CN1824238A - Quality control method of medicinal preparation for treating lypemania - Google Patents
Quality control method of medicinal preparation for treating lypemania Download PDFInfo
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Abstract
A quality control method for the Chinese medicine used to treat depression includes such steps as checking its characteristics, discrimination to cablin potchouli herb, atractylodes rhizome, katsumadai seed and tangerine peel, and measuring the content of hesperidin.
Description
Technical field: the present invention relates to a kind of method of quality control for the treatment of medicine (Yu Shuda) preparation of depression, belong to the technical field of medicine being carried out quality control.
Background technology: depression is a kind of common mental disorder, is one of principal disease of human high incidence.External investigation finds that depressed point prevalence is 4.3%, and lifetime prevalence is 8%～20%.According to scholarly forecast, the sickness rate of China's depression also will be improved largely than the eighties.At present antidepressants mostly are Western medicine greatly on the foreign market, but the part patient is not good to its reaction, and multiple side effect and contraindication are arranged, and patient can not be tolerated and be difficult to reach satisfactory effect, and relapse rate is also high, and various antidepressants all might bring out dry mad.Depressive disorder is a kind of affective disorders, and suppressing with depressed, retardation of thinking and psychomotor activity clinically is feature, belongs to the category of the traditional Chinese medical science " strongly fragrant disease ".The applicant has developed the YUSHUDA ZHIJI prescription of finishing and has been made up of Herba Pogostemonis, Pericarpium Citri Reticulatae, Fructus Amomi Rotundus, Semen Alpiniae Katsumadai, Rhizoma Atractylodis (parched with bran), and prescription is with light clear fragrance, and the dry product of bitter warm nature are main the composition, and all medicine compatibilities are gone into middle Jiao, the removing dampness of being amusing, the resolving depression of regulating the flow of vital energy.Studies show that the antidepressant effect of YUSHUDA ZHIJI is remarkable, side effect is little; Quality controllable, stable performance is a kind of preparation of very promising treatment by Chinese herbs depressive disorder; The applicant has submitted patent application to State Patent Office, application number: 200510200474.1.The applicant finds in the development process of whole medicine: if this medicine does not have the strict quality standard, the product quality reliability that obtains is just not high, and therapeutic effect can be not obvious; Think and reduce drug side effect by the clinical efficacy that improves this medicine, must formulate a reliable quality standard.
Summary of the invention:
The objective of the invention is to: a kind of method of quality control for the treatment of the YUSHUDA ZHIJI of depression is provided, and said preparation comprises all possible compound preparation of capsule, tablet, granule.The present invention is according to the contained chemical constituent of prescription taste of Chinese medicine, preparation technology and dosage form, quality control projects such as content assaying method, discrimination method, character, inspection have been studied and defined, controlling the quality of YUSHUDA ZHIJI effectively, thereby guarantee the clinical efficacy of this preparation.
The YUSHUDA ZHIJI of treatment depression of the present invention is made by Herba Pogostemonis 1000g, Pericarpium Citri Reticulatae 334g, Fructus Amomi Rotundus 500g, Semen Alpiniae Katsumadai 500g and Rhizoma Atractylodis (parched with bran) 666g, its preparation method is: five tastes medical material decocts with water four times, each 2 hours, amount of water was 14 times of medical material amount; Collecting decoction, filter, being concentrated into relative density is the clear paste of 1.04-1.05 (50 ℃), adds ethanol and makes and contain the alcohol amount and reach 70%, cold preservation (5～10 ℃) is spent the night, filter, filtrate recycling ethanol, and be concentrated into the clear paste that relative density is 1.32～1.35 (50 ℃), drying under reduced pressure (70 ℃), dried cream powder is broken into fine powder, adds the appropriate amount of auxiliary materials mixing again, makes corresponding preparation according to conventional method.
Method of quality control of the present invention mainly comprises character, discriminating, inspection and assay project, and wherein the character item should meet the pertinent regulations under each preparation item; Differentiate that item is the discriminating to Herba Pogostemonis, Rhizoma Atractylodis, Semen Alpiniae Katsumadai, Pericarpium Citri Reticulatae; Check that item should meet the pertinent regulations under each preparation item of appendix of Chinese Pharmacopoeia version in 2000; The assay item is for measuring Determination of Hesperidin Content in the preparation.
Wherein, the discrimination method of Herba Pogostemonis is to be contrast with the Herba Pogostemonis control medicinal material, and with toluene: ethyl acetate: normal hexane: formic acid=2: 4: 8: 0.1 is the thin layer discrimination method of developing solvent.
The discrimination method of Rhizoma Atractylodis is to be contrast with the Rhizoma Atractylodis control medicinal material, and with toluene: ethyl acetate: normal hexane=1.5: 0.3: 7 is the thin layer discrimination method of developing solvent.
The discrimination method of Semen Alpiniae Katsumadai is to be contrast with the plain reference substance of Semen Alpiniae Katsumadai control medicinal material, Alpinia japonica (Thunb.) Miq., and with chloroform: methanol=9: 0.5 is the thin layer discrimination method of developing solvent.
The discrimination method of Pericarpium Citri Reticulatae is to be contrast with Pericarpium Citri Reticulatae control medicinal material, Hesperidin reference substance, and with ethyl acetate: methanol: the upper solution of water=6: 1.5: 3 is the thin layer discrimination method of developing solvent.
Concrete discrimination method comprises the part or all of of following project:
(1) get YUSHUDA ZHIJI, porphyrize claims 3.0g, adds chloroform 25ml, and supersound process is 10 minutes under power 150W, frequency 20kHz condition, is cooled to room temperature, filters, and the filtrate evaporate to dryness adds the 1ml ethyl acetate and makes dissolving, as need testing solution; Get the blank preparation 3.0g of Herba Pogostemonis, make the Herba Pogostemonis blank solution with method; Other gets Herba Pogostemonis control medicinal material 3.0g, shines medical material solution in pairs with legal system; According to the test of an appendix VIB of Pharmacopoeia of People's Republic of China version in 2000 thin layer chromatography, draw need testing solution, each 4 μ l of blank solution, control medicinal material solution 4 μ l put in same silica gel G F
254On the lamellae, with toluene: ethyl acetate: normal hexane: formic acid=2: 4: 8: 0.1 is developing solvent, launches, and takes out, and dries, and puts under the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color; Negative sample does not then show;
(2) get YUSHUDA ZHIJI, porphyrize claims 4.0g, adds chloroform 25ml, and supersound process is 10 minutes under power 150W, frequency 20kHz condition, is cooled to room temperature, filters, and the filtrate evaporate to dryness adds the 1ml ethyl acetate and makes dissolving, as need testing solution; Get the blank preparation 4.0g of Rhizoma Atractylodis, make the Rhizoma Atractylodis blank solution with method; Other gets Rhizoma Atractylodis control medicinal material 0.5g, shines medical material solution in pairs with legal system; Test according to an appendix VIB of Pharmacopoeia of People's Republic of China version in 2000 thin layer chromatography, draw need testing solution, each 10 μ l of blank solution, control medicinal material solution 6 μ l, point is on same silica gel g thin-layer plate, with toluene: ethyl acetate: normal hexane=1.5: 0.3: 7 be developing solvent, expansion, take out, dry, spray is with 5% phosphomolybdic acid-alcoholic solution, and 105 ℃ to be heated to speckle colour developing clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color; Negative sample does not then show;
(3) get YUSHUDA ZHIJI, porphyrize claims 2.0g, adds methanol 15ml, puts and heats jolting 5 minutes in the water-bath, filter, filtrate is put in the separatory funnel, adds the ethyl acetate jolting and extracts 2 times, each 10ml, merge extractive liquid,, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Get the blank preparation 2.0g of Semen Alpiniae Katsumadai, make the Semen Alpiniae Katsumadai blank solution with method; Get Semen Alpiniae Katsumadai control medicinal material 2.0g, shine medical material solution in pairs with legal system; Other gets the plain reference substance of Alpinia japonica (Thunb.) Miq., adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VIB of Pharmacopoeia of People's Republic of China version in 2000 thin layer chromatography, draw need testing solution, blank solution, each 10 μ l of control medicinal material solution, reference substance solution 2 μ l, point is on same silica gel g thin-layer plate, with chloroform: methanol=9: 0.5 is developing solvent, launches, and takes out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color; With the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color; Negative sample does not then show;
(4) get YUSHUDA ZHIJI, porphyrize claims 4.0g, adds methanol 25ml, and supersound process is 30 minutes under power 150W, frequency 20kHz condition, is cooled to room temperature, filters, and filtrate is as need testing solution; Get the blank preparation 4.0g of Pericarpium Citri Reticulatae, make the Pericarpium Citri Reticulatae blank solution with method; Get Pericarpium Citri Reticulatae control medicinal material 2.0g, shine medical material solution in pairs with legal system; Other gets the Hesperidin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VIB of Pharmacopoeia of People's Republic of China version in 2000 thin layer chromatography, draw need testing solution, blank solution, each 6 μ l of control medicinal material solution, reference substance solution 8 μ l, point is on same silica gel g thin-layer plate, with ethyl acetate: methanol: the upper solution of water=6: 1.5: 3 is developing solvent, launches, take out, dry, spray is put under the 365nm ultra-violet lamp and is inspected with the aluminum chloride test solution; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color; With the corresponding position of reference substance chromatograph on, show an identical yellow-green fluorescence speckle; Negative sample does not then show.
