CN106153803A - A kind of based on the method for active component dissolution in Rotating shaker detection GUIZHI FULING JIAONANG - Google Patents
A kind of based on the method for active component dissolution in Rotating shaker detection GUIZHI FULING JIAONANG Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
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Abstract
The invention belongs to pharmaceutical analysis field, particularly relate to a kind of based on the method for active component dissolution in Rotating shaker detection GUIZHI FULING JIAONANG.The method that the present invention provides comprises the following steps: a), adding 500～900mL hydrochloric acid solutions in the stripping rotor of medicament dissolution instrument, the concentration of described hydrochloric acid solution is 0.05～0.15mol/L；To turning of medicament dissolution instrument, basket adds a GUIZHI FULING JIAONANG；B) in stripping rotor, by said spin basket soak more than 30min, obtain dissolution fluid；Turning basket rotating speed during described immersion is 50～100r/min；C), use chromatography that the active component in described dissolution fluid is carried out content detection, obtain the dissolution of active component in GUIZHI FULING JIAONANG according to chromatograph testing result.The present invention, by the conditional parameter during optimization GUIZHI FULING JIAONANG dissolution detection, improves accuracy and the repeatability of testing result.
Description
Technical field
The invention belongs to pharmaceutical analysis field, particularly relate to a kind of based on activity one-tenth in Rotating shaker detection GUIZHI FULING JIAONANG
The method dividing dissolution.
Background technology
GUIZHI FULING JIAONANG is made up of Ramulus Cinnamomi, Poria, the Radix Paeoniae Alba, Semen Persicae and Cortex Moutan gomi herbs, have invigorate blood circulation, blood stasis dispelling,
The effect disappeared.Cure mainly block, amenorrhea, dysmenorrhea, prolonged lochia caused by married woman's obstruction of collaterals by blood stasis；Hysteromyoma, chronic pelvic
Scorching enclosed mass, endometriosis, ovarian cyst is shown in above-mentioned patient.
The absorption of medicine be oral drugs play a role key the first step, and the dissolution of medicine be absorb premise bar
Part, therefore carries out dissolution detection and is very important GUIZHI FULING JIAONANG.The drug dissolution inspection that " Chinese Pharmacopoeia " is recorded
Survey method includes Rotating shaker, slurry processes, small-radius curve track, slurry dish method and rotating-cylinder method.It is known that the selection of dissolution detection method and inspection
Dissolution testing result is had a direct impact by the selection of survey condition, inhales to preferably embody the dissolution of GUIZHI FULING JIAONANG
Receipts situation, it is the most necessary for studying high and favorable repeatability the GUIZHI FULING JIAONANG dissolution detection method of a kind of accuracy.
Summary of the invention
In view of this, it is an object of the invention to provide one based on active component in Rotating shaker detection GUIZHI FULING JIAONANG
The method of dissolution, the method that the present invention provides can detect the dissolution of various active composition in GUIZHI FULING JIAONANG the most simultaneously
Degree, testing result has higher accuracy and good repeatability.
The invention provides a kind of based on the method for active component dissolution in Rotating shaker detection GUIZHI FULING JIAONANG, including
Following steps:
A), adding 500～900mL hydrochloric acid solutions in the stripping rotor of medicament dissolution instrument, the concentration of described hydrochloric acid solution is
0.05～0.15mol/L；To turning of medicament dissolution instrument, basket adds a GUIZHI FULING JIAONANG；
B) in stripping rotor, by said spin basket soak more than 30min, obtain dissolution fluid；Basket is turned during described immersion
Rotating speed is 50～100r/min；
C), use chromatography that the active component in described dissolution fluid is carried out content detection, obtain according to chromatograph testing result
The dissolution of active component in GUIZHI FULING JIAONANG.
Preferably, in step a), in described stripping rotor, the addition of hydrochloric acid solution is 500mL；Described hydrochloric acid solution dense
Degree is 0.1mol/L.
Preferably, in step b), the temperature of described immersion is 37 ± 1 DEG C；Said spin basket soak in stripping rotor 30～
60min；The rotating speed of said spin basket is 50r/min.
Preferably, containing gallic acid, peoniflorin, benzoic acid, benzoylpaeoniflorin, Cortex Moutan in described GUIZHI FULING JIAONANG
Phenol, cinnamic acid, cinnamic aldehyde and amygdaloside.
Preferably, in step c), the device that described chromatography uses is ultrahigh-pressure liquid chromatograph.
