CN102670728A - Quality control method for weeping forsythia seed soft capsules - Google Patents
Quality control method for weeping forsythia seed soft capsules Download PDFInfo
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Abstract
The invention relates to a quality control method for weeping forsythia seed soft capsules, and belongs to the technical field of medicaments. The quality control method specifically comprises an identification method and a content measurement method, wherein the identification method comprises character identification and thin-layer chromatography identification; the content measurement method is used for measuring forsythiaside content and alpha, beta-pinene content of the soft capsules; and the forsythiaside content is measured by adopting high performance liquid chromatography, and the alpha, beta-pinene content is measured by adopting gas chromatography. The method can be used for well controlling the quality of the weeping forsythia seed soft capsule product.
Description
Technical field
The present invention relates to a kind of method of quality control of Semen Fructus Forsythiae soft capsule, specifically comprise discrimination method and content assaying method, belong to medical technical field.
Background technology
On pharmaceutical technology, that pharmaceutical production will reach is safe and effective, quality stability, controlled basic demand.Perfect quality control standard can guarantee the reliability and the homogeneity of medicine.Medicine of the present invention is that a kind of from Semen Fructus Forsythiae, the extraction obtains, and has the Chinese medicinal soft capsule preparation of diseases such as treatment flu.
Oleaceae plant Fructus Forsythiae forsythia suspensa (Thunb.) Vahl is a traditional Chinese medical science heat and toxic materials clearing away medicine commonly used, always is regarded as persons particularly liable to develop skin infection's key medicine, its cold nature, and bitter in the mouth has the function of heat-clearing and toxic substances removing, dispersing swelling and dissipating binds.Fructus Forsythiae is one of clinical Chinese medicine commonly used of China; Modern pharmacological research shows that Fructus Forsythiae has antibiotic, heart tonifying, diuresis, town pharmacological action such as to tell; Be usually used in treating diseases such as acute anemopyretic cold, carbuncle sore tumefacting virus, tuberculous lymphadenitis, urinary tract infection, for waiting primary raw material of Chinese medicine preparation.The Chinese medicine preparation of relevant Fructus Forsythiae is compound recipe patent medicine mostly on the market, like SHUANGHUANGLIAN KOUFUYE, SHUANGHUANGLIAN FENZHENJI, QINGRE JIEDU KOUFUYE, the careless analgesic oral liquid of company, flos ionicerae and fructus forsythiae infusion for detoxication etc.
The Fructus Forsythiae medical material that Chinese Pharmacopoeia one one of version in 2005 is recorded is divided into green grass or young crops and sticks up and stick up two kinds always, and autumn, fruit was just ripely still gathered when band is green, removed impurity, cooked, and dried, and practised and claimed " green grass or young crops sticks up "; Gather when fruit is well-done, dry, remove impurity, practise and claim " sticking up always ".Green grass or young crops sticks up, and can keep Semen Fructus Forsythiae basically, and the Semen Fructus Forsythiae in sticking up always often is taken as impurity and removes.Tcm clinical practice is " sticking up always " mostly, removes OTC and writes " green grass or young crops sticks up " especially exactly.Therefore, a large amount of Semen Fructus Forsythiae resources are wasted.Discover that in recent years the volatile oil content in the Semen Fructus Forsythiae is higher, volatile oil has good antibacterial effect, external staphylococcus aureus is also had tangible antibacterial action.But do not find the related preparations of Semen Fructus Forsythiae in the market.
In addition, the inventor finds except volatile oil, to also have other active component also can bring into play the active constituents of medicine effect in the Semen Fructus Forsythiae in secular study of pharmacy.The inventor has been surprised to find that the soft capsule prepn and the method for preparing of a kind of abundant acquisition Semen Fructus Forsythiae active ingredient, has creatively proposed the method for quality control of said preparation simultaneously.
Summary of the invention
The method of quality control that the purpose of this invention is to provide a kind of Semen Fructus Forsythiae soft capsule can be controlled the quality of this Semen Fructus Forsythiae soft capsule through the method, well for this Semen Fructus Forsythiae soft capsule has been set up quality standard.
The Semen Fructus Forsythiae soft capsule that the present invention mentioned is prepared from through following method:
(1) get Semen Fructus Forsythiae, add 8 times of amounts of water (V/W), vapor distillation extracts volatile material, repeats 3 times, and the time was respectively 3 hours, 2 hours, 1 hour, after extraction finishes, merges volatile material, and airtight preservation gets extract A;
(2) water extract in (1) is merged, filter, filtrating is evaporated to relative density 1.05～1.10 in the time of 60 ℃, put cold; Add ethanol and make that to contain the alcohol amount be 80%, placement is spent the night, and gets the supernatant decompression recycling ethanol, is that every ml contains the 1.0g crude drug to concentrated solution concentration; Filter, AB-8 macroporous adsorbent resin on the filtrating, the control flow velocity is 0.5～1.5BV/h, the water with 5BV carries out remove impurity earlier; Use the 2BV80% ethanol elution then, collect eluent, concentrating under reduced pressure; 60-70 ℃ of vacuum drying pulverized, and promptly gets extract B;
(3) extract A and extract B are merged, promptly get active component C;
(4) with dispersant (a kind of or combination in soybean oil, Oleum Sesami, Oleum Brassicae campestris, safflower oil, Oleum Ricini, olive oil, Oleum Gossypii semen, Semen Maydis oil, perilla oil, the Oleum Arachidis hypogaeae semen) and suspending agent (a kind of or combination in Cera Flava, glyceryl monostearate, cocoa butter, castor oil hydrogenated, hydrogenated vegetable oil, the aluminum monostearate) heating and melting; After stirring; Be cooled to below 60 ℃, add C while stirring, mixture is crossed colloid mill or homogenizer; Make mixture cross the 100-200 eye mesh screen, subsequent use; Adjuvant (dispersant and suspending agent) weight ratio is 20-50% and 50-80% in active component C and the capsule.
