CN102078380A - Laxative traditional Chinese medicine capsule preparation as well as preparation method and detection method thereof - Google Patents
Laxative traditional Chinese medicine capsule preparation as well as preparation method and detection method thereof Download PDFInfo
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- CN102078380A CN102078380A CN200910207487XA CN200910207487A CN102078380A CN 102078380 A CN102078380 A CN 102078380A CN 200910207487X A CN200910207487X A CN 200910207487XA CN 200910207487 A CN200910207487 A CN 200910207487A CN 102078380 A CN102078380 A CN 102078380A
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Abstract
The invention provides a laxative traditional Chinese medicine capsule preparation as well as a preparation method and a detection method thereof. The preferential formulation of the laxative traditional Chinese medicine preparation is granule preferably, the laxative traditional Chinese medicine preparation is prepared from senna leaf, Chinese angelica and desertliving cistanche based on the mixture ratio in parts by weight of 8:1:1, and the content of aloe-emodin in the preparation is above 0.13mg/g. The senna leaf and Chinese angelica in the laxative traditional Chinese medicine preparation are identified by thin-layer chromatography. The content of the aloe-emodin which is an active ingredient in the preparation is measured by high performance liquid chromatography. The detection method provided by the invention can be applied in the treatment of hot junction constipation, constipation caused by long-term bed rest, temporary abdominal distentien and constipation and senile habitual constipation.
Description
Technical field
The present invention relates to field of traditional Chinese, particularly, the present invention relates to relieving constipation Chinese medicine preparation, its preparation method and detection method.
Background technology
Tongbianling preparation is to be principal agent with traditional relieving constipation Chinese medicine Folium Sennae, is equipped with the modern preparation that Herba Cistanches, Radix Angelicae Sinensis are made, and has the effect of the intestinal stasis relieving that purges heat, loosening bowel to relieve constipation.The clinical constipation with heat retention that is used for, long-term bed constipation, momentary abdominal distention constipation, senility habitual constipation.
TONGBIAN LING listing kind has capsule, medicinal tea etc.The TONGBIAN LING capsule records in the 7th in the Sanitation Ministry medicine standard Chinese traditional patent formulation preparation, standard numbering: WS
3-B-1420-93.TONGBIAN LING tea records in national standard for traditional Chinese medicines compilation Chinese patent medicine provincial standard rising national standard part internal medicine taste fascicle, standard numbering: WS-11145 (ZD-1145)-2002.
Summary of the invention
Therefore, the purpose of this invention is to provide a kind of relieving constipation Chinese medicinal capsule preparation.Another object of the present invention provides the preparation method of above-mentioned relieving constipation Chinese medicinal capsule preparation.Another purpose of the present invention provides the detection method of above-mentioned relieving constipation Chinese medicinal capsule preparation.A further object of the present invention provides the purposes of above-mentioned relieving constipation Chinese medicinal capsule preparation in treatment constipation with heat retention, long-term bed constipation, momentary abdominal distention constipation and senility habitual constipation.
The objective of the invention is to realize by the following technical solutions.On the one hand, the invention provides a kind of relieving constipation Chinese medicinal capsule preparation, this capsule preparations with Folium Sennae, Radix Angelicae Sinensis and Herba Cistanches be raw medicinal material by weight proportioning make at 8: 1: 1, the content of aloe-emodin is greater than 0.13mg/g in this capsule preparations, be preferably 0.13-0.60mg/g, more preferably 0.14-0.42mg/g.
Preferably, the preparation of this capsule preparations comprises that with Folium Sennae, Radix Angelicae Sinensis and Herba Cistanches decocting after-filtration filtrate is concentrated into the thick paste that relative density is 1.25-1.42, and described relative density is preferably 1.25-1.40, more preferably 1.30-1.40.
On the other hand, the invention provides the method for the above-mentioned relieving constipation Chinese medicinal capsule preparation of preparation, this method comprises the steps: Folium Sennae, Radix Angelicae Sinensis and Herba Cistanches decocting after-filtration, filtrate is concentrated into the thick paste that relative density is 1.25-1.42, described relative density is preferably 1.25-1.40, more preferably 1.30-1.40;
Wherein, the content of aloe-emodin is preferably 0.13-0.60mg/g greater than 0.13mg/g in the capsule preparations that makes, more preferably 0.14-0.42mg/g.
Preferably, described preparation method comprises the steps:
(1) Radix Angelicae Sinensis, Herba Cistanches two flavors are decocted with water, add the Folium Sennae of not pulverizing and decoct again, filter;
(2) filtrate that step (1) is obtained is condensed into the thick paste that relative density is 1.25～1.40 (25 ℃), adds the Senna Leaf after pulverizing, and mixing is granulated, and drying is sieved, mixing, promptly;
The wherein said Folium Sennae of not pulverizing and the parts by weight proportioning of the Senna Leaf after the described pulverizing are 3: 1～4: 1; Described relative density is preferably 1.25-1.40, more preferably 1.30-1.40.
Another aspect the invention provides the detection method of described relieving constipation Chinese medicinal capsule preparation, and this method comprises that following employing thin layer chromatography detects the step of Folium Sennae:
(1) preparation need testing solution: get described relieving constipation Chinese medicine preparation 1g, porphyrize adds 10% potassium hydroxide-ethanol solution 50ml, boiled 2 minutes, add water 10ml, filter, filtrate adds hydrochloric acid, and to transfer to pH value be 2～3, put and steam in the water-bath to there not being the alcohol flavor, extract with ether 10ml jolting, divide and get ether layer, volatilize, residue adds ethanol 0.5ml makes dissolving, gets supernatant as need testing solution;
(2) preparation control medicinal material solution: get Folium Sennae control medicinal material 0.5g, make control medicinal material solution according to the described method of step (1);
(3) adopt thin layer chromatography to differentiate Folium Sennae: to draw each 5 μ l of two kinds of solution that step (1) and step (2) are obtained, put respectively on same silica gel g thin-layer plate, upper solution with normal propyl alcohol-ethyl acetate-water (3: 4: 3) is developing solvent, launch, take out, dry, it is smoked clear to the speckle colour developing to put in the ammonia.