Preferably, in step c), using chromatography to the gallic acid in described dissolution fluid, peoniflorin, benzoic acid, benzene
When one or more in formyl peoniflorin, paeonol, cinnamic acid and cinnamic aldehyde carry out content detection, the flowing of employing is second mutually
Nitrile and 0.02vol% trifluoroacetic acid aqueous solution；
In step c), when using chromatography that the amygdaloside in described dissolution fluid is carried out content detection, the stream of employing
Dynamic is first alcohol and water mutually.
Preferably, in step c), the type of elution that described chromatography uses is gradient elution.
Preferably, in step c), using chromatography to the gallic acid in described dissolution fluid, peoniflorin, benzoic acid, benzene
When one or more in formyl peoniflorin, paeonol, cinnamic acid and cinnamic aldehyde carry out content detection, washing of described gradient elution
De-program is set to:
When 0～2min, 0.02vol% trifluoroacetic acid aqueous solution is 95:5 with the volume ratio of acetonitrile；During 8min,
0.02vol% trifluoroacetic acid aqueous solution is 83:17 with the volume ratio of acetonitrile；During 12min, 0.02vol% trifluoroacetic acid aqueous solution
It is 81:19 with the volume ratio of acetonitrile；During 16min, 0.02vol% trifluoroacetic acid aqueous solution is 74:26 with the volume ratio of acetonitrile；24
～the volume ratio of 28min, 0.02vol% trifluoroacetic acid aqueous solution and acetonitrile is 12:88；
In step c), when using chromatography that the amygdaloside in described dissolution fluid is carried out content detection, described gradient
The elution program of eluting is set to:
When 0～7min, methanol is 20:80 with the volume ratio of water；During 13min, methanol is 80:20 with the volume ratio of water.
Preferably, in step c), using chromatography to the gallic acid in described dissolution fluid, peoniflorin, benzoic acid, benzene
When one or more in formyl peoniflorin and paeonol carry out content detection, the detection wavelength of employing is 230nm；
In step c), when using chromatography that the cinnamic acid in described dissolution fluid and/or cinnamic aldehyde are carried out content detection,
The detection wavelength used is 275nm；
In step c), when using chromatography that the amygdaloside in described dissolution fluid is carried out content detection, the inspection of employing
Survey wavelength is 218nm.
Preferably, in step c), before the active component in described dissolution fluid carries out content detection, also include:
Described dissolution fluid is filtered；The filter sizes of described filtration is 0.2～0.25 μm.
Compared with prior art, the invention provides one molten based on active component in Rotating shaker detection GUIZHI FULING JIAONANG
The method of out-degree.The present invention provide method comprise the following steps: a), in the stripping rotor of medicament dissolution instrument add 500～
900mL hydrochloric acid solution, the concentration of described hydrochloric acid solution is 0.05～0.15mol/L；To turning of medicament dissolution instrument, basket adds one
Grain GUIZHI FULING JIAONANG；B) in stripping rotor, by said spin basket soak more than 30min, obtain dissolution fluid；The process of described immersion
Transfer basket rotating speed is 50～100r/min；C), use chromatography that the active component in described dissolution fluid is carried out content detection, root
The dissolution of active component in GUIZHI FULING JIAONANG is obtained according to chromatograph testing result.The present invention is molten by optimizing GUIZHI FULING JIAONANG
Conditional parameter during out-degree detection, improves accuracy and the repeatability of testing result.Test result indicate that, use this
The method that invention provides is to GUIZHI FULING JIAONANG dissolution fluid duplicate detection 6 times, the dissolution of each active component in GUIZHI FULING JIAONANG
Relative standard deviation (RSD) ＜ 1.8% of degree testing result；In average recovery is tested, each activity in GUIZHI FULING JIAONANG
The average recovery rate of composition be 95～103%, relative standard deviation (RSD) ＜ 1.6%.
Detailed description of the invention
Below the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment
It is only a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention, the common skill in this area
The every other embodiment that art personnel are obtained under not making creative work premise, broadly falls into the model of present invention protection
Enclose.