(5) take by weighing gelatin, water, plasticizer, pigment, preparation capsule skin;
(6) compacting soft capsule, every 650mg.
For the quality of active ingredient in the effective described Semen Fructus Forsythiae soft capsule of control, the inventor's proposed to be described below technical scheme of method of quality control is read for ease, carries out proper number.
The method of quality control of said Semen Fructus Forsythiae soft capsule comprises a kind of or whole in the following discrimination method: character identification, thin layer chromatography differentiate, one or more compositions of content are carried out assay.
One, the character identification of said Semen Fructus Forsythiae soft capsule is following:
Soft capsule, content are the sepia suspension, acrid in the mouth, little hardship, tool special aroma.
Two, the thin layer chromatography of said Semen Fructus Forsythiae soft capsule differentiates with the Fructus Forsythiae ester glycoside to be reference substance, and step is following:
Thin layer chromatography test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B.
1. usually, thin layer chromatography differentiates that step is following:
Reference substance solution preparation: get the Fructus Forsythiae ester glycoside reference substance, use the methanol wiring solution-forming;
The need testing solution preparation: get soft capsule content and add normal hexane, ultrasonic 2 minutes, filter, discard normal hexane liquid, residue volatilizes, and adds methanol, and dissolving promptly gets;
Thin layer chromatography discrimination method: draw above-mentioned two kinds of solution; Putting respectively on same silica gel g thin-layer plate, is that developing solvent launches with acetone-ethyl acetate-water of 4-6: 4-6: 0.4-0.6, and taking-up is dried; After the ethanol solution of sulfuric acid colour developing; It is clear to be heated to speckle colour developing, put under the daylight and inspect, the test sample chromatograph with reference substance chromatograph relevant position on show the speckle of same color.
2. preferably, thin layer chromatography differentiates that step is following:
Reference substance solution preparation: get the Fructus Forsythiae ester glycoside reference substance, be made into the reference substance solution that 1ml contains arbitrary dosage among the 2.8-3.5mg with methanol;
Need testing solution preparation: get that arbitrary dosage adds normal hexane 10ml among the soft capsule content 1.0-1.5g in the beaker of 50ml, (250W 40HZ), filtered, and discarded normal hexane liquid, and residue volatilizes, and adds 10ml methanol, and dissolving promptly gets in ultrasonic 2 minutes;
Thin layer chromatography discrimination method: draw above-mentioned two kinds of solution, get the arbitrary point sample amount of 10-30 μ l, put respectively on same silica gel g thin-layer plate; With acetone-ethyl acetate of 5: 5: 0.5-water is that developing solvent launches; Taking-up is dried, and after the colour developing of 10% ethanol solution of sulfuric acid, 105 ℃ to be heated to the speckle colour developing clear; Put under the daylight and inspect, the test sample chromatograph with reference substance chromatograph relevant position on show the speckle of same color.
3. more preferably, thin layer chromatography differentiates that step is following:
Reference substance solution preparation: get the Fructus Forsythiae ester glycoside reference substance, be made into the reference substance solution that 1ml contains 3.21mg with methanol;
The need testing solution preparation: get soft capsule content 1.3g in the beaker of 50ml, add normal hexane 10ml, (250W 40HZ), filtered, and discarded normal hexane liquid, and residue volatilizes, and adds 10ml methanol, and dissolving promptly gets in ultrasonic 2 minutes;
Negative sample solution preparation: by above-mentioned Semen Fructus Forsythiae preparation of soft capsule method, do not add extract B, press the need testing solution method for preparing and handle, promptly get;
The thin layer chromatography discrimination method: drawing each 10 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, is that developing solvent launches with acetone-ethyl acetate of 5: 5: 0.5-water; Taking-up is dried; After the colour developing of 10% ethanol solution of sulfuric acid, 105 ℃ to be heated to the speckle colour developing clear, puts under the daylight and inspect; The test sample chromatograph with reference substance chromatograph relevant position on show the speckle of same color, negative control is noiseless.
Three, the content assaying method of said Semen Fructus Forsythiae soft capsule is to measure content and the α of Fructus Forsythiae ester glycoside, the content of nopinene; Wherein Fructus Forsythiae ester glycoside content adopts high effective liquid chromatography for measuring, and α, nopinene adopt gas chromatography to measure.
According to an appendix VI of Chinese Pharmacopoeia version in 2005 D HPLC, an appendix VI of Chinese Pharmacopoeia version in 2005 E gas chromatography determination.
1. usually, the content of the content of Fructus Forsythiae ester glycoside and α, nopinene is to adopt following method:
(1) Fructus Forsythiae ester glycoside assay
Chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filler; With methanol-0.2% glacial acetic acid is mobile phase; The detection wavelength is 290nm; Flow velocity 1ml/ minute; Number of theoretical plate calculates by the Fructus Forsythiae ester glycoside peak should be not less than 5000.
The preparation of reference substance solution: take by weighing the Fructus Forsythiae ester glycoside reference substance, add methanol and be mixed with solution, promptly get.
The preparation of need testing solution: get soft capsule content, add normal hexane, ultrasonic, filter, discard normal hexane liquid, residue volatilizes, and adds methanol, and is ultrasonic, filters, and promptly gets.
Algoscopy: draw reference substance solution and need testing solution, inject chromatograph of liquid, measure, promptly get.
