Fructus Choerospondiatis with protocatechuic acid (C
7H
6O
4), must not be less than 0.09mg.
2) measure according to high performance liquid chromatography (Chinese Pharmacopoeia version appendix in 2010 VI D).
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filler; Methanol-0.2% aqueous formic acid (6:94) is mobile phase, and the detection wavelength is 270nm.Number of theoretical plate calculates by the gallic acid peak should be not less than 3000.
It is an amount of that the gallic acid reference substance is got in the preparation of reference substance solution, accurately weighed, adds 50% dissolve with methanol, makes the solution that every 1ml contains 0.1mg, and get final product.
This product 10.00ml is accurately measured in the preparation of need testing solution, and to evaporating dish, water bath method, residue add 50% dissolve with methanol and be transferred in the 10ml measuring bottle, add methanol to scale, shakes up, and filters with microporous filter membrane (0.45 μ m), and get final product.
Algoscopy respectively precision is measured reference substance and each 5 μ l of need testing solution, and the injection liquid chromatography is measured, and be get final product.
Every of this product contains Fructus Choerospondiatis with gallic acid (C
7H
8O
6), must not be less than 0.07mg.
Every of this product contains volatile oil must not be less than 0.05ml.Drug detection the results are shown in Table 5:
The assay of 6 batches three flavors of table 5 Lignum Santali Albi oral liquid
Claims (10)
1. three flavor Lignum Santali Albi oral liquids with heat clearing away effect is characterized in that, are prepared from by three flavor raw material of Chinese medicine medicines of following proportioning: Lignum Santali Albi 100-300g, Semen Myristicae 100-300g, Fructus Choerospondiatis 100-300g;
Its preparation method is as follows:
A) reflux, extract, Fructus Choerospondiatis, merging filtrate, filtrate concentration and recovery ethanol;
B) steam method extracts Lignum Santali Albi, myristic volatile oil;
C) Lignum Santali Albi, Semen Myristicae, medicine made from Fructus choerospondiatis pulp water decoct 1 time, and filtrate is concentrated, precipitate with ethanol, concentration and recovery ethanol;
D) Fructus Choerospondiatis backflow concentrated solution and precipitate with ethanol concentrated solution merge, and adding distil water is an amount of, cold preservation 48 hours.Room temperature is with bacteriological filtration plate sucking filtration, and it is 0.2% that filtrate adds sorbic acid to concentration, boil 15 minutes after, adding stevioside to concentration is 0.3%, boils 1 minute, with the volatile oil and the tween 20 stirring and evenly mixing that extract, distilled water is settled to 1000ml, fill is sterilized.
2. oral liquid according to claim 1 is characterized in that, is prepared from by three flavor raw material of Chinese medicine medicines of following proportioning: Folium Ginkgo 130g, Radix Ginseng Rubra 130g, Radix Et Caulis Acanthopanacis Senticosi 130g.
3. oral liquid according to claim 1 is characterized in that, wherein Fructus Choerospondiatis adds 6 times of amount 70%-80% alcohol reflux 2 times; Wherein Lignum Santali Albi, Semen Myristicae are used first steam method reflux, extract, volatile oil, separate volatile oil, Lignum Santali Albi then, and Semen Myristicae and Fructus Choerospondiatis medicinal residues add 10 times of water gagings again and extract 1 time, extract 2 hours; Wherein the ratio of volatile oil and tween 20 is 1:5-1:6.
4. the preparation method of oral liquid according to claim 1 is characterized in that, step is as follows:
1) it is an amount of to get Fructus Choerospondiatis, is ground into coarse powder, takes by weighing 100-300g, with 6 times of amount 70-80% alcohol reflux 2 times, filters, and medicinal residues are for subsequent use, and Recycled ethanol gets medicinal liquid;
2) get Lignum Santali Albi and Semen Myristicae is an amount of, Lignum Santali Albi medical material wood shavings, Semen Myristicae powder is broken into coarse powder, respectively takes by weighing 100-300g, mixes, and with steam method reflux, extract, volatile oil, separates volatile oil, and sealing is preserved, and medicinal residues are for subsequent use;
3) medicinal residues with three flavor medical materials mix, and decocting in water 1 time filters, and the medicinal liquid hold over night is got supernatant, and is concentrated, places room temperature, and the 50-70% concentration of alcohol stirs precipitate with ethanol, leaves standstill 24-48 hour, filters, and decompression filtrate recycling ethanol gets concentrated solution;
4) with the Fructus Choerospondiatis alcohol extract with merge with the precipitate with ethanol concentrated solution, adding distil water is to the about 1000ml of volume, 4 ℃ of cold preservation 48 hours, room temperature is with bacteriological filtration plate sucking filtration, and it is 0.2% that filtrate adds sorbic acid to concentration, boil 15 minutes after, adding stevioside to concentration is 0.3%, boiled 1 minute, with the volatile oil that extracts and tween 20 with the 1:5-1:6 stirring and evenly mixing, slowly add into the liquid (70 ℃), strong agitation is settled to 1000ml with distilled water, fill, sterilization, and get final product.