The Determination of Hesperidin Content assay method is to be contrast with the Hesperidin reference substance, and with acetonitrile: 1% acetic acid aqueous solution=20: 80 is the high performance liquid chromatography of mobile phase.
Concrete content assaying method is:
According to 2000 editions one appendix VID high effective liquid chromatography for measuring of Chinese Pharmacopoeia:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile: 1% acetic acid aqueous solution=20: 80 is a mobile phase; The detection wavelength is 283nm; 30 ℃ of column temperatures; Number of theoretical plate calculates by the Hesperidin peak should be not less than 2000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the Hesperidin reference substance, adds methanol and make the solution that every 1ml contains 0.4mg, promptly;
The about 0.2g of YUSHUDA ZHIJI is got in the preparation of need testing solution, porphyrize, and accurate the title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, and supersound process is 1 hour under power 150W, frequency 20kHz condition, put coldly, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, precision is measured subsequent filtrate 30ml, evaporate to dryness, with dissolve with methanol and be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter, get subsequent filtrate and filter, promptly with 0.45 μ m microporous filter membrane;
Accurate respectively reference substance solution 3 μ l, 6 μ l and the need testing solution 8 μ l of drawing of algoscopy inject chromatograph of liquid, measure, and the external standard two-point method calculates, promptly;
The every least unit of YUSHUDA ZHIJI contains Pericarpium Citri Reticulatae with Hesperidin C
28H
34O
15Meter must not be less than 6.70mg.
Described method of quality control comprises:
Character: medicine or its content show light brown, gas perfume (or spice), mildly bitter flavor;
Differentiate: (1) gets YUSHUDA ZHIJI, and porphyrize claims 3.0g, adds chloroform 25ml, and supersound process is 10 minutes under power 150W, frequency 20kHz condition, is cooled to room temperature, filters, and the filtrate evaporate to dryness adds the 1ml ethyl acetate and makes dissolving, as need testing solution; Get the blank preparation 3.0g of Herba Pogostemonis, make the Herba Pogostemonis blank solution with method; Other gets Herba Pogostemonis control medicinal material 3.0g, shines medical material solution in pairs with legal system; According to the test of an appendix VIB of Pharmacopoeia of People's Republic of China version in 2000 thin layer chromatography, draw need testing solution, each 4 μ l of blank solution, control medicinal material solution 4 μ l put in same silica gel G F
254On the lamellae, with toluene: ethyl acetate: normal hexane: formic acid=2: 4: 8: 0.1 is developing solvent, launches, and takes out, and dries, and puts under the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color; Negative sample does not then show;
(2) get YUSHUDA ZHIJI, porphyrize claims 4.0g, adds chloroform 25ml, and supersound process is 10 minutes under power 150W, frequency 20kHz condition, is cooled to room temperature, filters, and the filtrate evaporate to dryness adds the 1ml ethyl acetate and makes dissolving, as need testing solution; Get the blank preparation 4.0g of Rhizoma Atractylodis, make the Rhizoma Atractylodis blank solution with method; Other gets Rhizoma Atractylodis control medicinal material 0.5g, shines medical material solution in pairs with legal system; Test according to an appendix VIB of Pharmacopoeia of People's Republic of China version in 2000 thin layer chromatography, draw need testing solution, each 10 μ l of blank solution, control medicinal material solution 6 μ l, point is on same silica gel g thin-layer plate, with toluene: ethyl acetate: normal hexane=1.5: 0.3: 7 be developing solvent, expansion, take out, dry, spray is with 5% phosphomolybdic acid-alcoholic solution, and 105 ℃ to be heated to speckle colour developing clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color; Negative sample does not then show;
(3) get YUSHUDA ZHIJI, porphyrize claims 2.0g, adds methanol 15ml, puts and heats jolting 5 minutes in the water-bath, filter, filtrate is put in the separatory funnel, adds the ethyl acetate jolting and extracts 2 times, each 10ml, merge extractive liquid,, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Get the blank preparation 2.0g of Semen Alpiniae Katsumadai, make the Semen Alpiniae Katsumadai blank solution with method; Get Semen Alpiniae Katsumadai control medicinal material 2.0g, shine medical material solution in pairs with legal system; Other gets the plain reference substance of Alpinia japonica (Thunb.) Miq., adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VIB of Pharmacopoeia of People's Republic of China version in 2000 thin layer chromatography, draw need testing solution, blank solution, each 10 μ l of control medicinal material solution, reference substance solution 2 μ l, point is on same silica gel g thin-layer plate, with chloroform: methanol=9: 0.5 is developing solvent, launches, and takes out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color; With the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color; Negative sample does not then show;
(4) get YUSHUDA ZHIJI, porphyrize claims 4.0g, adds methanol 25ml, and supersound process is 30 minutes under power 150W, frequency 20kHz condition, is cooled to room temperature, filters, and filtrate is as need testing solution; Get the blank preparation 4.0g of Pericarpium Citri Reticulatae, make the Pericarpium Citri Reticulatae blank solution with method; Get Pericarpium Citri Reticulatae control medicinal material 2.0g, shine medical material solution in pairs with legal system; Other gets the Hesperidin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VIB of Pharmacopoeia of People's Republic of China version in 2000 thin layer chromatography, draw need testing solution, blank solution, each 6 μ l of control medicinal material solution, reference substance solution 8 μ l, point is on same silica gel g thin-layer plate, with ethyl acetate: methanol: the upper solution of water=6: 1.5: 3 is developing solvent, launches, take out, dry, spray is put under the 365nm ultra-violet lamp and is inspected with the aluminum chloride test solution; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color; With the corresponding position of reference substance chromatograph on, show an identical yellow-green fluorescence speckle; Negative sample does not then show;
Check: should meet the pertinent regulations under each preparation item of appendix of Chinese Pharmacopoeia version in 2000;
Assay: shine 2000 editions one appendix VID high effective liquid chromatography for measuring of Chinese Pharmacopoeia:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile: 1% acetic acid aqueous solution=20: 80 is a mobile phase; The detection wavelength is 283nm; 30 ℃ of column temperatures; Number of theoretical plate calculates by the Hesperidin peak should be not less than 2000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the Hesperidin reference substance, adds methanol and make the solution that every 1ml contains 0.4mg, promptly;
The about 0.2g of YUSHUDA ZHIJI is got in the preparation of need testing solution, porphyrize, and accurate the title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, and supersound process is 1 hour under power 150W, frequency 20kHz condition, put coldly, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, precision is measured subsequent filtrate 30ml, evaporate to dryness, with dissolve with methanol and be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter, get subsequent filtrate and filter, promptly with 0.45 μ m microporous filter membrane;
Accurate respectively reference substance solution 3 μ l, 6 μ l and the need testing solution 8 μ l of drawing of algoscopy inject chromatograph of liquid, measure, and the external standard two-point method calculates, promptly;
The every least unit of YUSHUDA ZHIJI contains Pericarpium Citri Reticulatae with Hesperidin C
28H
34O
15Meter must not be less than 6.70mg.