The invention provides a kind of based on the method for active component dissolution in Rotating shaker detection GUIZHI FULING JIAONANG, including
Following steps:
A), adding 500～900mL hydrochloric acid solutions in the stripping rotor of medicament dissolution instrument, the concentration of described hydrochloric acid solution is
0.05～0.15mol/L；To turning of medicament dissolution instrument, basket adds a GUIZHI FULING JIAONANG；
B) in stripping rotor, by said spin basket soak more than 30min, obtain dissolution fluid；Basket is turned during described immersion
Rotating speed is 50～100r/min；
C), use chromatography that the active component in described dissolution fluid is carried out content detection, obtain according to chromatograph testing result
The dissolution of active component in GUIZHI FULING JIAONANG.
The dissolution detection method that the present invention provides is carried out based on Rotating shaker, and said spin basket method refers to " Chinese Pharmacopoeia " 2015
Dissolution disclosed in year the 4th general rule 0931 of version and the first method in drug release determination method.
In the present invention, in the stripping rotor of medicament dissolution instrument, hydrochloric acid solution is first added.The present invention medicine to being used
The specification of thing digestion instrument is not particularly limited, and uses the medicament dissolution instrument that Rotating shaker well known to those skilled in the art uses i.e.
Can, described medicament dissolution instrument includes stripping rotor and turns basket, and described stripping rotor is used for holding dissolution medium, and said spin basket is used for placing
Medicine to be measured.In the embodiment that the present invention provides, use RCZ-8M intelligence digestion instrument.In the present invention, described hydrochloric acid
The concentration of solution is 0.05～0.15mol/L, preferably 0.1mol/L.The hydrochloric acid solution that present invention preferably employs 0.1mol/L is
Owing to the pH value of the hydrochloric acid solution of 0.1mol/L is similar to human body gastric acid, molten human stomach of GUIZHI FULING JIAONANG more can be reacted
Artificial situation.In the present invention, in described stripping rotor, the addition of hydrochloric acid solution is 500～900mL, preferably 500mL.By hydrochloric acid
After solution joins stripping rotor, to turning of medicament dissolution instrument, basket adds a GUIZHI FULING JIAONANG.In the present invention, described
GUIZHI FULING JIAONANG is a kind of Chinese medicinal capsule preparation, in described GUIZHI FULING JIAONANG containing gallic acid, peoniflorin, benzoic acid,
Benzoylpaeoniflorin, paeonol, cinnamic acid, cinnamic aldehyde and amygdaloside.In the embodiment that the present invention provides, described osmanthus
In branch Indian buead capsule, the content of gallic acid is 2.64mg/ grain, and the content of peoniflorin is 8.22mg/ grain, and benzoic content is
0.35mg/ grain, the content of benzoylpaeoniflorin is 0.79mg/ grain, and the content of paeonol is 4.95mg/ grain, the content of cinnamic acid
For 0.26mg/ grain, the content of cinnamic aldehyde is 0.79mg/ grain, and the content of amygdaloside is 7.55mg/ grain.
Will in stripping rotor add hydrochloric acid solution, and by GUIZHI FULING JIAONANG add turn basket after, by said spin basket at stripping rotor
Middle immersion.Wherein, the temperature of described immersion is preferably 37 ± 1 DEG C, more preferably 37 ± 0.5 DEG C；Turn during described immersion
Basket rotating speed is 50～100r/min, preferably 50r/min；The time that said spin basket is soaked in stripping rotor is more than 30min, excellent
Elect 30～60min as.After immersion terminates, obtain dissolution fluid.
After obtaining dissolution fluid, chromatography is used the active component in described dissolution fluid to be carried out content detection, according to chromatograph
Testing result obtains the dissolution of active component in GUIZHI FULING JIAONANG, this process particularly as follows:
C1), described dissolution fluid is carried out chromatograph detection, obtain the peak area of each active component in dissolution fluid；
C2), according to the concentration-peak area standard of the peak area of active component in described dissolution fluid Yu predetermined active component
Curve, obtains the content of active component in dissolution fluid；
C3), active component in GUIZHI FULING JIAONANG is obtained according to the cubage of active component in the dissolution fluid obtained
Dissolution.