(2) australene, the nopinene assay
Condition determination and system suitability test: adopt the HP-INNOWAX capillary chromatographic column; Detector is FID; With 40: 1 split sampling of split ratio; Sample introduction 1 μ l; Injector temperature: 240 ℃; Detector temperature: 300 ℃; Carrier gas: nitrogen; Make-up gas flow velocity: 25ml/ minute; The temperature programming condition: the column temperature initial temperature is 60 ℃, keeps 11 minutes, is warming up to 200 ℃ with 50 ℃/minute heating rates, keeps 5 minutes; Theoretical cam curve should be not less than 8000 in the nopinene peak.
The preparation of reference substance solution: take by weighing australene, the nopinene reference substance adds dehydrated alcohol and processes mixed solution, promptly gets;
The preparation of need testing solution: soft capsule content is added normal hexane, ultrasonic, shake up, filter, promptly get.
Algoscopy: draw reference substance solution and need testing solution inject gas chromatograph respectively, measure, promptly get.
2. preferably, the content of the content of Fructus Forsythiae ester glycoside and α, nopinene is to adopt following method:
(1) Fructus Forsythiae ester glycoside assay
Chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filler; With 32: 68 methanol-0.2% glacial acetic acid is mobile phase; The detection wavelength is 290nm; Flow velocity 1ml/ minute; Number of theoretical plate calculates by the Fructus Forsythiae ester glycoside peak should be not less than 5000.
The preparation of reference substance solution: precision takes by weighing the Fructus Forsythiae ester glycoside reference substance, adds 50% methanol and is mixed with the solution that every 1ml contains the arbitrary dosage of 35-45 μ g, promptly gets.
The preparation of need testing solution: get soft capsule content 90mg, the accurate title, decide, and places 50ml tool plug conical flask, the accurate normal hexane 5ml that adds; Ultrasonic 2 minutes, filter, discard normal hexane liquid, residue volatilizes; The accurate 50% methanol 50ml that adds claims to decide weight, ultrasonic 10 minutes; Supply weightlessness, 0.22 μ m filtering with microporous membrane promptly gets.
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly get.
(2) australene, the nopinene assay
Condition determination and system suitability test: adopt the HP-INNOWAX capillary chromatographic column; Detector is FID; With 40: 1 split sampling of split ratio; Sample introduction 1 μ l; Injector temperature: 240 ℃; Detector temperature: 300 ℃; Carrier gas: nitrogen; Make-up gas flow velocity: 25ml/ minute; The temperature programming condition: the column temperature initial temperature is 60 ℃, keeps 11 minutes, is warming up to 200 ℃ with 50 ℃/minute heating rates, keeps 5 minutes; Theoretical cam curve should be not less than 8000 in the nopinene peak.
The preparation of reference substance solution: take by weighing the australene reference substance; The nopinene reference substance; The accurate title, places two 10ml measuring bottles respectively surely, adds dehydrated alcohol and processes solution that contains the arbitrary concentration of australene 10-15mg/ml and the solution that contains the arbitrary concentration of nopinene 20-30mg/ml, shake up storing solution; Precision is measured the measuring bottle that above-mentioned storing solution 1ml places same 10ml respectively, behind the dehydrated alcohol standardize solution, shakes up, and promptly gets;
The preparation of need testing solution: with getting 3g behind the soft capsule content mixing, accurate title is in the tool plug conical flask of tool 50ml, and precision adds normal hexane 20ml, and ultrasonic 5 minutes, shake up, filter, promptly get.
Algoscopy: draw each 1 μ l inject gas chromatograph of reference substance solution and need testing solution respectively, measure, promptly get.
3. more preferably, the content of the content of Fructus Forsythiae ester glycoside and α, nopinene is to adopt following method:
(1) Fructus Forsythiae ester glycoside assay
Chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filler; With 32: 68 methanol-0.2% glacial acetic acid is mobile phase; The detection wavelength is 290nm; Flow velocity 1ml/ minute; Number of theoretical plate calculates by the Fructus Forsythiae ester glycoside peak should be not less than 5000.
The preparation of reference substance solution: precision takes by weighing the Fructus Forsythiae ester glycoside reference substance, adds 50% methanol and is mixed with the solution that every 1ml contains 40.56 μ g, promptly gets.
The preparation of need testing solution: get soft capsule content 90mg, the accurate title, decide, and places 50ml tool plug conical flask, the accurate normal hexane 5ml that adds; (250W 40Hz), filtered, and discarded normal hexane liquid in ultrasonic 2 minutes; Residue volatilizes, and the accurate 50% methanol 50ml that adds claims to decide weight, ultrasonic 10 minutes (250W; 40Hz), supply weightlessness, 0.22 μ m filtering with microporous membrane promptly gets.
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly get.
The Fructus Forsythiae ester glycoside content assaying method is investigated
The preparation of reference substance solution: precision takes by weighing the Fructus Forsythiae ester glycoside reference substance, adds 50% methanol and is mixed with the solution that every 1ml contains 40.56 μ g, promptly gets.
The preparation of need testing solution: get soft capsule content 90mg, the accurate title, decide, and places 50ml tool plug conical flask, the accurate normal hexane 5ml that adds; Ultrasonic 2 minutes, filter, discard normal hexane liquid, residue volatilizes; The accurate 50% methanol 50ml that adds claims to decide weight, ultrasonic 10 minutes; Supply weightlessness, 0.22 μ m filtering with microporous membrane promptly gets.
The preparation of negative sample solution: by above-mentioned Semen Fructus Forsythiae preparation of soft capsule method, do not add extract B, get 75mg, the accurate title, decide; Add 50% methanol solution 50ml, claim to decide weight, ultrasonic 10 minutes (250W, 40Hz); Supply weightlessness, microporous filter membrane (0.22 μ m) filters, and promptly gets.