Compared with prior art, method of quality control specificity of the present invention is strong, favorable reproducibility, and the precision height, good stability has guaranteed the clinical efficacy of this preparation effectively, has reached the goal of the invention of effective control drug quality.
For science and the reasonability of verifying method of quality control of the present invention, carried out following experimentation.
One, differentiates
1, the feature of contained Herba Pogostemonis is differentiated in the side of being: the discrimination method under the pharmacopeia Herba Pogostemonis item is the discriminating of volatile oil, this preparation is an aqueous extraction-alcohol precipitation technology, therefore the described discrimination method of pharmacopeia is inapplicable, the list of references report, by test, obtained medical material and test sample and had corresponding feature speckle, negative sample is noiseless, so adopt thin layer of the present invention to differentiate.
2, the feature of contained Rhizoma Atractylodis is differentiated in the side of being: the discrimination method under the pharmacopeia Rhizoma Atractylodis item is the discriminating of volatile oil,
This preparation is an aqueous extraction-alcohol precipitation technology, so the described discrimination method of pharmacopeia is inapplicable, by test, has obtained medical material and test sample and has had corresponding feature speckle, and negative sample is noiseless, so adopt thin layer of the present invention to differentiate.
3, the feature of contained Semen Alpiniae Katsumadai is differentiated in the side of being: according to the discrimination method under the pharmacopeia Semen Alpiniae Katsumadai item, feminine gender has interference, the list of references report, select different developing solvents for use, by test, obtain medical material and test sample and had corresponding feature speckle, be equipped with corresponding speckle with the plain reference substance corresponding positions of Alpinia japonica (Thunb.) Miq., negative sample is noiseless, so adopt thin layer of the present invention to differentiate.
4, the feature of contained Pericarpium Citri Reticulatae is differentiated in the side of being: with reference to the discrimination method under the pharmacopeia Pericarpium Citri Reticulatae item, negative sample is noiseless, so adopt thin layer of the present invention to differentiate.
Two, check
By " regulation under each preparation item of appendix of Chinese pharmacopoeia version in 2000 is carried out following inspection to three batch samples:
Weight differential is checked: according to weight differential under an appendix ID of Pharmacopoeia of People's Republic of China version in 2000 the tablet item three batch samples are checked, be the results are shown in Table 1.
Check disintegration: according to inspection technique disintegration (appendix XIIA of Pharmacopoeia of People's Republic of China version in 2000), three batch samples are checked, be the results are shown in Table 1.
Table 1 weight differential, disintegration check result
| Sample number | 040811 | 040812 | 040813 |
| Weight differential | Up to specification | Up to specification | Up to specification |
| Disintegration (branch) | 17 | 17 | 17 |
Heavy metal is checked: according to heavy metal inspection technique (appendix IXE of Pharmacopoeia of People's Republic of China version in 2000), three batch samples 040811,040812,040813 are checked, do not detected, so exclude content of the present invention.
Arsenic salt is checked: according to arsenic salt inspection technique (appendix IXF of Pharmacopoeia of People's Republic of China version in 2000), three batch samples 040811,040812,040813 are checked, do not detected, so exclude content of the present invention.
The organic chlorine agriculture chemicals residual quantity is checked: according to organic chlorine agriculture chemicals determination of residual amount method (appendix IXQ of Pharmacopoeia of People's Republic of China version in 2000) three batch samples 040811,040812,040813 are checked, the result shows, three batch sample Gamma Hexaochlorocyclohexane (BHC), clofenotane (DDT) content are all up to specification, so exclude content of the present invention.
Three, assay
According to high-efficient liquid phase technique (appendix VID of Pharmacopoeia of People's Republic of China version in 2000).
Instrument and reagent:
Instrument: Waters Delta 600 pumps; Waters 2478Dual λ Absobance Detector UV-detector; Waters Millennium32 work station; Ultrasonic oscillator (power 150W, frequency 20kHz).
Reagent: acetonitrile is a chromatographically pure, and methanol is that top grade is pure, and all the other reagent are analytical pure, and water is the deionization redistilled water; 0.45 μ m filter membrane (Millipore), Hesperidin reference substance (available from the 0721-200010 of Nat'l Pharmaceutical ﹠ Biological Products Control Institute).
1, the preparation of test sample: see this description text content assaying method.
2, the preparation of reference substance solution: see this description text content assaying method.
3, chromatographic condition
Chromatographic column: 150 * 4.6mm 5 μ Inertsil ODS-3, mobile phase: acetonitrile-1% acetic acid aqueous solution (20: 80), detect wavelength: 283nm, column temperature: 30 ℃, flow velocity: 1ml/min.
Once selected the described mobile phase methanol-acetic acid of pharmacopeia-water (35: 4: 61) for use, the Hesperidin separating effect is not good in the preparation, so transposing mobile phase, when selecting acetonitrile-1% acetic acid aqueous solution (20: 80) for use for mobile phase, the Hesperidin peak shape is better, does not have other composition and disturbs, so list content of the present invention in.
4, linear relationship is investigated
Hesperidin reference substance 1,2,3,4,5,6,7,8 Ma that accurate absorption concentration is 0.4042mg/ml inject chromatograph of liquid, measure.The result shows that Hesperidin is good linear relationship between 0.4042～3.2336 Therewith, and γ=0.9997 sees Table 2.
Table 2 Hesperidin linear relationship is investigated data
| Sample size | 1μl | 2μl | 3μl | 4μl | 5μl | 6μl | 7μl | 8μl |
| (μg) | 0.4042 | 0.8084 | 1.2126 | 1.6168 | 2.0210 | 2.4252 | 2.8294 | 3.2336 |
| Peak area | 604157 | 1101802 | 1794577 | 2416015 | 3009257 | 3649007 | 4296760 | 4916229 |
Y＝1540839.8X-79158.0 γ＝0.9997
5, blank assay
Get the blank preparation of Pericarpium Citri Reticulatae (going the Pericarpium Citri Reticulatae preparation), accurately claim decide 1.0g, make the Pericarpium Citri Reticulatae blank solution with the preparation method of text need testing solution by full prescription, sample introduction under above-mentioned HPLC chromatographic condition, the result shows that feminine gender is noiseless.
6, precision is investigated
Get formulation samples (040511), porphyrize, precision claims to conclude a contract or treaty puts 1.0g in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, supersound process (power 150W, frequency 20kHz) 1 hour, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, filter, precision is measured subsequent filtrate 10ml evaporate to dryness, and residue adds methanol makes dissolving, and be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter, get subsequent filtrate and filter, promptly with microporous filter membrane (0.45 μ m).The accurate respectively need testing solution 4 μ l that draw, sample introduction is measured its peak area under above-mentioned HPLC chromatographic condition, and the external standard two-point method calculates its content.The results are shown in Table 3.
Table 3 precision is investigated
| The sample introduction number of times | 1 | 2 | 3 | 4 | 5 |
| Peak area | 2835180 | 2787916 | 2912329 | 2864453 | 2846451 |
| Relative standard deviation (RSD%) 1.58% | |||||
The result shows that the instrument precision relative standard deviation is 1.58%, shows that instrument precision is good.
7, Wen Dingxing investigation
Get formulation samples (040511), porphyrize, precision claims to conclude a contract or treaty puts 1.0g in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, supersound process (power 150W, frequency 20kHz) 1 hour, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, filter, precision is measured subsequent filtrate 10ml evaporate to dryness, and residue adds methanol makes dissolving, and be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter, get subsequent filtrate and filter, promptly with microporous filter membrane (0.45 μ m).The accurate respectively need testing solution 4 μ l that draw, sample introduction is measured its peak area under above-mentioned HPLC chromatographic condition, and the external standard two-point method calculates its content.The results are shown in Table 4.
Table 4 study on the stability
| Time | 0 hour | 1 hour | 3 hours | 5 hours | 7 hours |
| Peak area | 2846451 | 2835180 | 2787916 | 2912329 | 2864453 |
| Relative standard deviation (RSD%) 1.58% | |||||
The result shows that its relative standard deviation is 1.58%, shows that sample was stable in 7 hours.