During the above-mentioned dissolution fluid chromatograph detection that the present invention provides, first described dissolution fluid is carried out chromatograph inspection
Survey.Wherein, the mode of described chromatograph detection is preferably the detection of ultrahigh pressure liquid phase chromatograph.The detection of described chromatograph is used by the present invention
Instrument does not has special restriction, uses chromatograph of liquid well known to those skilled in the art, as used Agilent
1290 ultrahigh-pressure liquid chromatograph.In the present invention, the chromatographic column of described chromatograph detection is preferably Agilent SB-RRHD C18
Post；The column temperature of described chromatographic column is preferably 30～35 DEG C；The type of elution of described chromatograph detection is preferably gradient elution；Described stream
Move and be preferably one or more in trifluoroacetic acid aqueous solution, acetonitrile, first alcohol and water mutually；The stream of the flowing phase of described chromatograph detection
Speed is preferably 0.1mL/min～0.5mL/min, more preferably 0.2mL/min；Described chromatograph detection wavelength be preferably 210～
280nm, more preferably 218～275nm.In the present invention, owing to GUIZHI FULING JIAONANG contains various active composition, therefore for obtaining
Obtain preferable chromatograph Detection results, use different chromatographic conditions for different activities composition.In the present invention, described activity becomes
Point refer to the medicinal active ingredient contained in GUIZHI FULING JIAONANG, as gallic acid, peoniflorin, benzoic acid, benzoylpaeoniflorin,
Paeonol, cinnamic acid, cinnamic aldehyde and amygdaloside.In the embodiment that the present invention provides, if the composition of chromatograph detection is
During one or more in gallic acid, peoniflorin, benzoic acid, benzoylpaeoniflorin and paeonol, chromatograph detection wavelength is
230nm；If the composition of chromatograph detection is cinnamic acid and/or cinnamic aldehyde, chromatograph detection wavelength is 275nm；If chromatograph detection
When composition is amygdaloside, chromatograph detection wavelength is 218nm.In the embodiment that the present invention provides, if chromatograph detection
Composition is one or more in gallic acid, peoniflorin, benzoic acid, benzoylpaeoniflorin, paeonol, cinnamic acid and cinnamic aldehyde
Time, flowing uses 0.02vol% trifluoroacetic acid aqueous solution and acetonitrile mutually；If the composition of chromatograph detection is amygdaloside, flowing
Use first alcohol and water mutually.The present invention provide an embodiment in, if chromatograph detection composition be gallic acid, peoniflorin,
During one or more in benzoic acid, benzoylpaeoniflorin, paeonol, cinnamic acid and cinnamic aldehyde, the flowing phase of its gradient elution
Arrange the most in such a way: when 0～2min, 0.02vol% trifluoroacetic acid aqueous solution and the volume ratio of acetonitrile
For 95:5；During 8min, 0.02vol% trifluoroacetic acid aqueous solution is 83:17 with the volume ratio of acetonitrile；During 12min, 0.02vol%
Trifluoroacetic acid aqueous solution is 81:19 with the volume ratio of acetonitrile；During 16min, 0.02vol% trifluoroacetic acid aqueous solution and the body of acetonitrile
Long-pending ratio is 74:26；24～28min, 0.02vol% trifluoroacetic acid aqueous solution is 12:88 with the volume ratio of acetonitrile.Carry in the present invention
In one embodiment of confession, if the composition of chromatograph detection is amygdaloside, the flowing of its gradient elution is the most over time
Arranging in such a way: when 0～7min, methanol is 20:80 with the volume ratio of water；During 13min, methanol with the volume ratio of water is
80:20.After chromatograph detection terminates, obtain the peak area of active component in dissolution fluid.In the present invention, if the activity in dissolution fluid
When composition is multiple, then every kind of active component all obtains corresponding active component peak area.
Obtaining in described dissolution fluid after the peak area of active component, the present invention is according to the peak of active component in described dissolution fluid
Area and the concentration-peak area standard curve of predetermined active component, obtain the content of active component in dissolution fluid.In the present invention
In, if the active component in dissolution fluid is multiple, then every kind of active component is required to set up the concentration-peak area of active component
Standard curve.Below as a example by gallic acid, the concentration of described predetermined gallic acid-peak area standard curve preferably according to
Lower method obtains:
First, it is provided that the standard solution of a series of gallic acids；Then, the standard solution to described a series of gallic acids
Carry out chromatograph detection, obtain the chromatogram of the standard solution of each concentration of gallic acid；Finally, right with it according to described chromatogram
The concentration of the standard solution answered, obtains the concentration-peak area standard curve of gallic acid.