One, the Fructus Forsythiae ester glycoside method is investigated
1, wavelength selection, specificity and system suitability are investigated
Get the Fructus Forsythiae ester glycoside reference substance solution, need testing solution and negative sample solution are blank with 50% methanol solution; Scan at 200～400nm respectively, the result shows that the need testing solution collection of illustrative plates is similar with the reference substance collection of illustrative plates; Its UV scanning collection of illustrative plates shows that the two all has absorption maximum at 290 ± 2nm place; And negative sample solution collection of illustrative plates does not have absworption peak in the relevant position, and explanation can use Fructus Forsythiae ester glycoside to be reference substance, and specificity is good.
System suitability is investigated: the accurate reference substance of drawing, and each 10 μ l sample introduction of (accompanying drawing 2) and test sample (accompanying drawing 3), the record collection of illustrative plates, the result shows that the separating degree at Fructus Forsythiae ester glycoside peak is good, theoretical cam curve is 15000, meets the assay requirement.Other gets negative need testing solution sample introduction, and negative test sample chromatogram does not have respective peaks and occurs at Fructus Forsythiae ester glycoside peak position place, explain that under this chromatographic condition, the specificity of content assaying method is good.
2, the selection of mobile phase
Selected for use and measured the high-efficient liquid phase technique of effective site and increased low amounts of water; Measured the preparation test sample; Result of the test shows; Fructus Forsythiae ester glycoside chromatographic peak and adjacent chromatographic peak have peak shape and separating degree preferably, so select the method to measure, the mobile phase of promptly selecting is methanol-0.2% glacial acetic acid (32: 68).
3, linear relationship is investigated:
Precision is measured reference substance solution 1ml and is placed in 2ml, 5ml, 10ml, 20ml, the 50ml volumetric flask; Add 50% methanol and be diluted to scale; Shake up, processing concentration is the solution of 8.112 μ g/ml, 20.28 μ g/ml, 40.56 μ g/ml, 81.12 μ g/ml, 202.8 μ g/ml and 405.6 μ g/ml.The above-mentioned solution 10 μ l of accurate respectively absorption inject high performance liquid chromatograph; Measure by above-mentioned chromatographic condition; With the peak area integrated value is vertical coordinate; Fructus Forsythiae ester glycoside reference substance sample size is that abscissa carries out linear regression, calculates regression equation: Y=1181.1X-4.0143, correlation coefficient r=1.0000; Show that Fructus Forsythiae ester glycoside is good in 0.08112～4.056 μ g scope internal linear relation.Measure the result and see table 1.
Table 1 linear relationship is investigated the result
4, precision is investigated
Get Fructus Forsythiae ester glycoside reference substance solution (40.56 μ g/ml), press linear relationship and investigate item method mensuration down, continuous sample introduction 6 times, each sample introduction 10 μ l, the result shows that instrument precision is good, the result sees table 2.
Table 2 Precision test result
5, study on the stability
Precision take by weighing test sample (lot number: 20080310) 90.34mg, press text need testing solution method for preparing preparation.The accurate need testing solution 10 μ l that draw, respectively at 0,2,4,6,8 hour sample introduction, the record peak area, the result shows that need testing solution is stable in 8 hours, can satisfy and measure requirement, the result sees table 3.
Table 3 study on the stability result
6, replica test:
6 parts of parallel samplings are pressed the test sample method for preparing and are handled, and measure content, and result of the test shows that the repeatability of this method is good, and the result sees table 4.
Table 4 repeatability is investigated the result
7, application of sample recovery test
Sample thief (content: 29.23mg/g) 9 parts, the accurate title, decide, and adds each three parts of Fructus Forsythiae ester glycoside reference substances respectively, according to the operation of need testing solution processing method, measures content, the calculating average recovery, and the result sees table 5.
Table 5 application of sample recovery test result
Two, australene, the nopinene method is investigated
Condition determination and system suitability test: adopt the HP-INNOWAX capillary chromatographic column; Detector is FID; With 40: 1 split sampling of split ratio; Sample introduction 1 μ l; Injector temperature: 240 ℃; Detector temperature: 300 ℃; Carrier gas: nitrogen; Make-up gas flow velocity: 25ml/ minute.The temperature programming condition: the column temperature initial temperature is 60 ℃, keeps 11 minutes, is warming up to 200 ℃ with 50 ℃/minute heating rates, keeps 5 minutes.Theoretical cam curve should be not less than 8000 in the nopinene peak.
The preparation of reference substance solution: take by weighing the about 0.14g of australene reference substance; The about 0.26g of nopinene reference substance; The accurate title, places two 10ml measuring bottles respectively surely, adds dehydrated alcohol and processes solution that contains australene 13mg/ml and the solution that contains nopinene 25mg/ml, shake up storing solution.Precision is measured the measuring bottle that above-mentioned storing solution 1ml places same 10ml respectively, behind the dehydrated alcohol standardize solution, shakes up, and promptly gets;
The preparation of need testing solution: with getting 3g behind the soft capsule content mixing, accurate title is in the tool plug conical flask of 50ml, and precision adds normal hexane 20ml, and (250W 40HZ), shook up, and filtered, and promptly got in ultrasonic 5 minutes.
The preparation of negative sample solution: press Semen Fructus Forsythiae preparation of soft capsule method, do not add extract A, press the need testing solution method for preparing and handle; Get 3g, the accurate title in the ground triangular flask of 50ml, the accurate normal hexane 20ml that adds; (250W 40HZ), shook up in ultrasonic 5 minutes; Leave standstill the filtering with microporous membrane of back slightly, promptly get with 0.22 μ m.
Algoscopy: accurate respectively reference substance solution and each 1 μ l of need testing solution, inject gas chromatograph, australene in the working sample, the content of nopinene drawn.
1, chromatographic condition
Chromatographic column: HP-INNOWax type capillary column (30m * 0.53mm * 1.0 μ m), immobile phase is a Polyethylene Glycol, U.S. Agilent company.