Preferably, described detection method comprises that following employing thin layer chromatography detects the step of Radix Angelicae Sinensis:
(1) preparation need testing solution: get described relieving constipation Chinese medicine preparation 5g, add active carbon powder 5g, the 50ml that adds methylene chloride, supersound process 15 minutes is put coldly, filters, and filtrate low temperature evaporate to dryness, residue add dehydrated alcohol 0.5ml makes dissolving, as need testing solution;
(2) preparation control medicinal material solution: get Radix Angelicae Sinensis control medicinal material 0.5g, make control medicinal material solution according to the described method of step (1);
(3) adopt thin layer chromatography to differentiate Radix Angelicae Sinensis: draw need testing solution 2～20 μ l, control medicinal material solution 2 μ l put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate (9: 1) is developing solvent, launches, and takes out, dry, put under the ultra-violet lamp 365nm and inspect.
Another aspect the invention provides the detection method of described relieving constipation Chinese medicinal capsule preparation, and this method comprises the content that adopts high performance liquid chromatography to measure aloe-emodin in the described capsule preparations.
Preferably, the preparation method of described need testing solution comprises the steps: to get preparation 1g, and accurate the title decides, put in the conical flask, the accurate methanol 50ml that adds claims to decide weight, supersound process 30 minutes is put coldly, supplies the weight that subtracts mistake with methanol, filter, precision is measured subsequent filtrate 15ml, puts in the conical flask, evaporate to dryness, residue add 8% hydrochloric acid solution 30ml, add chloroform 30ml, water-bath refluxed 1 hour, cooling is immediately shifted and is put in the separatory funnel, divides and gets the chloroform layer, the jolting of sour water layer reuse chloroform is extracted 3 times, each 20ml merges chloroform liquid, evaporate to dryness, residue adds methanol makes dissolving, be transferred in the 10ml measuring bottle, add methanol constant volume, shake up to scale, filter, get subsequent filtrate.
Preferably, it is an amount of that the preparation method of described reference substance solution comprises the steps: to get the aloe-emodin reference substance, and accurate the title decides, and adds mobile phase and makes the solution that every 1ml contains 15 μ g.
Preferably, the chromatographic condition in the described detection method is: filler is the 18 alkyl silica gel bonded silica gel; Mobile phase is methanol-0.3% phosphoric acid solution (60: 40); The detection wavelength is 254nm.
Preferably, the aloe-emodine content scope that described method is measured is that every gram granule contains aloe-emodin 0.077mg at least, and preferably, the aloe-emodine content scope that described method is measured is that every gram granule contains aloe-emodin 0.15mg at least.
Again on the one hand, the invention provides described relieving constipation Chinese medicinal capsule preparation and be used for the treatment of purposes in constipation with heat retention, long-term bed constipation, momentary abdominal distention constipation and the senility habitual constipation.
Below will be described in detail the present invention, according to one embodiment of the invention, relieving constipation Chinese medicine preparation of the present invention is a hard capsule, and content is powder and the granule of yellow green to pitchy; Feeble QI, mildly bitter flavor, salty.
In one embodiment, prescription of the present invention is Folium Sennae 1200g, Radix Angelicae Sinensis 150g and Herba Cistanches 150g, and preparation method provided by the invention is specific as follows:
(1) above three flavors are got Radix Angelicae Sinensis 75g and are ground into fine powder; Two flavors such as remaining Radix Angelicae Sinensis and all the other Folium Sennae decoct with water 1.5 hours, filter, and filtrate is condensed into the thick paste that relative density is 1.25～1.30 (25 ℃), adds Chinese Angelica Root, mixing, cold drying is pulverized, and sieves, mixing incapsulates, and makes 1000 (granules), promptly.
Or:
(2) above three flavors are got Folium Sennae 330g and are ground into fine powder; Radix Angelicae Sinensis, Herba Cistanches two flavors decoct with water 0.5 hour, add remaining Folium Sennae and decoct 0.5 hour again, filter, filtrate is condensed into the thick paste that relative density is 1.30～1.40 (25 ℃), add Senna Leaf, mixing is granulated, dry, sieve, mixing incapsulates, make 1000 (big grains), promptly.
The present invention has improved the discrimination method of relieving constipation Chinese medicine preparation prescription composition, and is specific as follows:
(1) adopt thin layer chromatography to differentiate that the step of Folium Sennae is as follows: get this product content 1g, porphyrize adds 10% potassium hydroxide-ethanol solution 50ml, boiled 2 minutes, add water 10ml, filter, filtrate adds hydrochloric acid and transfers to acidity (pH2～3), put and steam in the water-bath to there not being the alcohol flavor, extract with ether 10ml jolting, divide and get ether layer, volatilize, residue adds ethanol 0.5ml makes dissolving, gets supernatant as need testing solution.Other gets Folium Sennae control medicinal material 0.5g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, upper solution with normal propyl alcohol-ethyl acetate-water (3: 4: 3) is developing solvent, launch, take out, dry, it is smoked clear to the speckle colour developing to put in the ammonia.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(2) adopt thin layer chromatography to differentiate that the step of Radix Angelicae Sinensis is as follows: get this product content 5g, add active carbon powder 5g, 50ml adds methylene chloride, supersound process 15 minutes is put coldly, filters, filtrate low temperature evaporate to dryness, residue add dehydrated alcohol 0.5ml makes dissolving, as need testing solution.Other gets Radix Angelicae Sinensis control medicinal material 0.5g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution (granule) 2 μ l, need testing solution (big grain) 20 μ l, control medicinal material solution 2 μ l, put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate (9: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
In addition, the present invention also determines the detection method and the controlling index of product active ingredient, and is specific as follows
Measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability test are filler with the 18 alkyl silica gel bonded silica gel; With methanol-0.3% phosphoric acid solution (60: 40) is mobile phase; The detection wavelength is 254nm.Number of theoretical plate calculates by the aloe-emodin peak should be not less than 4000.
The preparation of reference substance solution: it is an amount of to get the aloe-emodin reference substance, and accurate the title decides, and adds mobile phase and makes the solution that every 1ml contains 15 μ g, promptly.
The preparation of need testing solution: get 10 of this product, the accurate title, decide, and gets 1g, the accurate title, decide, and puts in the conical flask, the accurate methanol 50ml that adds, claim to decide weight, and supersound process 30 minutes (300W, 40kHz), put coldly, supply the weight that subtracts mistake, filter with methanol, precision is measured subsequent filtrate 15ml, puts in the conical flask evaporate to dryness, residue adds 8% hydrochloric acid solution 30ml, adds chloroform 30ml, and water-bath refluxed 1 hour, cooling is immediately shifted and is put in the separatory funnel, divides and gets the chloroform layer, the jolting of sour water layer reuse chloroform is extracted 3 times, and each 20ml merges chloroform liquid, evaporate to dryness, residue adds methanol makes dissolving, is transferred in the 10ml measuring bottle, adds methanol constant volume to scale, shake up, filter, get subsequent filtrate, promptly.