8, repeatability is investigated
Get formulation samples (040511), porphyrize, the accurate title, decided 5 parts, every part of about 0.3g, put in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, supersound process (power 150W, frequency 20kHz) 1 hour is put coldly, claims to decide weight again, supply the weight that subtracts mistake with methanol, shake up, filter, precision is measured subsequent filtrate 20ml evaporate to dryness, residue adds methanol makes dissolving, and is transferred in the 5ml measuring bottle, adds methanol to scale, shakes up, filter, get subsequent filtrate and filter, promptly with microporous filter membrane (0.45 μ m).The accurate respectively need testing solution 4 μ l that draw, sample introduction is measured its peak area under above-mentioned HPLC chromatographic condition, and the external standard two-point method calculates its content.The results are shown in Table 5.
Table 5 repeatability is investigated
| Sample number | (g) weighs | Constant volume (ml) | Peak area | Content (mg/g preparation) | RSD％ |
| 1 | 0.3512 | 6 | 1387643 | 10.53 | 1.50％ |
| 2 | 0.3537 | 5 | 1737516 | 10.40 | |
| 3 | 0.3227 | 5 | 1537981 | 10.35 | |
| 4 | 0.3402 | 5 | 1695217 | 10.60 | |
| 5 | 0.3476 | 5 | 1769115 | 10.74 |
The result shows that its relative standard deviation is that RSD% is 1.50%, shows that the sample repeatability is good.
9, the investigation of extracting method
Different solvents, Different Extraction Method, different extraction time are investigated, the need testing solution that Different Extraction Method makes is measured under above-mentioned high-efficient liquid phase chromatogram condition, the result shows that ultrasonic 1 hour extraction ratio of methanol is the highest, extracts the most complete.The results are shown in Table 6,7,8,9,10.
9.1 the investigation of different solvents extracting method
Get formulation samples (040511), porphyrize, precision claims to conclude a contract or treaty puts 4.5g in the tool plug conical flask, accurate respectively methanol, ethyl acetate, each 50ml of dehydrated alcohol of adding, close plug claims to decide weight, supersound process (power 150W, frequency 20kHz) 45 minutes is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with solvent, filter, get subsequent filtrate and filter, promptly get need testing solution with microporous filter membrane (0.45 μ m), inject chromatograph of liquid, measure, the external standard two-point method calculates its content.The results are shown in Table 6.
The investigation of table 6 different solvents extracting method
| Sample number | (g) weighs | Sample size (μ l) | Peak area | Content of hesperidin (mg/g preparation) |
| Ethyl acetate | 4.6136 | 20 | 42088 | - |
| Methanol | 5.3022 | 2 | 3612484 | 10.39 |
| Dehydrated alcohol | 4.6186 | 20 | 2267405 | 0.80 |
The result shows that the methanol extraction rate is the highest.
9.2 different time methanol heating and refluxing extraction
Get formulation samples (040511), porphyrize, precision claims to conclude a contract or treaty 4.5g, add methanol 100ml, reflux was taken out after different time, be cooled to room temperature, shake up, filter, filtrate is transferred in the 100ml measuring bottle, adds methanol to scale, shakes up, filter, get subsequent filtrate and filter, promptly get need testing solution with microporous filter membrane (0.45 μ m), inject chromatograph of liquid, measure, the external standard two-point method calculates its content.The results are shown in Table 7.
The investigation of table 7 different heating time
| (g) weighs | Heat time heating time | Sample size (μ l) | Peak area | Content of hesperidin (mg/g preparation) |
| 4.6177 | 1 hour | 5 | 2837667 | 7.71 |
| 4.6131 | 3 hours | 5 | 2798305 | 7.62 |
| 4.6168 | 5 hours | 5 | 3333923 | 8.88 |
| 4.0923 | 7 hours | 5 | 2661274 | 8.22 |
The result shows that 5 hours extraction ratios of methanol heating are the highest, and content of hesperidin is the 8.88mg/g preparation.
9.3 extract after the different time reflux
The about 4.5g of sample thief (040511), porphyrize, the accurate title, decide, precision adds entry 50ml, and reflux was taken out after different time, be cooled to room temperature, shake up, filter, the accurate subsequent filtrate 30ml that draws puts in the separatory funnel, add the ethyl acetate jolting and extract 3 times, each 30ml, merge extractive liquid,, evaporate to dryness, with dissolve with methanol and be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter, get subsequent filtrate and filter, promptly get need testing solution, inject chromatograph of liquid with microporous filter membrane (0.45 μ m), measure, the external standard two-point method calculates its content.The results are shown in Table 8.
The investigation that extracts after the table 8 different time reflux
| (g) weighs | Heat time heating time | Sample size (μ l) | Peak area | Content of hesperidin (mg/g preparation) |
| 4.6232 | 1 hour | 1 | 2272200 | 2.65 |
| 4.6277 | 3 hours | 1 | 2326503 | 2.70 |
| 4.6240 | 5 hours | 1 | 2546579 | 2.92 |
The result shows, the water reflux extracts extraction ratio after 5 hours the highest, and content of hesperidin is the 2.92mg/g preparation.
9.4 Different Extraction Method
The about 4.5g of sample thief (040511), porphyrize, accurate claim surely, the accurate methanol 50ml that adds adopts ultrasonic 45 minutes extracting method and the merceration method of spending the night to extract respectively, above-mentioned two kinds of extracting method solution are filtered, get subsequent filtrate and filter, promptly get need testing solution, inject chromatograph of liquid with microporous filter membrane (0.45 μ m), measure, the external standard two-point method calculates its content.The results are shown in Table 9.
The investigation of table 9 Different Extraction Method
| (g) weighs | Extracting method | Sample size (μ l) | Peak area | Content of hesperidin (mg/g preparation) |
| 5.3022 | Ultrasonic 45 minutes | 2 | 3612484 | 10.39 |
| 4.6229 | Merceration spends the night | 2 | 919832 | 3.95 |
The result shows that the ultrasonic method extraction ratio is the highest.Content of hesperidin is the 10.39mg/g preparation.
9.5 the investigation of ultrasonic extraction different extraction times
The about 0.3g of sample thief (040511), porphyrize, the accurate title, decide, put in the tool plug conical flask accurate methanol 50ml, the close plug of adding, claim to decide weight, supersound process (power 150W, frequency 20kHz) is after different time, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, filter, accurate absorption subsequent filtrate is quantitative, evaporate to dryness, with dissolve with methanol and be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter, get subsequent filtrate and filter, promptly get need testing solution, inject chromatograph of liquid with microporous filter membrane (0.45 μ m), measure, the external standard two-point method calculates its content.The results are shown in Table 10.
The investigation of table 10 different extraction times
| (g) weighs | The supersound extraction time | Sample size (μ l) | Get subsequent filtrate amount (ml) | Peak area | Content of hesperidin (mg/g preparation) |
| 0.3889 | 15 minutes | 5 | 30 | 2725911 | 7.36 |
| 0.3476 | 30 minutes | 4 | 30 | 2002486 | 7.93 |
| 0.3460 | 45 minutes | 4 | 20 | 1686080 | 10.38 |
| 0.3472 | 60 minutes | 4 | 30 | 2846451 | 10.70 |
| 0.3458 | 90 minutes | 4 | 20 | 1531749 | 9.62 |
The result shows that 60 minutes extraction ratios of supersound extraction are the highest.Content of hesperidin is the 10.70mg/g preparation.
The investigation result of comprehensive said extracted method, as can be known, the methanol supersound extraction was extracted the most complete in 60 minutes.
10, the response rate is investigated
Adopt the test of application of sample absorption method.(040511) 5 part in the sample that precision takes by weighing known content adds the Hesperidin reference substance respectively, presses under the text assay item preparation need testing solution and measures, and with the following formula calculate recovery rate, the results are shown in Table 11.