Column temperature: temperature programming, initial temperature are 60 ℃, keep 11 minutes, rise to 200 ℃ with 50 ℃ of per minutes, keep 5 minutes.Detector temperature: 300 ℃; Injector temperature: 240 ℃; Shunting: split ratio is 40: 1; Column flow rate: 4.0ml/min; Carrier gas: nitrogen.
2, the preparation of reference substance and need testing solution
The preparation of reference substance solution: take by weighing the about 0.14g of australene reference substance; The about 0.26g of nopinene reference substance; The accurate title, places two 10ml measuring bottles respectively surely, adds dehydrated alcohol and processes solution that contains australene 13mg/ml and the solution that contains nopinene 25mg/ml, shake up storing solution.Precision is measured the measuring bottle that above-mentioned storing solution 1ml places same 10ml respectively, behind the dehydrated alcohol standardize solution, shakes up, and promptly gets.
The preparation of need testing solution: with getting 3g behind the content mixing under these article content uniformity item, the accurate title in the tool plug conical flask of 50ml, the accurate normal hexane 20ml that adds; (250W 40HZ), shook up in ultrasonic 5 minutes; Leave standstill the filtering with microporous membrane of back slightly, promptly get with 0.22 μ m.
The preparation of negative sample solution: press Semen Fructus Forsythiae preparation of soft capsule method, do not add extract A, press the need testing solution method for preparing and handle; Get 3g, the accurate title in the ground triangular flask of 50ml, the accurate normal hexane 20ml that adds; (250W 40HZ), shook up in ultrasonic 5 minutes; Leave standstill the filtering with microporous membrane of back slightly, promptly get with 0.22 μ m.
3, specificity test
The solvent for use normal hexane, dehydrated alcohol is noiseless to determinand, and impurity peaks does not disturb determinand in the sample (accompanying drawing 4,5); Determinand peak and Interference Peaks do not appear in the negative sample; Australene figure, the separating degree of nopinene figure and adjacent peak meets the requirements, and explains that this law specificity is strong.
4, linear relationship is investigated
The preparation of series standard liquid
Precision takes by weighing australene reference substance 0.13760g, and nopinene reference substance 0.24328g places the 10ml measuring bottle respectively, adds dehydrated alcohol and processes solution that contains australene 13.4848mg/ml and the reference substance storing solution that contains nopinene 23.8414mg/ml.Accurately respectively measure the measuring bottle that above-mentioned storing solution 5ml places same 10ml, shake up, promptly get contain australene 6.7424mg/ml and nopinene 11.9207mg/ml the mixing reference substance solution 6..
The respectively accurate reference substance solution of drawing is 6. in 1ml to 2ml, 5ml, 10ml, 20ml, the 50ml measuring bottle; Add dehydrated alcohol to scale; Shake up; Make respectively and contain australene 3.3712mg/ml and the reference substance solution that contains nopinene 5.9604mg/ml 5., the reference substance solution that contains australene 1.3485mg/ml and nopinene 2.3841mg/ml 4., the reference substance solution that contains australene 0.6742mg/ml and nopinene 1.1921mg/ml is 3.; The reference substance solution that contains australene 0.3371mg/ml and nopinene 0.5960mg/ml 2., the reference substance solution that contains australene 0.1348mg/ml and nopinene 0.2384mg/ml is 1..
The drafting of standard curve: accurate respectively each the 1 μ l of above-mentioned series standard liquid that draws, sample introduction analysis, record peak area.With constituent concentration to be measured is abscissa, and peak area is a vertical coordinate, and the drawing standard curve is seen table 6.
Table 6 standard curve
Standard curve equation: australene y=454.04x+12.837 (r=0.9999)
Nopinene y=450.09x+22.372 (r=0.9999)
The range of linearity
The above results shows: australene is at 0.1348～6.7424 μ g, and nopinene is good in 0.2384～11.9207 μ g scope internal linear relation, so adopt the external standard single-point method to carry out quantitatively.
5, precision test
Get and contain australene 0.6742mg/ml, the reference substance solution continuous sample introduction of nopinene 1.1921mg/ml 6 times calculates the RSD value, and the result sees table 7.
The test of table 7 precision
6, replica test
6 parts of these article of getting prepare need testing solution by the method for working out respectively, and sample introduction is measured, and calculate content, and the result sees table 8.
Table 8 replica test
7, stability test
These article of getting (lot number: 20080310), prepare need testing solution, measure in 0,1,2,3,4 hour sample introduction by the method for working out, the record peak area, the result shows that need testing solution is stable in 4 hours, the result sees table 9.
Table 9 stability test
8, recovery test
These article of getting (lot number: 20080310, content is australene 6.85mg/g, nopinene 15.40mg/g) 1.5g; Parallel nine parts; Add respectively 3 parts of reference substance solution (australene 2.2462mg/ml, nopinene 5.0230mg/ml) 4ml, 5ml, 6ml respectively, measure content by working out method; Calculate recovery rate, the result sees table 10.
Table 10 recovery test
Recovery test is the result show: this law response rate is good, and accuracy is high.
Figure of description
Fig. 1 soft capsule content thin-layer chromatogram of the present invention;
Fig. 2 Fructus Forsythiae ester glycoside reference substance high performance liquid chromatogram collection of illustrative plates;
Fig. 3 soft capsule content high performance liquid chromatogram of the present invention collection of illustrative plates;
Fig. 4 australene, nopinene reference substance gas chromatogram;
Fig. 5 soft capsule content gas chromatogram of the present invention.