Algoscopy: the accurate respectively reference substance solution 10 μ l that draw, need testing solution 10～20 μ l inject chromatograph of liquid, measure, promptly.
Every dress of this product 0.25g (granule); (0.48g big grain), every contains Folium Sennae with aloe-emodin (C
15H
10O
5) meter, granule must not be less than 0.077mg; Big grain must not be less than 0.15mg.
Description of drawings
Below, describe embodiment of the present invention in conjunction with the accompanying drawings in detail, wherein:
Fig. 1 differentiates figure for the Folium Sennae thin layer chromatography, and wherein 1-3 is the relieving constipation Chinese medicine preparation of different batches, and 4 is the Folium Sennae control medicinal material, and 5 is the Folium Sennae negative control;
Fig. 2 differentiates figure for the Radix Angelicae Sinensis thin layer chromatography, and wherein 1-3 is the relieving constipation Chinese medicine preparation of different batches, and 4 is the Radix Angelicae Sinensis control medicinal material, and 5 is the Radix Angelicae Sinensis negative control;
Fig. 3 A and Fig. 3 B are 10 batches of thin-layer chromatograms for Radix Angelicae Sinensis in the test agent, and wherein 1-10 is for supplying test agent, and 11 is the Radix Angelicae Sinensis control medicinal material, and 12 is the Radix Angelicae Sinensis negative control;
Fig. 4 A to Fig. 4 C is the thin-layer chromatogram of the Radix Angelicae Sinensis on the different lamellaes, and wherein Fig. 4 A is the Merck precoated plate; Fig. 4 B is that Yantai Chemical Industry Research Inst. produces precoated plate; Fig. 4 C is hands shop silica gel G-CMC-Na plate;
Fig. 5 A and Fig. 5 B are the thin-layer chromatogram of the Radix Angelicae Sinensis under the different temperatures, and wherein Fig. 5 A represents that temperature is 10 ℃, and Fig. 5 B represents that temperature is 30 ℃;
Fig. 6 A and Fig. 6 B are the thin-layer chromatogram of the Radix Angelicae Sinensis under the different humidity, and wherein Fig. 6 A represents that temperature is 10 ℃, and humidity is 25%; Fig. 6 B represents that temperature is 30 ℃, and humidity is 75%;
Fig. 7 A-7D is the thin-layer chromatogram that employing method one is differentiated Herba Cistanches among the embodiment 2, and 1,5 are Herba Cistanches negative control product among Fig. 7 A, and 2,4 are the relieving constipation Chinese medicine preparation, and 3 is the betanin reference substance; Among Fig. 7 B, 1,6 are Herba Cistanches negative control product, and 2,4,5 are the relieving constipation Chinese medicine preparation, and 3 is the betanin reference substance; Among Fig. 7 C, 1,5 are Herba Cistanches negative control product, and 2,4 are the relieving constipation Chinese medicine preparation, and 3 is the betanin reference substance; Among Fig. 7 D, 1-3 is the relieving constipation Chinese medicine preparation, and 4 is the betanin reference substance;
Fig. 8 adopts method two to differentiate the thin-layer chromatogram of Herba Cistanches among the embodiment 2, wherein 1,5 are Herba Cistanches negative control product, and 2,4 are the relieving constipation Chinese medicine preparation, and 3 is the betanin reference substance;
Fig. 9 is aloe-emodin UV scanning figure;
Figure 10 A-10D is respectively the chromatogram of TONGBIAN LING capsule Folium Sennae feminine gender, aloe-emodin reference substance, TONGBIAN LING capsule (granule), TONGBIAN LING capsule (big grain);
Figure 11 is the aloe-emodin linear relationship chart.
The specific embodiment
Followingly the present invention is described with reference to specific embodiment.It will be appreciated by those skilled in the art that these embodiment only are used to illustrate the present invention, the scope that it does not limit the present invention in any way.
The preparation method of embodiment 1 relieving constipation Chinese medicine preparation
The preparation method of relieving constipation Chinese medicine preparation of the present invention is as follows: prescription of the present invention is Folium Sennae 1200g, Radix Angelicae Sinensis 150g and Herba Cistanches 150g, more than three the flavor, get Radix Angelicae Sinensis 75g and be ground into fine powder; Two flavors such as remaining Radix Angelicae Sinensis and all the other Folium Sennae decoct with water 1.5 hours, filter, and filtrate is condensed into the thick paste that relative density is 1.25～1.30 (25 ℃), adds Chinese Angelica Root, mixing, cold drying is pulverized, and sieves, mixing incapsulates, and makes 1000 (granules), promptly.
The relieving constipation Chinese medicine preparation that more than makes is a hard capsule, and content is powder and the granule of yellow green to pitchy; Feeble QI, mildly bitter flavor, one-tenth, every dress 0.25g (granule), every contains Folium Sennae with aloe-emodin (C
15H
10O
5) meter, must not be less than 0.077mg.
The preparation method of embodiment 2 relieving constipation Chinese medicine preparation
The preparation method of relieving constipation Chinese medicine preparation of the present invention is as follows: prescription of the present invention is Folium Sennae 1200g, Radix Angelicae Sinensis 150g and Herba Cistanches 150g, more than three the flavor, get Folium Sennae 330g and be ground into fine powder; Radix Angelicae Sinensis, Herba Cistanches two flavors decoct with water 0.5 hour, add remaining Folium Sennae and decoct 0.5 hour again, filter, filtrate is condensed into the thick paste that relative density is 1.30～1.40 (25 ℃), add Senna Leaf, mixing is granulated, dry, sieve, mixing incapsulates, make 1000 (big grains), promptly.
The relieving constipation Chinese medicine preparation that more than makes is a hard capsule, and content is powder and the granule of yellow green to pitchy; Feeble QI, mildly bitter flavor, one-tenth, every dress 0.48g (big grain), every contains Folium Sennae with aloe-emodin (C
15H
10O
5) meter, must not be less than 0.15mg.
The discrimination method of embodiment 3 relieving constipation Chinese medicine preparation
Present embodiment is the thin layer chromatography discrimination method of each component of relieving constipation Chinese medicine preparation provided by the present invention.
1, the thin layer chromatography of Folium Sennae is differentiated
This method with the Folium Sennae control medicinal material serve as the contrast differentiate, empirical tests with check, this method basic feasible solution specifies as follows:
(1) reagent and reagent
Negative sample: prepare according to method for making by TONGBIAN LING capsule prescription (lacking Folium Sennae), promptly.