5. the preparation method of oral liquid according to claim 1 is characterized in that, step is as follows:
1) it is an amount of to get Fructus Choerospondiatis, is ground into coarse powder, takes by weighing 130g, with 6 times of amount 70-80% alcohol reflux 2 times, filters, and medicinal residues are for subsequent use, and Recycled ethanol gets medicinal liquid;
2) get Lignum Santali Albi and Semen Myristicae is an amount of, Lignum Santali Albi medical material wood shavings, Semen Myristicae powder is broken into coarse powder, respectively takes by weighing 130g, mixes, and with steam method reflux, extract, volatile oil 3h, separates volatile oil, and sealing is preserved, and medicinal residues are for subsequent use;
3) medicinal residues with three flavor medical materials mix, and 10 times of water gagings boil 1 time, filter, and the medicinal liquid hold over night is got supernatant, and are concentrated, place room temperature, and 60% concentration of alcohol stirs precipitate with ethanol, leave standstill 24 hours, filter, and decompression filtrate recycling ethanol gets concentrated solution;
4) with the Fructus Choerospondiatis alcohol extract with merge with the precipitate with ethanol concentrated solution, adding distil water is to the about 1000ml of volume, 4 ℃ of cold preservation 48 hours, room temperature is with bacteriological filtration plate sucking filtration, and it is 0.2% that filtrate adds sorbic acid to concentration, boil 15 minutes after, adding stevioside to concentration is 0.3%, boiled 1 minute, with the volatile oil that extracts and tween 20 with the 1:5-1:6 stirring and evenly mixing, slowly add into the liquid (70 ℃), strong agitation is settled to 1000ml with distilled water, fill, sterilization, and get final product.
6. the detection method of the described three flavor Lignum Santali Albi oral liquids of claim 1 is characterized in that comprising Lignum Santali Albi, Semen Myristicae in the preparation is differentiated; The gallic acid of Fructus Choerospondiatis in the preparation, the content of protocatechuic acid are measured; Content to the volatile oil in Lignum Santali Albi, the Semen Myristicae in the preparation is measured.
7. detection method according to claim 6 is characterized in that, wherein Lignum Santali Albi, Semen Myristicae in the preparation is differentiated that step is as follows:
The Semen Myristicae thin layer chromatography is differentiated and is got three flavor Lignum Santali Albi oral liquid 100ml, water-bath is transferred in the separatory funnel after being concentrated into thick paste, with extracted with diethyl ether to the complete layering of solution, solution after the extraction poured into treat in the evaporating dish that solution evaporates into fully without ether and distinguish the flavor of, make dissolving to wherein adding chloroform 5ml again, as need testing solution.Other gets Semen Myristicae control medicinal material 10g, decocts with water 1h, filtered while hot, and filtrate is concentrated into thick paste, is made in the same way of control medicinal material solution.Draw each 15 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate take sodium carboxymethyl cellulose as binding agent, take chloroform-methanol (95:5) as developing solvent, launch, take out, dry, spray is with sulphuric acid-methanol (1:1) solution, 105 degrees centigrade of lower bakings 5 minutes, put under the uviol lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, the fluorescence speckle of aobvious same color;
The Lignum Santali Albi thin layer chromatography differentiates and gets three flavor Lignum Santali Albi oral liquid 30ml that 20ml extracts at twice with ether, merges ether solution, waves loose ether to 2ml, as need testing solution; Other gets the Lignum Santali Albi control medicinal material, presses determination of volatile oil Division A League Matches of French Football method (Chinese Pharmacopoeia version appendix in 2010 X D) and extracts volatile oil, adds diethyl ether and makes the solution that 1ml contains 0.1ml, in contrast medical material solution.Test according to thin layer chromatography (Chinese Pharmacopoeia version appendix in 2010 VI B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate take sodium carboxymethyl cellulose as binding agent, take petroleum ether (60～90 ℃)-normal hexane-Ethyl formate-formic acid (1:3:1.5:0.1) as developing solvent, launch, take out, dry, spray is with paradime thylaminobenzaldehyde solution, 80～90 ℃ of bakings 5 minutes.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, the speckle of aobvious same color.