The specific embodiment
Embodiment 1 thin layer chromatography is differentiated
Reference substance solution preparation: get the Fructus Forsythiae ester glycoside reference substance, be made into the reference substance solution that 1ml contains 3.21mg with methanol;
The need testing solution preparation: get soft capsule content 1.3g in the beaker of 50ml, add normal hexane 10ml, (250W 40HZ), filtered, and discarded normal hexane liquid, and residue volatilizes, and adds 10ml methanol, and dissolving promptly gets in ultrasonic 2 minutes;
Negative sample solution preparation: press Semen Fructus Forsythiae preparation of soft capsule method, do not add extract B, press the need testing solution method for preparing and handle, promptly get;
Thin layer chromatography discrimination method: according to the thin layer chromatography test of an appendix VI of Chinese Pharmacopoeia version in 2005 B, draw each 10 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate; With acetone-ethyl acetate of 5: 5: 0.5-water is that developing solvent launches, and taking-up is dried, after 10% ethanol solution of sulfuric acid colour developing; 105 ℃ to be heated to speckle colour developing clear; Put under the daylight and inspect, the test sample chromatograph with reference substance chromatograph relevant position on show the speckle of same color, negative control is noiseless.(seeing accompanying drawing 1)
Reference substance solution preparation: get the Fructus Forsythiae ester glycoside reference substance, be made into the reference substance solution that 1ml contains 2.8mg with methanol;
The need testing solution preparation: get soft capsule content 1.0g in the beaker of 50ml, add normal hexane 10ml, (250W 40HZ), filtered, and discarded normal hexane liquid, and residue volatilizes, and adds 10ml methanol, and dissolving promptly gets in ultrasonic 2 minutes;
Negative sample solution preparation: press Semen Fructus Forsythiae preparation of soft capsule method, do not add extract B, press the need testing solution method for preparing and handle, promptly get;
Thin layer chromatography discrimination method: according to the thin layer chromatography test of an appendix VI of Chinese Pharmacopoeia version in 2005 B, draw each 10 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate; With acetone-ethyl acetate of 5: 5: 0.5-water is that developing solvent launches, and taking-up is dried, after 10% ethanol solution of sulfuric acid colour developing; 105 ℃ to be heated to speckle colour developing clear; Put under the daylight and inspect, the test sample chromatograph with reference substance chromatograph relevant position on show the speckle of same color, negative control is noiseless.
Embodiment 3 thin layer chromatographys are differentiated
Reference substance solution preparation: get the Fructus Forsythiae ester glycoside reference substance, be made into the reference substance solution that 1ml contains 3.5mg with methanol;
The need testing solution preparation: get soft capsule content 1.5g in the beaker of 50ml, add normal hexane 10ml, (250W 40HZ), filtered, and discarded normal hexane liquid, and residue volatilizes, and adds 10ml methanol, and dissolving promptly gets in ultrasonic 2 minutes;
Negative sample solution preparation: press Semen Fructus Forsythiae preparation of soft capsule method, do not add extract B, press the need testing solution method for preparing and handle, promptly get;
Thin layer chromatography discrimination method: according to the thin layer chromatography test of an appendix VI of Chinese Pharmacopoeia version in 2005 B; Drawing each 30 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, is that developing solvent launches with acetone-ethyl acetate of 5.5: 5: 0.6-water; Taking-up is dried; After the colour developing of 10% ethanol solution of sulfuric acid, 105 ℃ to be heated to the speckle colour developing clear, puts under the daylight and inspect; The test sample chromatograph with reference substance chromatograph relevant position on show the speckle of same color, negative control is noiseless.
Embodiment 4 Fructus Forsythiae ester glycoside assays
Method for preparing by need testing solution prepares need testing solution, measures three lot sample article by method under the linear relationship investigation item, and every lot sample article are parallel to be done 2 times, and the result sees table 11.
Fructus Forsythiae ester glycoside assay result in the table 11 three lot sample article
Embodiment 5 australenes, the nopinene assay
Accurate respectively reference substance solution and each 1 μ l of need testing solution of drawing, inject gas chromatograph is pressed australene in the summary of the invention prescriptive procedure working sample, the content of nopinene.3 lot sample article assay results see table 12.
The assay result of α, nopinene in the table 12 three lot sample article
Claims (9)
1. the method for quality control of a Semen Fructus Forsythiae soft capsule is characterized in that comprising a kind of or whole in the following discrimination method: character identification, thin layer chromatography differentiate, one or more compositions of content are carried out assay.
2. according to the method for quality control of the said a kind of Semen Fructus Forsythiae soft capsule of claim 1, it is characterized in that character identification is following: soft capsule, content are the sepia suspension, acrid in the mouth, little hardship, tool special aroma.
3. according to the method for quality control of the said a kind of Semen Fructus Forsythiae soft capsule of claim 1, it is characterized in that thin layer chromatography discriminating step is following:
Reference substance solution preparation: get the Fructus Forsythiae ester glycoside reference substance, use the methanol wiring solution-forming;
The need testing solution preparation: get soft capsule content and add normal hexane, ultrasonic 2 minutes, filter, discard normal hexane liquid, residue volatilizes, and adds methanol, and dissolving promptly gets;
Thin layer chromatography discrimination method: draw above-mentioned two kinds of solution; Putting respectively on same silica gel g thin-layer plate, is that developing solvent launches with acetone-ethyl acetate-water of 4-6: 4-6: 0.4-0.6, and taking-up is dried; After the ethanol solution of sulfuric acid colour developing; It is clear to be heated to speckle colour developing, put under the daylight and inspect, the test sample chromatograph with reference substance chromatograph relevant position on show the speckle of same color.