The Folium Sennae control medicinal material: lot number is 996-9401, purchases in Nat'l Pharmaceutical ﹠ Biological Products Control Institute
Lamellae: silica gel G plate, from making sheet (Haiyang Chemical Plant, Qingdao), Merck plate (Germany), thin layer chromatography is used.
Other reagent is analytical pure
(2) experimentation
The need testing solution preparation: get this product content 1g, porphyrize adds 10% potassium hydroxide-ethanol solution 50ml, boiled 2 minutes, add water 10ml, filter, filtrate adds hydrochloric acid and transfers to acidity (pH2～3), put and steam in the water-bath to there not being the alcohol flavor, extract with ether 10ml jolting, divide and get ether layer, volatilize, residue adds ethanol 0.5ml makes dissolving, gets supernatant as need testing solution.
Folium Sennae control medicinal material formulations prepared from solutions: other gets Folium Sennae control medicinal material 0.5g, shines medical material solution in pairs with legal system.
Folium Sennae negative control solution preparation: get the Folium Sennae negative sample, make the Folium Sennae negative control solution by the preparation method of need testing solution.
Lamellae: adopt the self-control silica gel g thin-layer plate.
Point sample amount: draw each 5 μ l of above-mentioned three kinds of solution
Point sample mode: spot application
Developing solvent: normal propyl alcohol-ethyl acetate-water (3: 4: 3)
Exhibition distance: 8cm
Colour developing and inspecting: dry, put in the ammonia smokedly, under daylight, inspect to clear spot.
Experimental situation: temperature: 10 ℃ of relative humiditys: 56%
Experimental result shows, on sample and the Folium Sennae control medicinal material chromatograph relevant position tangible corresponding speckle arranged, and negative noiseless (see figure 1), the method can be used as the specificity of Folium Sennae and differentiate.
2, the thin layer chromatography of Radix Angelicae Sinensis is differentiated
This method with the Radix Angelicae Sinensis control medicinal material serve as the contrast differentiate, empirical tests with check, this method is feasible, specifies as follows:
(1) reagent and reagent
Negative sample: by TONGBIAN LING capsule prescription, preparation lacks the negative sample of Radix Angelicae Sinensis.
The Radix Angelicae Sinensis control medicinal material: lot number is 120927-200512, purchases in Nat'l Pharmaceutical ﹠ Biological Products Control Institute
Silica gel G plate: self-control silica gel g thin-layer plate
Reagent is analytical pure
(2) experimentation
The preparation of need testing solution: get this product content 5g, add active carbon powder 5g, the 50ml that adds methylene chloride, supersound process 15 minutes is put coldly, filters, and filtrate low temperature evaporate to dryness, residue add dehydrated alcohol 0.5ml makes dissolving, as need testing solution.
The preparation of control medicinal material solution: other gets Radix Angelicae Sinensis control medicinal material 0.5g, shines medical material solution in pairs with legal system.
The preparation of negative control solution: get scarce Radix Angelicae Sinensis negative control product 5g, make negative control solution with method.
Point sample amount: test liquid 20 μ l, control medicinal material solution 2 μ l, negative controls 20 μ l.
Developing solvent: Zheng Ji Wan-ethyl acetate (9: 1)
Lamellae: self-control silica gel g thin-layer plate
The colour developing and inspect: put under the ultra-violet lamp (365nm) and inspect
Experimental situation: temperature: 15 ℃ of relative humiditys: 56%
Experimental result shows that TONGBIAN LING capsule, Radix Angelicae Sinensis control medicinal material are put tangible corresponding speckle under the ultra-violet lamp (365nm), and negative noiseless (see figure 2), this method can be used as the specificity of Radix Angelicae Sinensis and differentiate.
(3) research of thin layer chromatography
A. the preparation of need testing solution
This experiment is studied the preparation method of need testing solution.Once studied following test sample preparation method:
(1) get this product content 4g, add methanol 20ml, supersound extraction 15 minutes filters, and filtrate is as need testing solution.
(2) get this product content 5g, (20: the 1) 20ml that adds diethyl ether-formic acid, supersound extraction 20 minutes filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.
(3) get this product content 5g, add 1% sodium bicarbonate solution 50ml, supersound process 10 minutes, centrifugal, get supernatant and regulate pH value to 2～3 with dilute hydrochloric acid, extract 2 times with the ether jolting, each 20ml merges ether solution, volatilize, residue adds methanol 1ml makes dissolving, as need testing solution.
(4) get this product content 5g, the 30ml that adds diethyl ether, supersound extraction 10 minutes filters, and filtrate is waved to 1ml, as need testing solution.
(5) get this product content 5g, add activated carbon 5g, the 50ml that adds methylene chloride, supersound process 15 minutes is put coldly, filters, and filtrate low temperature evaporate to dryness, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution.
Last system of selection (5) is the need testing solution preparation method.Select need testing solution, ask the client that what is provided as and select this prescription for use
B. the preparation of control medicinal material solution
Get Radix Angelicae Sinensis control medicinal material 1g, make control medicinal material solution with the test sample preparation method.
C. the preparation of negative control solution
Make the negative control sample that lacks Radix Angelicae Sinensis by prescription and method for making.Get the amount that is equivalent to test sample, make negative control solution by the preparation method of need testing solution.
D. the selection of chromatographic condition
(1) chromatoplate: with the sodium carboxymethyl cellulose is the silica gel g thin-layer plate of adhesive
(2) point sample amount: control medicinal material solution 2 μ l, need testing solution (granule) 2 μ l, (big grain) 20 μ l.
(3) developing solvent: compared following developing solvent
A) normal hexane-ethyl acetate (9: 1)
B) dimethylbenzene-ethyl acetate-formic acid (4: 1: 0.1)
Determine with normal hexane-ethyl acetate (9: 1) to be that the expansion effect of developing solvent is best at last.
(4) inspection method: put under the ultra-violet lamp (365nm) and inspect
E. test sample is differentiated
Get 10 batches of test samples respectively, by the condition test of selecting, favorable reproducibility (seeing Fig. 3 A and Fig. 3 B) as a result; Wherein experimental temperature is 30 ℃, and humidity is 60%; Fig. 3 A is the granule sampling test; Fig. 3 B is big grain sampling test.