8. detection method according to claim 6 is characterized in that, wherein the gallic acid of Fructus Choerospondiatis in the preparation, the content of protocatechuic acid is measured, and step is as follows:
The assay of protocatechuic acid
Be filler with octadecylsilane chemically bonded silica; Methanol-water (containing 2.5% acetic acid) (10:90) is mobile phase, and the detection wavelength is 260nm.Number of theoretical plate calculates by the protocatechuic acid peak should be not less than 2500;
It is an amount of that the protocatechuic acid reference substance is got in the preparation of reference substance solution, accurately weighed, adds 70% dissolve with ethanol, makes the solution that every 1ml contains 0.1mg, and get final product;
Three flavor Lignum Santali Albi oral liquid 10.00ml are accurately measured in the preparation of need testing solution, and to evaporating dish, water bath method, residue add 70% dissolve with ethanol and be transferred in the 10ml measuring bottle, add 70% ethanol to scale, shake up, and filter with microporous filter membrane (0.45 μ m), and get final product;
Algoscopy respectively precision is measured reference substance and each 10 μ l of need testing solution, and the injection liquid chromatography is measured, and be get final product;
The assay of gallic acid
Be filler with octadecylsilane chemically bonded silica; Methanol-0.2% aqueous formic acid (6:94) is mobile phase, and the detection wavelength is 270nm.Number of theoretical plate calculates by the gallic acid peak should be not less than 3000;
It is an amount of that the gallic acid reference substance is got in the preparation of reference substance solution, accurately weighed, adds 50% dissolve with methanol, makes the solution that every 1ml contains 0.1mg, and get final product;
Three flavor Lignum Santali Albi oral liquid 10.00ml are accurately measured in the preparation of need testing solution, and to evaporating dish, water bath method, residue add 50% dissolve with methanol and be transferred in the 10ml measuring bottle, add methanol to scale, shake up, and filter with microporous filter membrane (0.45 μ m), and get final product;
Algoscopy respectively precision is measured reference substance and each 5 μ l of need testing solution, and the injection liquid chromatography is measured, and be get final product.
9. detection method according to claim 6 is characterized in that, wherein the content of the volatile oil in Lignum Santali Albi, the Semen Myristicae in the preparation is measured, and step is as follows:
The assay of volatile oil
Get three flavor Lignum Santali Albi oral liquid 100ml(and be equivalent to approximately contain volatile oil 0.5～1.0ml), put in the flask, add water an amount of with bead number, after jolting mixes, connection volatile oil determination apparatus and reflux condensing tube.Autocondensation pipe upper end adds water makes the scale part that is full of volatile oil determination apparatus, and overflow when entering flask till.Put in the electric jacket or slowly be heated to other proper method and boil, and keep little and boiled about 5 hours, oil mass no longer increases to the determinator, stopped heating is placed a moment, opens the piston of determinator lower end, water is slowly emitted, above oil reservoir upper end arrives scale 0 line till the 5mm place.Place more than 1 hour, open again piston and make oil reservoir drop to its upper end just and scale.Line is concordant, reads the volatilization oil mass, and calculates the content of volatile oil in the test sample.