Response rate computing formula: (C-A)/B * 100%=response rate %
A: sample is contained measured
B: add pure product amount
C: measured value
Table 11 response rate is investigated
| Sample number | Sample weighting amount (g) | Content of hesperidin in the known sample (mg/g preparation) | Add Hesperidin amount (mg) | Content of hesperidin theoretical value (mg) | Content of hesperidin measured value (mg) | The response rate (%) | Average recovery rate (%) |
| 1 | 0.1802 | 10.9844 | 1.475 | 1.9794 | 3.4921 | 102.56 | 100.94 |
| 2 | 0.1796 | 1.475 | 1.9728 | 3.4236 | 98.36 | ||
| 3 | 0.1803 | 1.475 | 1.9805 | 3.4661 | 100.72 | ||
| 4 | 0.1803 | 1.4604 | 1.9805 | 3.4954 | 103.73 | ||
| 5 | 0.1805 | 1.4604 | 1.9827 | 3.4335 | 99.34 |
The determination of recovery rates result: average recovery rate is 100.94%, relative standard deviation RSD%=2.20%.
11, the mensuration of sample
Sample thief 040510,040511,040512, preparation method makes need testing solution with text need testing solution preparation.Accurate respectively reference substance solution 3 μ l, 6 μ l and the need testing solution 8 μ l of drawing inject chromatograph of liquid, measure under the chromatographic condition of drafting, and the external standard two-point method calculates Determination of Hesperidin Content in the preparation.The results are shown in Table 12.
The mensuration of table 12 sample
| Sample number | Sample weighting amount (g) | Peak area (1) | Peak area (2) | Average peak area | Content of hesperidin (mg/ sheet) |
| 040510 | 0.1847 | 2949863 | 3051753 | 3000808 | 9.24 |
| 040510 | 0.1806 | 2862567 | 2937082 | 2899824.5 | 9.13 |
| 040511 | 0.1723 | 2547425 | 2566273 | 2556849 | 8.52 |
| 040511 | 0.1566 | 2768504 | 2786177 | 2777340.5 | 8.56 |
| 040512 | 0.1617 | 2578017 | 2586661 | 2582339 | 8.99 |
| 040512 | 0.1745 | 2358026 | 2359397 | 2358711.5 | 9.05 |
Conclusion: according to the surely lower limit of the data of three batch samples, get then its 80%, the every least unit of YUSHUDA ZHIJI contain Pericarpium Citri Reticulatae with Hesperidin (C
28H
34O
15) meter, must not be less than 6.70mg.
The specific embodiment:
Embodiments of the invention 1:
Character: medicine or its content show light brown, gas perfume (or spice), mildly bitter flavor.
Differentiate: (1) gets YUSHUDA ZHIJI, and porphyrize claims 3.0g, adds chloroform 25ml, and supersound process is 10 minutes under power 150W, frequency 20kHz condition, is cooled to room temperature, filters, and the filtrate evaporate to dryness adds the 1ml ethyl acetate and makes dissolving, as need testing solution; Get the blank preparation 3.0g of Herba Pogostemonis, make the Herba Pogostemonis blank solution with method; Other gets Herba Pogostemonis control medicinal material 3.0g, shines medical material solution in pairs with legal system; According to the test of an appendix VIB of Pharmacopoeia of People's Republic of China version in 2000 thin layer chromatography, draw need testing solution, each 4 μ l of blank solution, control medicinal material solution 4 μ l put in same silica gel G F
254On the lamellae, with toluene: ethyl acetate: normal hexane: formic acid=2: 4: 8: 0.1 is developing solvent, launches, and takes out, and dries, and puts under the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color; Negative sample does not then show.
(2) get YUSHUDA ZHIJI, porphyrize claims 4.0g, adds chloroform 25ml, and supersound process is 10 minutes under power 150W, frequency 20kHz condition, is cooled to room temperature, filters, and the filtrate evaporate to dryness adds the 1ml ethyl acetate and makes dissolving, as need testing solution; Get the blank preparation 4.0g of Rhizoma Atractylodis, make the Rhizoma Atractylodis blank solution with method; Other gets Rhizoma Atractylodis control medicinal material 0.5g, shines medical material solution in pairs with legal system; Test according to an appendix VIB of Pharmacopoeia of People's Republic of China version in 2000 thin layer chromatography, draw need testing solution, each 10 μ l of blank solution, control medicinal material solution 6 μ l, point is on same silica gel g thin-layer plate, with toluene: ethyl acetate: normal hexane=1.5: 0.3: 7 be developing solvent, expansion, take out, dry, spray is with 5% phosphomolybdic acid-alcoholic solution, and 105 ℃ to be heated to speckle colour developing clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color; Negative sample does not then show.
(3) get YUSHUDA ZHIJI, porphyrize claims 2.0g, adds methanol 15ml, puts and heats jolting 5 minutes in the water-bath, filter, filtrate is put in the separatory funnel, adds the ethyl acetate jolting and extracts 2 times, each 10ml, merge extractive liquid,, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Get the blank preparation 2.0g of Semen Alpiniae Katsumadai, make the Semen Alpiniae Katsumadai blank solution with method; Get Semen Alpiniae Katsumadai control medicinal material 2.0g, shine medical material solution in pairs with legal system; Other gets the plain reference substance of Alpinia japonica (Thunb.) Miq., adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VIB of Pharmacopoeia of People's Republic of China version in 2000 thin layer chromatography, draw need testing solution, blank solution, each 10 μ l of control medicinal material solution, reference substance solution 2 μ l, point is on same silica gel g thin-layer plate, with chloroform: methanol=9: 0.5 is developing solvent, launches, and takes out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color; With the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color; Negative sample does not then show.
(4) get YUSHUDA ZHIJI, porphyrize claims 4.0g, adds methanol 25ml, and supersound process is 30 minutes under power 150W, frequency 20kHz condition, is cooled to room temperature, filters, and filtrate is as need testing solution; Get the blank preparation 4.0g of Pericarpium Citri Reticulatae, make the Pericarpium Citri Reticulatae blank solution with method; Get Pericarpium Citri Reticulatae control medicinal material 2.0g, shine medical material solution in pairs with legal system; Other gets the Hesperidin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VIB of Pharmacopoeia of People's Republic of China version in 2000 thin layer chromatography, draw need testing solution, blank solution, each 6 μ l of control medicinal material solution, reference substance solution 8 μ l, point is on same silica gel g thin-layer plate, with ethyl acetate: methanol: the upper solution of water=6: 1.5: 3 is developing solvent, launches, take out, dry, spray is put under the 365nm ultra-violet lamp and is inspected with the aluminum chloride test solution; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color; With the corresponding position of reference substance chromatograph on, show an identical yellow-green fluorescence speckle; Negative sample does not then show.
Check: should meet the pertinent regulations under each preparation item of appendix of Chinese Pharmacopoeia version in 2000.
Assay: shine 2000 editions one appendix VID high effective liquid chromatography for measuring of Chinese Pharmacopoeia:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile: 1% acetic acid aqueous solution=20: 80 is a mobile phase; The detection wavelength is 283nm; 30 ℃ of column temperatures; Number of theoretical plate calculates by the Hesperidin peak should be not less than 2000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the Hesperidin reference substance, adds methanol and make the solution that every 1ml contains 0.4mg, promptly;
The about 0.2g of YUSHUDA ZHIJI is got in the preparation of need testing solution, porphyrize, and accurate the title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, and supersound process is 1 hour under power 150W, frequency 20kHz condition, put coldly, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, precision is measured subsequent filtrate 30ml, evaporate to dryness, with dissolve with methanol and be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter, get subsequent filtrate and filter, promptly with 0.45 μ m microporous filter membrane;
Accurate respectively reference substance solution 3 μ l, 6 μ l and the need testing solution 8 μ l of drawing of algoscopy inject chromatograph of liquid, measure, and the external standard two-point method calculates, promptly;
The every least unit of YUSHUDA ZHIJI contains Pericarpium Citri Reticulatae with Hesperidin C
28H
34O
15Meter must not be less than 6.70mg.
Embodiments of the invention 2:
Character: medicine or its content show light brown, gas perfume (or spice), mildly bitter flavor.