(4) ruggedness is investigated
1. the comparison of different lamellaes:
Get Merck precoated plate, Yantai Chemical Industry Research Inst.'s product precoated plate, hands shop silica gel G-CMC-Na plate, respectively by the method suggested test, the basic zero difference of result (seeing Fig. 4 A-C), wherein experimental temperature is 30 ℃, humidity is 60%; 1 is Radix Angelicae Sinensis negative control (granule), and 2-4 is the preparation (granule) of different batches; 5 is the Radix Angelicae Sinensis control medicinal material; 6-8 is the preparation (big grain) of different batches, and 9 is Radix Angelicae Sinensis negative control (big grain).
2. the comparison of different temperatures:
Get the lamellae behind the point sample, in 10 ℃ and 30 ℃, launch respectively, inspect.The result shows in 10～30 ℃ of scopes and tests not have significantly influence (seeing Fig. 5 A and 5B) to differentiating, wherein the experimental temperature of Fig. 5 A is 10 ℃, and humidity is 25%, 1 to be Radix Angelicae Sinensis negative control (granule), and 2-4 is the preparation (granule) of different batches; 5 is the Radix Angelicae Sinensis control medicinal material; 6-8 is the preparation (big grain) of different batches, and 9 is Radix Angelicae Sinensis negative control (big grain); Wherein the experimental temperature of Fig. 5 B is 30 ℃, and humidity is 25%, 1 to be Radix Angelicae Sinensis negative control (granule), and 2-4 is the preparation (granule) of different batches; 5 is the Radix Angelicae Sinensis control medicinal material; 6-8 is the preparation (big grain) of different batches, and 9 is Radix Angelicae Sinensis negative control (big grain).
3. the comparison of different humidity:
Get the lamellae behind the point sample, in the chromatography cylinder of regulating relative humidity 25% and 75% with sulphuric acid, launch respectively, inspect.The result shows test between relative humidity 25%～75%, does not have significantly influence (seeing Fig. 6 A and 6B) to differentiating.Wherein the experimental temperature of Fig. 6 A is 10 ℃, and humidity is 25%, 1 to be Radix Angelicae Sinensis negative control (granule), and 2-4 is the preparation (granule) of different batches; 5 is the Radix Angelicae Sinensis control medicinal material; 6-8 is the preparation (big grain) of different batches, and 9 is Radix Angelicae Sinensis negative control (big grain); Wherein the experimental temperature of Fig. 6 B is 30 ℃, and humidity is 75%, 1 to be Radix Angelicae Sinensis negative control (granule), and 2-4 is the preparation (granule) of different batches; 5 is the Radix Angelicae Sinensis control medicinal material; 6-8 is the preparation (big grain) of different batches, and 9 is Radix Angelicae Sinensis negative control (big grain).
Learn demonstration test through said method, the result shows that the variation of lamellae, humiture is little to the influence that launches effect.Therefore, the good tolerance of this method.
3, the thin layer chromatography of Herba Cistanches is differentiated
This method has been studied the discriminating of the thin layer chromatography of Herba Cistanches, and after deliberation, the Herba Cistanches thin layer chromatography is differentiated no feature speckle, illustrates that this method is not suitable for carrying out the discriminating of Herba Cistanches, and concrete grammar is as follows:
(1) reagent and reagent
Negative sample: by TONGBIAN LING capsule prescription, the negative sample of preparation misrun Herba Cistanches.
The Herba Cistanches control medicinal material: lot number is 121195-200401, purchases in Nat'l Pharmaceutical ﹠ Biological Products Control Institute
The silica gel G plate: from making sheet, the Merck lamellae.
Reagent is analytical pure
(2) experimentation
Method one:
The preparation of need testing solution: get this product content 4g, add methanol 20ml, supersound extraction 15 minutes filters, and filtrate is as need testing solution.
The preparation of reference substance solution: other gets the betanin reference substance, adds methanol and makes the solution that every 1ml contains 5mg, in contrast product solution.
The preparation of negative control solution: get misrun Herba Cistanches negative control product 4g, make negative control solution with the test liquid preparation method.
Point sample amount: need testing solution 10 μ l, reference substance solution 5 μ l, negative control solution 10 μ l
Lamellae: silica gel G hands bed board (Qingdao Marine Chemical Co., Ltd.).
Developing solvent: ethyl acetate-methanol-acetic acid (4; 8: 1).
Colour developing and inspecting: take out, dry, spray is with the improvement bismuth potassium iodide test solution, and it is clear to be heated to the speckle colour developing at 105 ℃.
The result shows that the test sample hangover is serious, and the corresponding feature speckle of reference substance is not obvious, sees Fig. 3 A.Attempted the neutral alumina post to reduce hangover and yellowish green impurity, the yellow green speckle of background trails and has reduced as a result, but the corresponding feature speckle of reference substance rounding not has hangover, sees Fig. 3 B.Attempt again removing chlorophyll with activated carbon, developing solvent changes methanol-acetic acid (7: 3) into, and speckle still is unintelligible as a result, sees Fig. 3 C.With water 40ml eluting, eluent evaporate to dryness, residue add methanol 5ml makes dissolving to attempt active oxidation of coal aluminum post (activated carbon 1.5g, neutral alumina (200～300 order) 15g, column internal diameter 1.5cm), filters, and filtrate is as need testing solution.Results sample runs not get on, and is inconsistent with the reference substance speckle displacement, and unintelligible, sees Fig. 3 D.
Method two:
The preparation of need testing solution: get this product content 4g, add activated carbon 1g, add 80% ethanol 30ml, reflux 10 minutes filters, and filtrate is as need testing solution.
The preparation of reference substance solution: other gets the betanin reference substance, adds methanol and makes the solution that every 1ml contains 5mg, in contrast product solution.
The preparation of negative control solution: get misrun Herba Cistanches negative control product 4g, make negative control solution with the test liquid preparation method.
Point sample amount: need testing solution 10 μ l, reference substance solution 5 μ l, negative control solution 10 μ l
Lamellae: silica gel G hands bed board (Qingdao Marine Chemical Co., Ltd.).
Developing solvent: methanol-water-acetic acid (9: 2: 0.5).
Colour developing and inspecting: take out, dry, spray is with the improvement bismuth potassium iodide test solution, and it is clear to be heated to the speckle colour developing at 105 ℃.
The result shows that the corresponding feature speckle of reference substance is not obvious, sees Fig. 4.
Method three:
The preparation of need testing solution: get this product content 5g, add methanol 20ml, supersound process 15 minutes filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.
The preparation of reference substance solution: other gets echinacoside reference substance, verbascoside reference substance, adds methanol respectively and makes the solution that every 1ml contains 1mg, in contrast product solution.