In the method for the concentration-peak area standard curve of the above-mentioned acquisition gallic acid of present invention offer, first provide
The standard solution of a series of gallic acid concentration, described standard solution is obtained by standard substance preparation.The present invention is to described standard substance
Source there is no special restriction, use gallic acid standard substance well known to those skilled in the art, as bought not
The standard substance of gallate-based.The present invention does not has special restriction to the compound method of described standard solution, uses people in the art
The compound method of the standard solution known to Yuan.After obtaining the standard solution of a series of gallic acid concentration, the present invention is to institute
The standard solution stating a series of gallic acid concentration carries out chromatograph detection, obtains the color of the gallic acid standard solution of each concentration
Spectrogram.Present invention preferably employs above-mentioned dense to described a series of gallic acids to the technical scheme of gallic acid detection in dissolution fluid
The standard solution of degree carries out chromatograph detection, does not repeats them here.Obtain the chromatogram of the gallic acid standard solution of each concentration
After, the present invention is calculated the peak area of the gallic acid standard solution of each concentration, corresponding according to the peak area obtained
The concentration of gallic acid standard solution, obtain gallic acid concentration-peak area standard curve.
Obtain in dissolution fluid after the content of active component, obtain according to the cubage of active component in the dissolution fluid obtained
The dissolution of active component in GUIZHI FULING JIAONANG.
The present invention, by the conditional parameter during active component dissolution detects in optimization GUIZHI FULING JIAONANG, improves
The accuracy of testing result and repeatability.Test result indicate that, the method using the present invention to provide is molten to GUIZHI FULING JIAONANG
Go out liquid duplicate detection 6 times, relative standard deviation (RSD) ＜ of the dissolution testing result of each composition in GUIZHI FULING JIAONANG
1.8%；Average recovery test in, in GUIZHI FULING JIAONANG the average recovery rate of each composition be 95～103%, relative standard
Deviation (RSD) ＜ 1.6%.
For the sake of becoming apparent from, it is described in detail below by following example.
In the present invention, following embodiment is directed to use with following instrument and reagent:
1, instrument:
RCZ-8M intelligence digestion instrument (huge sky, Tianjin is sent out)；Agilent 1290 ultrahigh-pressure liquid chromatograph (U.S.)；Point
Analysis balance (startorius).
2, reagent:
GUIZHI FULING JIAONANG (lot number: 20130501,20130601,20141101；The Jiangsu Kang Yuan limited public affairs of Pharmaceutical share
Department)；Gallic acid (lot number: 110831-201204, purity: 89.9%；National Institute for Food and Drugs Control), peoniflorin (batch
Number: 110736-201337, purity: 94.9%；National Institute for Food and Drugs Control), benzoic acid (lot number: 100419-
201302, purity: 100%；National Institute for Food and Drugs Control), benzoylpaeoniflorin (lot number: MUST-14112704, pure
Degree: 99.28%；Man Site bio tech ltd, Chengdu), paeonol (lot number: 110708-201407, purity: 99.9%；
National Institute for Food and Drugs Control), cinnamic acid (lot number: 110786-200503, purity: 100%；Chinese food drug assay
Academy), cinnamic aldehyde (lot number: 110710-201418, purity: 99.4%；National Institute for Food and Drugs Control), Semen Armeniacae Amarum
Glycosides (lot number: 110820-201004, purity: 93.6%；National Institute for Food and Drugs Control)；Methanol (chromatographically pure, the U.S.
Tedia company), acetonitrile (chromatographically pure, Tedia company of the U.S.), trifluoroacetic acid (chromatographically pure, aladdin), hydrochloric acid, sodium acetate, ice
Acetic acid, potassium dihydrogen phosphate, sodium hydroxide are analytical pure, make purified water by oneself.