10. detection method according to claim 6 is characterized in that, step is as follows:
A) the Semen Myristicae thin layer chromatography is differentiated and is got three flavor Lignum Santali Albi oral liquid 100ml, water-bath is transferred in the separatory funnel after being concentrated into thick paste, with extracted with diethyl ether to the complete layering of solution, solution after the extraction poured into treat in the evaporating dish that solution evaporates into fully without ether and distinguish the flavor of, make dissolving to wherein adding chloroform 5ml again, as need testing solution.Other gets Semen Myristicae control medicinal material 10g, decocts with water 1h, filtered while hot, and filtrate is concentrated into thick paste, is made in the same way of control medicinal material solution.Draw each 15 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate take sodium carboxymethyl cellulose as binding agent, take chloroform-methanol (95:5) as developing solvent, launch, take out, dry, spray is with sulphuric acid-methanol (1:1) solution, 105 degrees centigrade of lower bakings 5 minutes, put under the uviol lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, the fluorescence speckle of aobvious same color;
B) the Lignum Santali Albi thin layer chromatography is differentiated and is got three flavor Lignum Santali Albi oral liquid 30ml, and 20ml extracts at twice with ether, merges ether solution, waves loose ether to 2ml, as need testing solution; Other gets the Lignum Santali Albi control medicinal material, presses determination of volatile oil Division A League Matches of French Football method (Chinese Pharmacopoeia version appendix in 2010 X D) and extracts volatile oil, adds diethyl ether and makes the solution that 1ml contains 0.1ml, in contrast medical material solution.Test according to thin layer chromatography (Chinese Pharmacopoeia version appendix in 2010 VI B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate take sodium carboxymethyl cellulose as binding agent, take petroleum ether (60～90 ℃)-normal hexane-Ethyl formate-formic acid (1:3:1.5:0.1) as developing solvent, launch, take out, dry, spray is with paradime thylaminobenzaldehyde solution, 80～90 ℃ of bakings 5 minutes.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, the speckle of aobvious same color;
C) assay of protocatechuic acid
Be filler with octadecylsilane chemically bonded silica; Methanol-water (containing 2.5% acetic acid) (10:90) is mobile phase, and the detection wavelength is 260nm.Number of theoretical plate calculates by the protocatechuic acid peak should be not less than 2500;
It is an amount of that the protocatechuic acid reference substance is got in the preparation of reference substance solution, accurately weighed, adds 70% dissolve with ethanol, makes the solution that every 1ml contains 0.1mg, and get final product;
Three flavor Lignum Santali Albi oral liquid 10.00ml are accurately measured in the preparation of need testing solution, and to evaporating dish, water bath method, residue add 70% dissolve with ethanol and be transferred in the 10ml measuring bottle, add 70% ethanol to scale, shake up, and filter with microporous filter membrane (0.45 μ m), and get final product;
Algoscopy respectively precision is measured reference substance and each 10 μ l of need testing solution, and the injection liquid chromatography is measured, and be get final product;
D) assay of gallic acid
Be filler with octadecylsilane chemically bonded silica; Methanol-0.2% aqueous formic acid (6:94) is mobile phase, and the detection wavelength is 270nm.Number of theoretical plate calculates by the gallic acid peak should be not less than 3000;
It is an amount of that the gallic acid reference substance is got in the preparation of reference substance solution, accurately weighed, adds 50% dissolve with methanol, makes the solution that every 1ml contains 0.1mg, and get final product;
Three flavor Lignum Santali Albi oral liquid 10.00ml are accurately measured in the preparation of need testing solution, and to evaporating dish, water bath method, residue add 50% dissolve with methanol and be transferred in the 10ml measuring bottle, add methanol to scale, shake up, and filter with microporous filter membrane (0.45 μ m), and get final product;
Algoscopy respectively precision is measured reference substance and each 5 μ l of need testing solution, and the injection liquid chromatography is measured, and be get final product;
E) assay of volatile oil
Get three flavor Lignum Santali Albi oral liquid 100ml(and be equivalent to approximately contain volatile oil 0.5～1.0ml), put in the flask, add water an amount of with bead number, after jolting mixes, connection volatile oil determination apparatus and reflux condensing tube.Autocondensation pipe upper end adds water makes the scale part that is full of volatile oil determination apparatus, and overflow when entering flask till.Put in the electric jacket or slowly be heated to other proper method and boil, and keep little and boiled about 5 hours, oil mass no longer increases to the determinator, stopped heating is placed a moment, opens the piston of determinator lower end, water is slowly emitted, above oil reservoir upper end arrives scale 0 line till the 5mm place.Place more than 1 hour, open again piston and make oil reservoir drop to its upper end just and scale.Line is concordant, reads the volatilization oil mass, and calculates the content of volatile oil in the test sample.
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| CN106937962A (en) * | 2017-03-29 | 2017-07-11 | 青海大学 | A kind of three-flavor sandalwood dissipates preparation and the medical usage of total volatile oil |
| CN111579737A (en) * | 2020-06-23 | 2020-08-25 | 内蒙古凯蒙药业有限公司 | Medicine for treating heart disease and detection method |
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| CN106727951B (en) * | 2016-12-29 | 2020-06-23 | 贵阳中医学院第二附属医院 | Medicine for protecting arteriovenous internal fistula and preparation method thereof |
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| CN102370677A (en) * | 2010-08-26 | 2012-03-14 | 江西济民可信集团有限公司 | Three-flavor sandalwood preparation and preparation method thereof |
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| CN106937962A (en) * | 2017-03-29 | 2017-07-11 | 青海大学 | A kind of three-flavor sandalwood dissipates preparation and the medical usage of total volatile oil |
| CN111579737A (en) * | 2020-06-23 | 2020-08-25 | 内蒙古凯蒙药业有限公司 | Medicine for treating heart disease and detection method |
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