4. according to the method for quality control of the said a kind of Semen Fructus Forsythiae soft capsule of claim 3, it is characterized in that thin layer chromatography discriminating step is following:
Reference substance solution preparation: get the Fructus Forsythiae ester glycoside reference substance, be made into the reference substance solution that 1ml contains arbitrary dosage among the 2.8-3.5mg with methanol;
Need testing solution preparation: get that arbitrary dosage adds normal hexane 10ml among the soft capsule content 1.0-1.5g in the beaker of 50ml, ultrasonic 2 minutes, filter, discard normal hexane liquid, residue volatilizes, and adds 10ml methanol, and dissolving promptly gets;
Thin layer chromatography discrimination method: draw above-mentioned two kinds of solution, get the arbitrary point sample amount of 10-30 μ l, put respectively on same silica gel g thin-layer plate; With acetone-ethyl acetate of 5: 5: 0.5-water is that developing solvent launches; Taking-up is dried, and after the colour developing of 10% ethanol solution of sulfuric acid, 105 ℃ to be heated to the speckle colour developing clear; Put under the daylight and inspect, the test sample chromatograph with reference substance chromatograph relevant position on show the speckle of same color.
5. according to the method for quality control of the said a kind of Semen Fructus Forsythiae soft capsule of claim 4, it is characterized in that thin layer chromatography discriminating step is following:
Reference substance solution preparation: get the Fructus Forsythiae ester glycoside reference substance, be made into the reference substance solution that 1ml contains 3.21mg with methanol;
The need testing solution preparation: get soft capsule content 1.3g in the beaker of 50ml, add normal hexane 10ml, ultrasonic 2 minutes, filter, discard normal hexane liquid, residue volatilizes, and adds 10ml methanol, and dissolving promptly gets;
Thin layer chromatography discrimination method: draw each 10 μ l of above-mentioned two kinds of solution; Putting respectively on same silica gel g thin-layer plate, is that developing solvent launches with acetone-ethyl acetate of 5: 5: 0.5-water, and taking-up is dried; After 10% ethanol solution of sulfuric acid colour developing; 105 ℃ to be heated to speckle colour developing clear, put under the daylight and inspect, the test sample chromatograph with reference substance chromatograph relevant position on show the speckle of same color.
6. according to the method for quality control of the said a kind of Semen Fructus Forsythiae soft capsule of claim 1, it is characterized in that the Fructus Forsythiae ester glycoside content in the content and α, nopinene content are measured; Wherein Fructus Forsythiae ester glycoside content adopts high effective liquid chromatography for measuring, and α, nopinene adopt gas chromatography to measure.
7. according to the method for quality control of the said a kind of Semen Fructus Forsythiae soft capsule of claim 6, it is characterized in that Fructus Forsythiae ester glycoside content and α, nopinene assay adopt following method:
(1) Fructus Forsythiae ester glycoside assay
Chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filler; With methanol-0.2% glacial acetic acid is mobile phase; The detection wavelength is 290nm; Flow velocity 1ml/ minute; Number of theoretical plate calculates by the Fructus Forsythiae ester glycoside peak should be not less than 5000;
The preparation of reference substance solution: take by weighing the Fructus Forsythiae ester glycoside reference substance, add methanol and be mixed with solution, promptly get;
The preparation of need testing solution: get soft capsule content, add normal hexane, ultrasonic, filter, discard normal hexane liquid, residue volatilizes, and adds methanol, and is ultrasonic, filters, and promptly gets;
Algoscopy: draw reference substance solution and need testing solution, inject chromatograph of liquid, measure, promptly get.
(2) australene, the nopinene assay
Condition determination and system suitability test: adopt the HP-INNOWAX capillary chromatographic column; Detector is FID; With 40: 1 split sampling of split ratio; Sample introduction 1 μ l; Injector temperature: 240 ℃; Detector temperature: 300 ℃; Carrier gas: nitrogen; Make-up gas flow velocity: 25ml/ minute; The temperature programming condition: the column temperature initial temperature is 60 ℃, keeps 11 minutes, is warming up to 200 ℃ with 50 ℃/minute heating rates, keeps 5 minutes; Theoretical cam curve should be not less than 8000 in the nopinene peak.
The preparation of reference substance solution: take by weighing australene, the nopinene reference substance adds dehydrated alcohol and processes mixed solution, promptly gets;
The preparation of need testing solution: soft capsule content is added normal hexane, ultrasonic, shake up, filter, promptly get.
Algoscopy: draw reference substance solution and need testing solution inject gas chromatograph respectively, measure, promptly get.
8. according to the method for quality control of the said a kind of Semen Fructus Forsythiae soft capsule of claim 7, it is characterized in that α, nopinene content and Fructus Forsythiae ester glycoside assay adopt following method:
(1) Fructus Forsythiae ester glycoside assay
Chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filler; With 32: 68 methanol-0.2% glacial acetic acid is mobile phase; The detection wavelength is 290nm; Flow velocity 1ml/ minute; Number of theoretical plate calculates by the Fructus Forsythiae ester glycoside peak should be not less than 5000.
The preparation of reference substance solution: precision takes by weighing the Fructus Forsythiae ester glycoside reference substance, adds 50% methanol and is mixed with the solution that every 1ml contains the arbitrary dosage of 35-45 μ g, promptly gets.
The preparation of need testing solution: get soft capsule content 90mg, the accurate title, decide, and places 50ml tool plug conical flask, the accurate normal hexane 5ml that adds; Ultrasonic 2 minutes, filter, discard normal hexane liquid, residue volatilizes; The accurate 50% methanol 50ml that adds claims to decide weight, ultrasonic 10 minutes; Supply weightlessness, 0.22 μ m filtering with microporous membrane promptly gets.
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly get.
(2) australene, the nopinene assay
Condition determination and system suitability test: adopt the HP-INNOWAX capillary chromatographic column; Detector is FID; With 40: 1 split sampling of split ratio; Sample introduction 1 μ l; Injector temperature: 240 ℃; Detector temperature: 300 ℃; Carrier gas: nitrogen; Make-up gas flow velocity: 25ml/ minute; The temperature programming condition: the column temperature initial temperature is 60 ℃, keeps 11 minutes, is warming up to 200 ℃ with 50 ℃/minute heating rates, keeps 5 minutes; Theoretical cam curve should be not less than 8000 in the nopinene peak.