The preparation of negative control solution: get misrun Herba Cistanches negative control product 5g, make negative control solution with the test liquid preparation method.
Point sample amount: need testing solution 5 μ l, reference substance solution 2 μ l, negative control solution 5 μ l
Lamellae: polyamide lamellae.
Developing solvent: methanol-acetic acid-water (2: 1: 7).
Colour developing and inspecting: take out, dry, put under the ultra-violet lamp (365nm) and inspect.
The result shows there is not the feature speckle of above-mentioned reference substance.
Studies show that above-mentioned three kinds of methods fail to find Herba Cistanches separation method preferably.
The detection method of aloe-emodine content in the embodiment 4 relieving constipation Chinese medicine preparation
The present invention has set up the content that high performance liquid chromatography (HPLC) method is measured aloe-emodin, empirical tests with check, this method is feasible, mainly is described as follows:
1. instrument and reagent
Instrument: high performance liquid chromatograph island Tianjin LC-20A (C1119), aters2695/2487 high performance liquid chromatograph (C1127), Agilent1100 (C1172) high performance liquid chromatograph.
Chromatographic column: DIKMA Diamonsil C
18, (5 μ, 4.6 * 250mm, 8032155 (40#)); Agilent ZORBAX SB, C
18(5 μ, 4.6 * 150mm (78#)); Kromasil C
18(5 μ, 4.6 * 150mm (61#)).
Balance: CP224D (C1060).
Ultrasound Instrument: KQ-300DA (C1103).
Reagent: ethyl acetate, phosphoric acid are analytical pure; HPLC methanol is chromatographically pure; Water is redistilled water.
Reagent: TONGBIAN LING capsule (Huanqiu Pharmaceutical Co., Ltd., Guangdong's production); The negative preparation (providing) of TONGBIAN LING capsule Folium Sennae by Huanqiu Pharmaceutical Co., Ltd., Guangdong; Aloe-emodin reference substance (Nat'l Pharmaceutical ﹠ Biological Products Control Institute, lot number 110795-200504);
2. methodology checking
(1) accuracy test
The preparation of reference substance solution: it is an amount of that precision takes by weighing the aloe-emodin reference substance, is mixed with the reference substance solution of 0.03024mg/ml, 0.1008mg/ml, 0.1403mg/ml, 0.2005mg/ml.
The preparation of recovery need testing solution: precision takes by weighing each 3 parts of known aloe-emodine content working sample (lot number: granule 060301, content 0.1351mg/g) 0.2g, 0.5g, 0.833g; Each 3 parts of sample (lot number: big grain 060301, content 0.3919mg/g) 0.192g, 0.5g, 0.772g.Corresponding respectively aloe-emodin reference substance solution (0.03024mg/ml) 1ml, aloe-emodin reference substance solution (0.1008mg/ml) 0.5ml, aloe-emodin reference substance solution (0.1403mg/ml) 1ml of adding of sample (granule 060301); Corresponding respectively aloe-emodin reference substance solution (0.03024mg/ml) 2ml, aloe-emodin reference substance solution (0.2005mg/ml) 1ml, aloe-emodin reference substance solution (0.1008mg/ml) 3ml of adding of sample (big grain 060301), volatilize solvent, press the preparation method preparation of need testing solution, promptly.The results are shown in Table 1A and table 1B.
Table 1A TONGBIAN LING capsule granule (060301) recovery test measurement result
The big grain of table 1B TONGBIAN LING capsule (060301) recovery test measurement result
This law response rate is good as seen from the above table, is fit to the assay of this product.
(2) precision test
1. replica test
Precision takes by weighing each 6 parts of same Oxyphenisatin Acetate capsule samples (060301 (granule), 060301 (big grain)) respectively, presses the preparation of need testing solution preparation method, measures the content of aloe-emodin.The average measurement result that the every 1g of this product (granule, big grain) contains aloe-emodin be respectively 0.1351mg (RSD0.4%, n=6), (RSD1.1%, n=6), the result shows that this law repeatability is good to 0.3919mg.The results are shown in Table 2A and table 2B.
Table 2A TONGBIAN LING capsule granule replica test result (lot number 060301)
The big grain of table 2B TONGBIAN LING capsule replica test result (lot number 060301)
2. precision in the middle of
By the above-mentioned analysis condition that provides, adopt the different brands high performance liquid chromatograph that same lot number sample (granule (060301), big grain (060301)) is measured respectively, the results are shown in Table 3A and table 3B.
Table 3A granule repeatability result (mg/g)
The big grain of table 3B repeatability result (mg/g)
(3) specificity
Detect the selection of wavelength:
Get the about 10mg of aloe-emodin reference substance, add methanol-ethyl acetate (2: 1) and be settled to 20ml, the accurate 2ml that draws adds methanol-ethyl acetate (2: 1) and is settled to 10ml, sweep measuring between 210～450nm.As a result, aloe-emodin has absorption maximum at the 254nm place, and spectrogram is seen Fig. 9.
The Folium Sennae negative control:
Get Folium Sennae negative control 1g, by above-mentioned test sample preparation method preparation, the accurate 10 μ l that draw inject high performance liquid chromatograph.As a result, negative control is noiseless.Chromatogram is seen Figure 10.
(4) linear relationship
It is an amount of that precision takes by weighing the aloe-emodin reference substance, adding methanol-ethyl acetate (2: 1) is settled to respectively in 10ml, 100ml, 100ml, the 100ml measuring bottle, ultrasonic making fully dissolved, and makes aloe-emodin reference substance mother solution (concentration is 0.8350mg/ml (1), 0.1008mg/ml (2), 0.1403mg/ml (3), 0.2005mg/ml (4)).Precision is measured aloe-emodin reference substance mother solution, is mixed with the reference substance solution of 0.000648mg/ml, 0.002005mg/ml, 0.006048mg/ml, 0.02005mg/ml, 0.0252mg/ml, 0.03024mg/ml respectively.Accurate respectively each reference substance mother solution and each reference substance solution 10 μ l of drawing inject high performance liquid chromatograph, and the record peak area is an abscissa with the sample size, and peak area is a vertical coordinate, the drawing standard curve.Regression equation is: Y=4000000X+82279, and correlation coefficient r=0.9999, The above results shows that the aloe-emodin sample size is good in 0.006048-8.350 μ g scope internal linear relation.See Figure 11.