Differentiate: get YUSHUDA ZHIJI, porphyrize claims 4.0g, adds chloroform 25ml, and supersound process is 10 minutes under power 150W, frequency 20kHz condition, is cooled to room temperature, filters, and the filtrate evaporate to dryness adds the 1ml ethyl acetate and makes dissolving, as need testing solution; Get the blank preparation 4.0g of Rhizoma Atractylodis, make the Rhizoma Atractylodis blank solution with method; Other gets Rhizoma Atractylodis control medicinal material 0.5g, shines medical material solution in pairs with legal system; Test according to an appendix VIB of Pharmacopoeia of People's Republic of China version in 2000 thin layer chromatography, draw need testing solution, each 10 μ l of blank solution, control medicinal material solution 6 μ l, point is on same silica gel g thin-layer plate, with toluene: ethyl acetate: normal hexane=1.5: 0.3: 7 be developing solvent, expansion, take out, dry, spray is with 5% phosphomolybdic acid-alcoholic solution, and 105 ℃ to be heated to speckle colour developing clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color; Negative sample does not then show.
Check: should meet the pertinent regulations under each preparation item of appendix of Chinese Pharmacopoeia version in 2000.
Assay: shine 2000 editions one appendix VID high effective liquid chromatography for measuring of Chinese Pharmacopoeia:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile: 1% acetic acid aqueous solution=20: 80 is a mobile phase; The detection wavelength is 283nm; 30 ℃ of column temperatures; Number of theoretical plate calculates by the Hesperidin peak should be not less than 2000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the Hesperidin reference substance, adds methanol and make the solution that every 1ml contains 0.4mg, promptly;
The about 0.2g of YUSHUDA ZHIJI is got in the preparation of need testing solution, porphyrize, and accurate the title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, and supersound process is 1 hour under power 150W, frequency 20kHz condition, put coldly, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, precision is measured subsequent filtrate 30ml, evaporate to dryness, with dissolve with methanol and be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter, get subsequent filtrate and filter, promptly with 0.45 μ m microporous filter membrane;
Accurate respectively reference substance solution 3 μ l, 6 μ l and the need testing solution 8 μ l of drawing of algoscopy inject chromatograph of liquid, measure, and the external standard two-point method calculates, promptly;
The every least unit of YUSHUDA ZHIJI contains Pericarpium Citri Reticulatae with Hesperidin C
28H
34O
15Meter must not be less than 6.70mg.
Embodiments of the invention 3:
Character: medicine or its content show light brown, gas perfume (or spice), mildly bitter flavor;
Differentiate: get YUSHUDA ZHIJI, porphyrize claims 2.0g, adds methanol 15ml, puts and heats jolting 5 minutes in the water-bath, filter, filtrate is put in the separatory funnel, adds the ethyl acetate jolting and extracts 2 times, each 10ml, merge extractive liquid,, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Get the blank preparation 2.0g of Semen Alpiniae Katsumadai, make the Semen Alpiniae Katsumadai blank solution with method; Get Semen Alpiniae Katsumadai control medicinal material 2.0g, shine medical material solution in pairs with legal system; Other gets the plain reference substance of Alpinia japonica (Thunb.) Miq., adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VIB of Pharmacopoeia of People's Republic of China version in 2000 thin layer chromatography, draw need testing solution, blank solution, each 10 μ l of control medicinal material solution, reference substance solution 2 μ l, point is on same silica gel g thin-layer plate, with chloroform: methanol=9: 0.5 is developing solvent, launches, and takes out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color; With the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color; Negative sample does not then show.
Check: should meet the pertinent regulations under each preparation item of appendix of Chinese Pharmacopoeia version in 2000.
Assay: shine 2000 editions one appendix VID high effective liquid chromatography for measuring of Chinese Pharmacopoeia:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile: 1% acetic acid aqueous solution=20: 80 is a mobile phase; The detection wavelength is 283nm; 30 ℃ of column temperatures; Number of theoretical plate calculates by the Hesperidin peak should be not less than 2000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the Hesperidin reference substance, adds methanol and make the solution that every 1ml contains 0.4mg, promptly;
The about 0.2g of YUSHUDA ZHIJI is got in the preparation of need testing solution, porphyrize, and accurate the title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, and supersound process is 1 hour under power 150W, frequency 20kHz condition, put coldly, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, precision is measured subsequent filtrate 30ml, evaporate to dryness, with dissolve with methanol and be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter, get subsequent filtrate and filter, promptly with 0.45 μ m microporous filter membrane;
Accurate respectively reference substance solution 3 μ l, 6 μ l and the need testing solution 8 μ l of drawing of algoscopy inject chromatograph of liquid, measure, and the external standard two-point method calculates, promptly;
The every least unit of YUSHUDA ZHIJI contains Pericarpium Citri Reticulatae with Hesperidin C
28H
34O
15Meter must not be less than 6.70mg.
Embodiments of the invention 4:
Character: medicine or its content show light brown, gas perfume (or spice), mildly bitter flavor.
Differentiate: (1) gets YUSHUDA ZHIJI, and porphyrize claims 3.0g, adds chloroform 25ml, and supersound process is 10 minutes under power 150W, frequency 20kHz condition, is cooled to room temperature, filters, and the filtrate evaporate to dryness adds the 1ml ethyl acetate and makes dissolving, as need testing solution; Get the blank preparation 3.0g of Herba Pogostemonis, make the Herba Pogostemonis blank solution with method; Other gets Herba Pogostemonis control medicinal material 3.0g, shines medical material solution in pairs with legal system; According to the test of an appendix VIB of Pharmacopoeia of People's Republic of China version in 2000 thin layer chromatography, draw need testing solution, each 4 μ l of blank solution, control medicinal material solution 4 μ l put in same silica gel G F
254On the lamellae, with toluene: ethyl acetate: normal hexane: formic acid=2: 4: 8: 0.1 is developing solvent, launches, and takes out, and dries, and puts under the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color; Negative sample does not then show.
(2) get YUSHUDA ZHIJI, porphyrize claims 4.0g, adds methanol 25ml, and supersound process is 30 minutes under power 150W, frequency 20kHz condition, is cooled to room temperature, filters, and filtrate is as need testing solution; Get the blank preparation 4.0g of Pericarpium Citri Reticulatae, make the Pericarpium Citri Reticulatae blank solution with method; Get Pericarpium Citri Reticulatae control medicinal material 2.0g, shine medical material solution in pairs with legal system; Other gets the Hesperidin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VIB of Pharmacopoeia of People's Republic of China version in 2000 thin layer chromatography, draw need testing solution, blank solution, each 6 μ l of control medicinal material solution, reference substance solution 8 μ l, point is on same silica gel g thin-layer plate, with ethyl acetate: methanol: the upper solution of water=6: 1.5: 3 is developing solvent, launches, take out, dry, spray is put under the 365nm ultra-violet lamp and is inspected with the aluminum chloride test solution; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color; With the corresponding position of reference substance chromatograph on, show an identical yellow-green fluorescence speckle; Negative sample does not then show.
Check: should meet the pertinent regulations under each preparation item of appendix of Chinese Pharmacopoeia version in 2000.
Embodiments of the invention 5:
Character: medicine or its content show light brown, gas perfume (or spice), mildly bitter flavor.
Check: should meet the pertinent regulations under each preparation item of appendix of Chinese Pharmacopoeia version in 2000.
Assay: shine 2000 editions one appendix VID high effective liquid chromatography for measuring of Chinese Pharmacopoeia:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile: 1% acetic acid aqueous solution=20: 80 is a mobile phase; The detection wavelength is 283nm; 30 ℃ of column temperatures; Number of theoretical plate calculates by the Hesperidin peak should be not less than 2000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the Hesperidin reference substance, adds methanol and make the solution that every 1ml contains 0.4mg, promptly;
The about 0.2g of YUSHUDA ZHIJI is got in the preparation of need testing solution, porphyrize, and accurate the title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, and supersound process is 1 hour under power 150W, frequency 20kHz condition, put coldly, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, precision is measured subsequent filtrate 30ml, evaporate to dryness, with dissolve with methanol and be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter, get subsequent filtrate and filter, promptly with 0.45 μ m microporous filter membrane;
Accurate respectively reference substance solution 3 μ l, 6 μ l and the need testing solution 8 μ l of drawing of algoscopy inject hplc determination, and the external standard two-point method calculates, promptly;
The every least unit of YUSHUDA ZHIJI contains Pericarpium Citri Reticulatae with Hesperidin C
28H
34O
15Meter must not be less than 6.70mg.