The preparation of reference substance solution: take by weighing the australene reference substance; The nopinene reference substance; The accurate title, places two 10ml measuring bottles respectively surely, adds dehydrated alcohol and processes solution that contains the arbitrary concentration of australene 10-15mg/ml and the solution that contains the arbitrary concentration of nopinene 20-30mg/ml, shake up storing solution; Precision is measured the measuring bottle that above-mentioned storing solution 1ml places same 10ml respectively, behind the dehydrated alcohol standardize solution, shakes up, and promptly gets;
The preparation of need testing solution: with getting 3g behind the soft capsule content mixing, accurate title is in the tool plug conical flask of tool 50ml, and precision adds normal hexane 20ml, and ultrasonic 5 minutes, shake up, filter, promptly get.
Algoscopy: draw each 1 μ l inject gas chromatograph of reference substance solution and need testing solution respectively, measure, promptly get.
9. the method for quality control of said according to Claim 8 a kind of Semen Fructus Forsythiae soft capsule is characterized in that α, nopinene content and Fructus Forsythiae ester glycoside assay adopt following method:
(1) Fructus Forsythiae ester glycoside assay
Chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filler; With 32: 68 methanol-0.2% glacial acetic acid is mobile phase; The detection wavelength is 290nm; Flow velocity 1ml/ minute; Number of theoretical plate calculates by the Fructus Forsythiae ester glycoside peak should be not less than 5000.
The preparation of reference substance solution: precision takes by weighing the Fructus Forsythiae ester glycoside reference substance, adds 50% methanol and is mixed with the solution that every 1ml contains 40.56 μ g, promptly gets.
The preparation of need testing solution: get soft capsule content 90mg, the accurate title, decide, and places 50ml tool plug conical flask, the accurate normal hexane 5ml that adds; Ultrasonic 2 minutes, filter, discard normal hexane liquid, residue volatilizes; The accurate 50% methanol 50ml that adds claims to decide weight, ultrasonic 10 minutes; Supply weightlessness, 0.22 μ m filtering with microporous membrane promptly gets.
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly get.
(2) australene, the nopinene assay
Condition determination and system suitability test: adopt the HP-INNOWAX capillary chromatographic column; Detector is FID; With 40: 1 split sampling of split ratio; Sample introduction 1 μ l; Injector temperature: 240 ℃; Detector temperature: 300 ℃; Carrier gas: nitrogen; Make-up gas flow velocity: 25ml/ minute; The temperature programming condition: the column temperature initial temperature is 60 ℃, keeps 11 minutes, is warming up to 200 ℃ with 50 ℃/minute heating rates, keeps 5 minutes; Theoretical cam curve should be not less than 8000 in the nopinene peak.
The preparation of reference substance solution: take by weighing australene reference substance 0.14g; Nopinene reference substance 0.26g; The accurate title, places two 10ml measuring bottles respectively surely, adds dehydrated alcohol and processes solution that contains australene 13mg/ml and the solution that contains nopinene 25mg/ml, shake up storing solution; Precision is measured the measuring bottle that above-mentioned storing solution 1ml places same 10ml respectively, behind the dehydrated alcohol standardize solution, shakes up, and promptly gets;
The preparation of need testing solution: with getting 3g behind the soft capsule content mixing, accurate title is in the tool plug conical flask of 50ml, and precision adds normal hexane 20ml, and ultrasonic 5 minutes, shake up, filter, promptly get;
Algoscopy: draw each 1 μ l inject gas chromatograph of reference substance solution and need testing solution respectively, measure, promptly get.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104931642A (en) * | 2015-06-18 | 2015-09-23 | 河北中医学院 | Rapid multi-information thin-layer identification method of fructus forsythiae medical material and water extract of fructus forsythiae medical material |
| CN112946113A (en) * | 2021-02-01 | 2021-06-11 | 湖北医药学院 | Method for identifying genuine medicinal material Shiweir fructus forsythiae basal source |
| CN114113419A (en) * | 2020-08-26 | 2022-03-01 | 尚科生物医药（上海）有限公司 | Chromatographic separation method of saxagliptin and isomer thereof |
| CN115236239A (en) * | 2022-08-09 | 2022-10-25 | 多特瑞(上海)商贸有限公司 | Method for detecting content of alpha-copal in schisandra essential oil |
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2011
- 2011-03-18 CN CN2011100656074A patent/CN102670728A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104931642A (en) * | 2015-06-18 | 2015-09-23 | 河北中医学院 | Rapid multi-information thin-layer identification method of fructus forsythiae medical material and water extract of fructus forsythiae medical material |
| CN104931642B (en) * | 2015-06-18 | 2016-10-05 | 河北中医学院 | A kind of Fructus Forsythiae medical material and the quick multi information thin-layer identification method of water extract thereof |
| CN114113419A (en) * | 2020-08-26 | 2022-03-01 | 尚科生物医药（上海）有限公司 | Chromatographic separation method of saxagliptin and isomer thereof |
| CN112946113A (en) * | 2021-02-01 | 2021-06-11 | 湖北医药学院 | Method for identifying genuine medicinal material Shiweir fructus forsythiae basal source |
| CN115236239A (en) * | 2022-08-09 | 2022-10-25 | 多特瑞(上海)商贸有限公司 | Method for detecting content of alpha-copal in schisandra essential oil |
| CN115236239B (en) * | 2022-08-09 | 2023-12-29 | 多特瑞(上海)商贸有限公司 | Method for detecting content of alpha-copaene in schisandra essential oil |
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