(5) scope
The bottom line of this standard code is every and contains Folium Sennae with aloe-emodin (C
15H
10O
5) meter, granule must not be less than 0.077mg; Big grain must not be less than 0.16mg.So 20% and 600% (granule) (being 0.015mg/ grain～0.45mg/ grain) by limit; 40% and 500% (big grain) (being 0.057mg/ grain～0.75mg/ grain) of limit, the accuracy of investigation measurement range.
Adopt the application of sample absorption method, the accuracy of measurement range.Precision takes by weighing the sample (granule (060301) of known content, content 0.1351mg/g) 0.204g, (granule (060307), content 0.5578mg/g) 1.385g is each 6 parts, corresponding respectively accurate aloe-emodin reference substance solution (0.03024mg/ml) 1ml, aloe-emodin reference substance solution (0.2005mg/ml) 4ml of adding, volatilize solvent, by test sample preparation method preparation under the above-mentioned assay item, measure, be calculated as follows the scope response rate.The result is referring to table 4A.
Table 4A granule (060301) the scope response rate
Adopt the application of sample absorption method, the accuracy of measurement range.Precision takes by weighing sample (the big grain (060301) of known content, content 0.3919mg/g) 0.192g, (big grain (060204), content 0.7737mg/g) 1.5g is each 6 parts, corresponding respectively aloe-emodin reference substance solution (0.03024mg/ml) 2ml, aloe-emodin reference substance solution (0.8350mg/ml) 1.6ml of adding, volatilize solvent, by test sample preparation method preparation under the above-mentioned assay item, measure, be calculated as follows the scope response rate.The result is referring to table 4B.
The big grain of table 4B (060301) scope response rate
(6) ruggedness is investigated
1. extract choice of Solvent
Precision takes by weighing same lot number sample (granule 060301, big grain 060204) 1g, selects chloroform, dichloromethane as extracting solvent respectively, and by above-mentioned need testing solution preparation method preparation, the accurate test sample liquid 10 μ l that draw inject high performance liquid chromatograph.The result shows that granule sample chloroform and dichloromethane difference are little, and big grain sample differs bigger.Select chloroform as extracting solvent at last.The results are shown in Table 5A.
Table 5A is different to extract ratio of solvent
2. extraction time determines
Precision takes by weighing same lot number sample (granule 060301, big grain 060301) 1g, uses chloroform water-bath reflux, extract, 1 hour, 1.5 hours respectively by above-mentioned need testing solution preparation method, and the accurate need testing solution 10 μ l that draw inject high performance liquid chromatograph.The result shows that 1 hour, 1.5 hours difference of water-bath reflux, extract, are little, so select water-bath reflux, extract, 1 hour.The results are shown in Table 5B.
Table 5B is different, and extraction times compare
3. the stability of need testing solution:
The same need testing solution of accurate respectively absorption, sample introduction is measured in 0-30 hour in the preparation back, and the result shows that need testing solution is basicly stable in 30 hours, (granule) RSD1.3% (n=7), (big) RSD1.6% (n=7).The results are shown in Table 5C.
The stability of table 5C need testing solution
4. chromatographic column is investigated: different chromatographic column separation case relatively reach determining of number of theoretical plate.By the above-mentioned chromatographiccondition that provides, investigate the chromatographic column of 3 different brands fillers, relatively its chromatographic isolation situation sees Table 5D.Analysis result sees Table 5E.
Table 5D is different, and the chromatographic column separation case is investigated
Table 5E is different, and the chromatogram column analysis result investigates
By above-mentioned condition, on the chromatographic column of 3 different brands, all obtained satisfied separation.Imitate according to the actual measurement post, order number of theoretical plate temporarily and should be not less than 4000 with the calculating of aloe-emodin peak.Dikma Diamasil C18,5 μ m, 250mm * 4.6 μ m are selected in this research.
(7) the TONGBIAN LING capsule sample is measured
Get the TONGBIAN LING capsule of different lot numbers, measure in accordance with the law, the results are shown in Table 6A and table 6B.
The table 6A capsular aloe-emodine content measurement result of TONGBIAN LING (granule)
The capsular aloe-emodine content measurement result of table 6B TONGBIAN LING (big grain)
Record the result according to ten batch samples, remove a peak, remove calculating mean value behind the minimum, downward modulation 20%, tentative every contains Folium Sennae with aloe-emodin (C
15H
10O
5) meter, granule must not be less than 0.077mg, big grain must not be less than 0.15mg.
3. situation is checked in checking
According to the content measuring standard of working out, empirical tests with check, all with to draft unit deviation little, the repeatability of illustration method is better, sees Table 7 for the result.
Table 7 is the assay result of commensurate not
By the investigation that the TONGBIAN LING capsule of being produced is kept sample,, revise and enlarge specification and be " every dress 0.48g " in conjunction with producing practical situation.Former ministry standard " specification " is " every dress 0.25g ", so revision " specification " is " every dress 0.25g (granule); (0.48g big grain).”
Abovely described the present invention in detail, to those skilled in the art, should be understood that the above-mentioned specific embodiment should not be understood that to limit scope of the present invention with reference to the specific embodiment.Therefore, can make various changes and improvements to embodiment of the present invention without departing from the spirit and scope of the present invention.
Claims (12)
1. relieving constipation Chinese medicinal capsule preparation, this capsule preparations with Folium Sennae, Radix Angelicae Sinensis and Herba Cistanches be raw medicinal material by weight proportioning make at 8: 1: 1, it is characterized in that, the content of aloe-emodin is greater than 0.13mg/g in this capsule preparations, be preferably 0.13-0.60mg/g, more preferably 0.14-0.42mg/g.
2. the described relieving constipation Chinese medicinal capsule of claim 1 preparation, it is characterized in that, the preparation of this capsule preparations comprises Folium Sennae, Radix Angelicae Sinensis and Herba Cistanches decocting after-filtration, filtrate is concentrated into the thick paste that relative density is 1.25-1.42, described relative density is preferably 1.25-1.40, more preferably 1.30-1.40.
3. method for preparing claim 1 or 2 described relieving constipation Chinese medicinal capsule preparations, it is characterized in that, this method comprises the steps: Folium Sennae, Radix Angelicae Sinensis and Herba Cistanches decocting after-filtration, filtrate is concentrated into the thick paste that relative density is 1.25-1.42, described relative density is preferably 1.25-1.40, more preferably 1.30-1.40;
Wherein, the content of aloe-emodin is preferably 0.13-0.60mg/g greater than 0.13mg/g in the capsule preparations that makes, more preferably 0.14-0.42mg/g.