Claims (9)
1. method of quality control for the treatment of the YUSHUDA ZHIJI of depression, described preparation is all possible compound preparation of being made by Herba Pogostemonis 1000g, Pericarpium Citri Reticulatae 334g, Fructus Amomi Rotundus 500g, Semen Alpiniae Katsumadai 500g and parched with bran Rhizoma Atractylodis 666g that comprises capsule, tablet, granule, it is characterized in that: described method of quality control mainly comprises character, discriminating, inspection and assay project, and wherein the character item should meet the pertinent regulations under each preparation item; Differentiate that item is the discriminating to Herba Pogostemonis, Rhizoma Atractylodis, Semen Alpiniae Katsumadai, Pericarpium Citri Reticulatae; Check that item should meet the pertinent regulations under each preparation item of appendix of Chinese Pharmacopoeia version in 2000; The assay item is for measuring Determination of Hesperidin Content in the preparation.
2. according to the method for quality control of the YUSHUDA ZHIJI of the described treatment depression of claim 1, it is characterized in that: the discrimination method of Herba Pogostemonis is to be contrast with the Herba Pogostemonis control medicinal material, and with toluene: ethyl acetate: normal hexane: formic acid=2: 4: 8: 0.1 is the thin layer chromatography discrimination method of developing solvent.
3. according to the method for quality control of the YUSHUDA ZHIJI of the described treatment depression of claim 1, it is characterized in that: the discrimination method of Rhizoma Atractylodis is to be contrast with the Rhizoma Atractylodis control medicinal material, and with toluene: ethyl acetate: normal hexane=1.5: 0.3: 7 is the thin layer discrimination method of developing solvent.
4. according to the method for quality control of the YUSHUDA ZHIJI of the described treatment depression of claim 1, it is characterized in that: the discrimination method of Semen Alpiniae Katsumadai is to be contrast with the plain reference substance of Semen Alpiniae Katsumadai control medicinal material, Alpinia japonica (Thunb.) Miq., and with chloroform: methanol=9: 0.5 is the thin layer discrimination method of developing solvent.
5. according to the method for quality control of the YUSHUDA ZHIJI of the described treatment depression of claim 1, it is characterized in that: the discrimination method of Pericarpium Citri Reticulatae is to be contrast with Pericarpium Citri Reticulatae control medicinal material, Hesperidin reference substance, and with ethyl acetate: methanol: the upper solution of water=6: 1.5: 3 is the thin layer discrimination method of developing solvent.
6. according to the method for quality control of the YUSHUDA ZHIJI of claim 1,2,3,4 or 5 described treatment depressions, it is characterized in that: concrete discrimination method comprise following project partly or entirely:
(1) get YUSHUDA ZHIJI, porphyrize claims 3.0g, adds chloroform 25ml, and supersound process is 10 minutes under power 150W, frequency 20kHz condition, is cooled to room temperature, filters, and the filtrate evaporate to dryness adds the 1ml ethyl acetate and makes dissolving, as need testing solution; Get the blank preparation 3.0g of Herba Pogostemonis, make the Herba Pogostemonis blank solution with method; Other gets Herba Pogostemonis control medicinal material 3.0g, shines medical material solution in pairs with legal system; Test according to an appendix VIB of Pharmacopoeia of People's Republic of China version in 2000 thin layer chromatography, draw need testing solution, each 4 μ l of blank solution, control medicinal material solution 4 μ l, point is on same silica GF254 lamellae, with toluene: ethyl acetate: normal hexane: formic acid=2: 4: 8: 0.1 is developing solvent, launches, and takes out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color; Negative sample does not then show;
(2) get YUSHUDA ZHIJI, porphyrize claims 4.0g, adds chloroform 25ml, and supersound process is 10 minutes under power 150W, frequency 20kHz condition, is cooled to room temperature, filters, and the filtrate evaporate to dryness adds the 1ml ethyl acetate and makes dissolving, as need testing solution; Get the blank preparation 4.0g of Rhizoma Atractylodis, make the Rhizoma Atractylodis blank solution with method; Other gets Rhizoma Atractylodis control medicinal material 0.5g, shines medical material solution in pairs with legal system; Test according to an appendix VIB of Pharmacopoeia of People's Republic of China version in 2000 thin layer chromatography, draw need testing solution, each 10 μ l of blank solution, control medicinal material solution 6 μ l, point is on same silica gel g thin-layer plate, with toluene: ethyl acetate: normal hexane=1.5: 0.3: 7 be developing solvent, expansion, take out, dry, spray is with 5% phosphorus aluminic acid-alcoholic solution, and 105 ℃ to be heated to speckle colour developing clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color; Negative sample does not then show;
(3) get YUSHUDA ZHIJI, porphyrize claims 2.0g, adds methanol 15ml, puts and heats jolting 5 minutes in the water-bath, filter, filtrate is put in the separatory funnel, adds the ethyl acetate jolting and extracts 2 times, each 10ml, merge extractive liquid,, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Get the blank preparation 2.0g of Semen Alpiniae Katsumadai, make the Semen Alpiniae Katsumadai blank solution with method; Get Semen Alpiniae Katsumadai control medicinal material 2.0g, shine medical material solution in pairs with legal system; Other gets the plain reference substance of Alpinia japonica (Thunb.) Miq., adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VIB of Pharmacopoeia of People's Republic of China version in 2000 thin layer chromatography, draw need testing solution, blank solution, each 10 μ l of control medicinal material solution, reference substance solution 2 μ l, point is on same silica gel g thin-layer plate, with chloroform: methanol=9: 0.5 is developing solvent, launches, and takes out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color; With the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color; Negative sample does not then show;
(4) get YUSHUDA ZHIJI, porphyrize claims 4.0g, adds methanol 25ml, and supersound process is 30 minutes under power 150W, frequency 20kHz condition, is cooled to room temperature, filters, and filtrate is as need testing solution; Get the blank preparation 4.0g of Pericarpium Citri Reticulatae, make the Pericarpium Citri Reticulatae blank solution with method; Get Pericarpium Citri Reticulatae control medicinal material 2.0g, shine medical material solution in pairs with legal system; Other gets the Hesperidin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VIB of Pharmacopoeia of People's Republic of China version in 2000 thin layer chromatography, draw need testing solution, blank solution, each 6 μ l of control medicinal material solution, reference substance solution 8 μ l, point is on same silica gel g thin-layer plate, with ethyl acetate: methanol: the upper solution of water=6: 1.5: 3 is developing solvent, launches, take out, dry, spray is put under the 365nm ultra-violet lamp and is inspected with the aluminum chloride test solution; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color; With the corresponding position of reference substance chromatograph on, show an identical yellow-green fluorescence speckle; Negative sample does not then show.
7. according to the method for quality control of the YUSHUDA ZHIJI of the described treatment depression of claim 1, it is characterized in that: the Determination of Hesperidin Content assay method is to be contrast with the Hesperidin reference substance, and with acetonitrile: 1% acetic acid aqueous solution=20: 80 is the high performance liquid chromatography of mobile phase.
8. according to the method for quality control of claim 1 or 7 described YUSHUDA ZHIJI, it is characterized in that: concrete content assaying method is:
According to 2000 editions one appendix VI D of Chinese Pharmacopoeia high effective liquid chromatography for measuring:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile: 1% acetic acid aqueous solution=20: 80 is a mobile phase; The detection wavelength is 283nm; 30 ℃ of column temperatures; Number of theoretical plate calculates by the Hesperidin peak should be not less than 2000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the Hesperidin reference substance, adds methanol and make the solution that every 1ml contains 0.4mg, promptly;
The about 0.2g of YUSHUDA ZHIJI is got in the preparation of need testing solution, porphyrize, and accurate the title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, and supersound process is 1 hour under power 150W, frequency 20kHz condition, put coldly, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, precision is measured subsequent filtrate 30ml, evaporate to dryness, with dissolve with methanol and be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter, get subsequent filtrate and filter, promptly with 0.45 μ m microporous filter membrane;
Accurate respectively reference substance solution 3 μ l, 6 μ l and the need testing solution 8 μ l of drawing of algoscopy inject chromatograph of liquid, measure, and the external standard two-point method calculates, promptly;
The every least unit of YUSHUDA ZHIJI contains Pericarpium Citri Reticulatae in Hesperidin C28H34O15, must not be less than 6.70mg.