4. method according to claim 3 is characterized in that this method comprises the steps:
(1) Radix Angelicae Sinensis, Herba Cistanches two flavors are decocted with water, add the Folium Sennae of not pulverizing and decoct again, filter;
(2) filtrate that step (1) is obtained is condensed into the thick paste that relative density is 1.25～1.40 (25 ℃), adds the Senna Leaf after pulverizing, and mixing is granulated, and drying is sieved, mixing, promptly;
The wherein said Folium Sennae of not pulverizing and the parts by weight proportioning of the Senna Leaf after the described pulverizing are 3: 1～4: 1; Described relative density is preferably 1.25-1.40, more preferably 1.30-1.40.
5. the detection method of claim 1 or 2 described relieving constipation Chinese medicinal capsule preparations, this method comprises that following employing thin layer chromatography detects the step of Folium Sennae:
(1) preparation need testing solution: get described relieving constipation Chinese medicine preparation 1g, porphyrize adds 10% potassium hydroxide-ethanol solution 50ml, boiled 2 minutes, add water 10ml, filter, filtrate adds hydrochloric acid, and to transfer to pH value be 2～3, put and steam in the water-bath to there not being the alcohol flavor, extract with ether 10ml jolting, divide and get ether layer, volatilize, residue adds ethanol 0.5ml makes dissolving, gets supernatant as need testing solution;
(2) preparation control medicinal material solution: get Folium Sennae control medicinal material 0.5g, make control medicinal material solution according to the described method of step (1);
(3) adopt thin layer chromatography to differentiate Folium Sennae: to draw each 5 μ l of two kinds of solution that step (1) and step (2) are obtained, put respectively on same silica gel g thin-layer plate, upper solution with normal propyl alcohol-ethyl acetate-water (3: 4: 3) is developing solvent, launch, take out, dry, it is smoked clear to the speckle colour developing to put in the ammonia.
6. detection method according to claim 5 is characterized in that, this method comprises that following employing thin layer chromatography detects the step of Radix Angelicae Sinensis:
(1) preparation need testing solution: get described relieving constipation Chinese medicine preparation 5g, add active carbon powder 5g, the 50ml that adds methylene chloride, supersound process 15 minutes is put coldly, filters, and filtrate low temperature evaporate to dryness, residue add dehydrated alcohol 0.5ml makes dissolving, as need testing solution;
(2) preparation control medicinal material solution: get Radix Angelicae Sinensis control medicinal material 0.5g, make control medicinal material solution according to the described method of step (1);
(3) adopt thin layer chromatography to differentiate Radix Angelicae Sinensis: draw need testing solution 2～20 μ l, control medicinal material solution 2 μ l put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate (9: 1) is developing solvent, launches, and takes out, dry, put under the ultra-violet lamp 365nm and inspect.
7. the detection method of claim 1 or 2 described relieving constipation Chinese medicinal capsule preparations, this method comprises the content that adopts high performance liquid chromatography to measure aloe-emodin in the described capsule preparations.
8. detection method according to claim 7 is characterized in that the preparation method of described need testing solution comprises the steps: to get preparation 1g, the accurate title, decide, and puts in the conical flask, the accurate methanol 50ml that adds, claim to decide weight, supersound process 30 minutes is put cold, supply the weight that subtracts mistake with methanol, filter, precision is measured subsequent filtrate 15ml, put in the conical flask, evaporate to dryness, residue add 8% hydrochloric acid solution 30ml, add chloroform 30ml, water-bath refluxed 1 hour, immediately cooling, transfer is put in the separatory funnel, divide and get the chloroform layer, the jolting of sour water layer reuse chloroform is extracted 3 times, each 20ml, merge chloroform liquid, evaporate to dryness, residue add methanol makes dissolving, is transferred in the 10ml measuring bottle, add methanol constant volume to scale, shake up, filter, get subsequent filtrate.
9. detection method according to claim 7 is characterized in that it is an amount of that the preparation method of described reference substance solution comprises the steps: to get the aloe-emodin reference substance, and accurate the title decides, and adds mobile phase and makes the solution that every 1ml contains 15 μ g.
10. according to each described detection method of claim 7-9, it is characterized in that the chromatographic condition in the described method is: filler is the 18 alkyl silica gel bonded silica gel; Mobile phase is methanol-0.3% phosphoric acid solution (60: 40); The detection wavelength is 254nm.
11. according to each described detection method of claim 7-9, it is characterized in that, the aloe-emodine content scope that described method is measured is that every gram granule contains aloe-emodin 0.077mg at least, preferably, the aloe-emodine content scope of described method mensuration is that every gram granule contains aloe-emodin 0.15mg at least.
12. claim 1 or 2 described relieving constipation Chinese medicinal capsule preparations are used for the treatment of purposes in constipation with heat retention, long-term bed constipation, momentary abdominal distention constipation and the senility habitual constipation in preparation.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102526211A (en) * | 2012-03-05 | 2012-07-04 | 中国人民解放军第四军医大学 | Composition of oral medicine for treating constipation and preparation technology |
| CN107440118A (en) * | 2017-08-16 | 2017-12-08 | 河南树铭药业有限公司 | A kind of health food with defecating feces excretion and preparation method thereof |
| CN111024878A (en) * | 2019-12-30 | 2020-04-17 | 江苏艾兰得营养品有限公司 | Analysis method capable of rapidly identifying folium sennae extract |
| CN115436490A (en) * | 2021-06-02 | 2022-12-06 | 武汉康乐药业股份有限公司 | Tongbianling capsule fingerprint spectrum and construction method and application thereof |
-
2009
- 2009-11-27 CN CN200910207487XA patent/CN102078380A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102526211A (en) * | 2012-03-05 | 2012-07-04 | 中国人民解放军第四军医大学 | Composition of oral medicine for treating constipation and preparation technology |
| CN102526211B (en) * | 2012-03-05 | 2014-04-23 | 中国人民解放军第四军医大学 | Composition of oral medicine for treating constipation and preparation technology |
| CN107440118A (en) * | 2017-08-16 | 2017-12-08 | 河南树铭药业有限公司 | A kind of health food with defecating feces excretion and preparation method thereof |
| CN111024878A (en) * | 2019-12-30 | 2020-04-17 | 江苏艾兰得营养品有限公司 | Analysis method capable of rapidly identifying folium sennae extract |
| CN115436490A (en) * | 2021-06-02 | 2022-12-06 | 武汉康乐药业股份有限公司 | Tongbianling capsule fingerprint spectrum and construction method and application thereof |
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Application publication date: 20110601 |