9. according to the method for quality control of the described YUSHUDA ZHIJI of claim 1, it is characterized in that: described character is:
Medicine or its content show light brown, gas perfume (or spice), mildly bitter flavor;
Discriminating is:
(1) get YUSHUDA ZHIJI, porphyrize claims 3.0g, adds chloroform 25ml, and supersound process is 10 minutes under power 150W, frequency 20kHz condition, is cooled to room temperature, filters, and the filtrate evaporate to dryness adds the 1ml ethyl acetate and makes dissolving, as need testing solution; Get the blank preparation 3.0g of Herba Pogostemonis, make the Herba Pogostemonis blank solution with method; Other gets Herba Pogostemonis control medicinal material 3.0g, shines medical material solution in pairs with legal system; Test according to an appendix VIB of Pharmacopoeia of People's Republic of China version in 2000 thin layer chromatography, draw need testing solution, each 4 μ l of blank solution, control medicinal material solution 4 μ l, point is on same silica GF254 lamellae, with toluene: ethyl acetate: normal hexane: formic acid=2: 4: 8: 0.1 is developing solvent, launches, and takes out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color; Negative sample does not then show;
(2) get YUSHUDA ZHIJI, porphyrize claims 4.0g, adds chloroform 25ml, and supersound process is 10 minutes under power 150W, frequency 20kHz condition, is cooled to room temperature, filters, and the filtrate evaporate to dryness adds the 1ml ethyl acetate and makes dissolving, as need testing solution; Get the blank preparation 4.0g of Rhizoma Atractylodis, make the Rhizoma Atractylodis blank solution with method; Other gets Rhizoma Atractylodis control medicinal material 0.5g, shines medical material solution in pairs with legal system; Test according to an appendix VIB of Pharmacopoeia of People's Republic of China version in 2000 thin layer chromatography, draw need testing solution, each 10 μ l of blank solution, control medicinal material solution 6 μ l, point is on same silica gel g thin-layer plate, with toluene: ethyl acetate: normal hexane=1.5: 0.3: 7 be developing solvent, expansion, take out, dry, spray is with 5% phosphomolybdic acid-alcoholic solution, and 105 ℃ to be heated to speckle colour developing clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color; Negative sample does not then show;
(3) get YUSHUDA ZHIJI, porphyrize claims 2.0g, adds methanol 15ml, puts and heats jolting 5 minutes in the water-bath, filter, filtrate is put in the separatory funnel, adds the ethyl acetate jolting and extracts 2 times, each 10ml, merge extractive liquid,, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Get the blank preparation 2.0g of Semen Alpiniae Katsumadai, make the Semen Alpiniae Katsumadai blank solution with method; Get Semen Alpiniae Katsumadai control medicinal material 2.0g, shine medical material solution in pairs with legal system; Other gets the plain reference substance of Alpinia japonica (Thunb.) Miq., adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VIB of Pharmacopoeia of People's Republic of China version in 2000 thin layer chromatography, draw need testing solution, blank solution, each 10 μ l of control medicinal material solution, reference substance solution 2 μ l, point is on same silica gel g thin-layer plate, with chloroform: methanol=9: 0.5 is developing solvent, launches, and takes out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color; With the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color; Negative sample does not then show;
(4) get YUSHUDA ZHIJI, porphyrize claims 4.0g, adds methanol 25ml, and supersound process is 30 minutes under power 150W, frequency 20kHz condition, is cooled to room temperature, filters, and filtrate is as need testing solution; Get the blank preparation 4.0g of Pericarpium Citri Reticulatae, make the Pericarpium Citri Reticulatae blank solution with method; Get Pericarpium Citri Reticulatae control medicinal material 2.0g, shine medical material solution in pairs with legal system; Other gets the Hesperidin reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VIB of Pharmacopoeia of People's Republic of China version in 2000 thin layer chromatography, draw need testing solution, blank solution, each 6 μ l of control medicinal material solution, reference substance solution 8 μ l, point is on same silica gel g thin-layer plate, with ethyl acetate: methanol: the upper solution of water=6: 1.5: 3 is developing solvent, launches, take out, dry, spray is put under the 365nm ultra-violet lamp and is inspected with the aluminum chloride test solution; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color; With the corresponding position of reference substance chromatograph on, show an identical yellow-green fluorescence speckle; Negative sample does not then show;
Inspection is: should meet the pertinent regulations under each preparation item of appendix of Chinese Pharmacopoeia version in 2000;
Assay: shine 2000 editions one appendix VI D of Chinese Pharmacopoeia high effective liquid chromatography for measuring:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile: 1% acetic acid aqueous solution=20: 80 is a mobile phase; The detection wavelength is 283nm; 30 ℃ of column temperatures; Number of theoretical plate calculates by the Hesperidin peak should be not less than 2000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the Hesperidin reference substance, adds methanol and make the solution that every 1ml contains 0.4mg, promptly;
The about 0.2g of YUSHUDA ZHIJI is got in the preparation of need testing solution, porphyrize, and accurate the title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, and supersound process is 1 hour under power 150W, frequency 20kHz condition, put coldly, claim again to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, precision is measured subsequent filtrate 30ml, evaporate to dryness, with dissolve with methanol and be transferred in the 5ml measuring bottle, add methanol to scale, shake up, filter, get subsequent filtrate and filter, promptly with 0.45 μ m microporous filter membrane;
Accurate respectively reference substance solution 3 μ l, 6 μ l and the need testing solution 8 μ l of drawing of algoscopy inject chromatograph of liquid, measure, and the external standard two-point method calculates, promptly;
The every least unit of YUSHUDA ZHIJI contains Pericarpium Citri Reticulatae in Hesperidin C28H34O15, must not be less than 6.70mg.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101596296B (en) * | 2008-06-02 | 2011-08-17 | 北京亚东生物制药有限公司 | Method for controlling quality of infant antidiarrheal granules |
| CN103142630A (en) * | 2013-03-21 | 2013-06-12 | 中国医学科学院药用植物研究所 | Application of hesperidin or derivatives thereof as antidepressant drug |
| CN104547873A (en) * | 2015-02-02 | 2015-04-29 | 刘平 | Method for preparing traditional Chinese medicine oral instant film for treating depression |
| CN110376326A (en) * | 2019-07-25 | 2019-10-25 | 河北中医学院 | A kind of multizone thin layer identification differentiating method of dried orange peel and Fructus Aurantii Immaturus |
| CN111487361A (en) * | 2020-04-20 | 2020-08-04 | 浙江金大康动物保健品有限公司 | Gradient full-information thin-layer identification method for rhizoma atractylodis medicinal material |
| CN112730698A (en) * | 2021-02-03 | 2021-04-30 | 仲景宛西制药股份有限公司 | Content determination method of traditional Chinese medicine preparation for treating depression |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1055238C (en) * | 1997-04-18 | 2000-08-09 | 宋杨 | Calming and desadening pill preparing process thereof |
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2005
- 2005-12-27 CN CNB2005102008668A patent/CN100464188C/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101596296B (en) * | 2008-06-02 | 2011-08-17 | 北京亚东生物制药有限公司 | Method for controlling quality of infant antidiarrheal granules |
| CN103142630A (en) * | 2013-03-21 | 2013-06-12 | 中国医学科学院药用植物研究所 | Application of hesperidin or derivatives thereof as antidepressant drug |
| CN104547873A (en) * | 2015-02-02 | 2015-04-29 | 刘平 | Method for preparing traditional Chinese medicine oral instant film for treating depression |
| CN110376326A (en) * | 2019-07-25 | 2019-10-25 | 河北中医学院 | A kind of multizone thin layer identification differentiating method of dried orange peel and Fructus Aurantii Immaturus |
| CN111487361A (en) * | 2020-04-20 | 2020-08-04 | 浙江金大康动物保健品有限公司 | Gradient full-information thin-layer identification method for rhizoma atractylodis medicinal material |
| CN112730698A (en) * | 2021-02-03 | 2021-04-30 | 仲景宛西制药股份有限公司 | Content determination method of traditional Chinese medicine preparation for treating depression |
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