Embodiment 1
Criterion curve
1, chromatographic condition
1.1, gallic acid, peoniflorin, benzoic acid, benzoylpaeoniflorin, paeonol, cinnamic acid, cinnamic aldehyde
Flowing phase: 0.02% trifluoroacetic acid aqueous solution is mobile phase A, and acetonitrile is Mobile phase B；Flow velocity: 0.2ml/min；Inspection
Survey wavelength I: 230nm (gallic acid, peoniflorin, benzoic acid, benzoylpaeoniflorin, paeonol)；Detection wavelength II:275nm (meat
Cinnamic acid, cinnamic aldehyde)；Sample size: 2 μ l；Chromatographic column: Agilent SB-RRHD C18,2.1 × 100mm, 1.8 μm；Column temperature: 30
℃；Gradient elution program is shown in Table 1:
Table 1 gallic acid, peoniflorin, benzoic acid, benzoylpaeoniflorin, paeonol, cinnamic acid, the gradient elution of cinnamic aldehyde
Table
1.2, amygdaloside
Flowing phase: methanol is mobile phase A, and water is Mobile phase B；Flow velocity: 0.2ml/min；Detection wavelength 218nm；Sample size:
2μl；Agilent SB-RRHD C18,2.1 × 100mm, 1.8 μm；Column temperature: 30 DEG C；Gradient elution program is shown in Table 2:
The gradient elution table of table 2 amygdaloside
2, Criterion curve
Precision weighs gallic acid, peoniflorin, paeonol reference substance 5.426mg, 5.116mg, 5.418mg in 100ml appearance
In measuring bottle, add 50vol% methanol dissolved dilution to scale, more respectively precision measure 5ml, 4ml, 3ml, 2ml, 1ml, 0.4ml,
0.2ml, 0.1ml, 0.02ml in 9 10ml volumetric flasks 1. in；Another precision weighs benzoic acid, benzoylpaeoniflorin, cinnamic acid pair
According to product 5.262mg, 5.334mg, 5.005mg in 50ml volumetric flask, add 50vol% methanol dissolved dilution to scale more accurate
Measure 10ml mixing in comparison with another 100ml volumetric flask 2. in；Another precision weighs cinnamic aldehyde comparison 13.17mg in 25ml volumetric flask
In, dissolved dilution to scale, then precision measure 2ml in above-mentioned 100ml volumetric flask 2. in, add 50vol% methanol dissolved dilution extremely
Scale, then precision measures 5ml, 4ml, 3ml, 2ml, 1ml, 0.5ml, 0.25ml, 0.1ml, 0.05ml in above-mentioned 9 10ml respectively
Volumetric flask 1. in, with 50vol% methanol dilution to scale, shake up, standby.Another precision weighs amygdaloside reference substance 5.158mg
In 100ml volumetric flask, add 50vol% methanol dissolved dilution to scale, more respectively precision measure 5ml, 4ml, 3ml, 2ml,
1ml, 0.4ml, 0.2ml, 0.1ml, 0.02ml are in 9 10ml volumetric flasks, with 50vol% methanol dilution to scale, standby.Press
Above-mentioned chromatographic condition sample introduction, records peak area, and with concentration as abscissa, peak area is vertical coordinate, carries out linear regression, and result is such as
Shown in table 3:
38 kinds of component linear regression results of table
By table 3 it can be seen that gallic acid is 24.3899～0.0976ug/ml, peoniflorin 24.2754～
0.0971ug/ml, benzoic acid 5.262～0.0526ug/ml, benzoylpaeoniflorin 5.2956～0.053ug/ml, Cortex Moutan
Phenol is 27.0629～0.1083ug/ml, and cinnamic acid is 5.005～0.0501ug/ml, and cinnamic aldehyde is 5.2364～0.0524ug/
Ml, amygdaloside concentration and peak area in the range of 24.1395～0.0966ug/ml are good linear relationship.
Embodiment 2
GUIZHI FULING JIAONANG dissolution detects
Taking 6 GUIZHI FULING JIAONANG (20130501), by dissolution method, (" Chinese Pharmacopoeia " version the 4th in 2015 is led to
Then 0,931 first method), with 0.1mol/L hydrochloric acid 500ml as dissolution medium, design temperature 37 DEG C, rotating speed 50r/min, treats that temperature reaches
In each turn of basket, put into a seed lac capsule after to, sample after 45min, through 0.22 μm filtering with microporous membrane, use Agilent
1290 ultrahigh-pressure liquid chromatograph sample is carried out chromatograph detection (each active component be given in chromatographic condition and embodiment 1
Testing conditions is consistent), calculate the dissolution of each active component, the results are shown in Table 4:
Table 4 GUIZHI FULING JIAONANG (20130501) dissolution determination result
By table 4 it can be seen that in GUIZHI FULING JIAONANG the dissolution of gallic acid be 96.17～98.85%, treat for 6
Survey the relative standard deviation (RSD)=0.97% of the gallic acid dissolution of capsule；The dissolution of peoniflorin be 96.75～
99.46%, the relative standard deviation (RSD)=1.01% of the peoniflorin dissolution of 6 capsules to be measured；Benzene in GUIZHI FULING JIAONANG
The dissolution of formic acid is 89.41～91.78%, the relative standard deviation (RSD) of the benzoic acid dissolution of 6 capsules to be measured=
0.95%；In GUIZHI FULING JIAONANG, the dissolution of benzoylpaeoniflorin is 95.86～98.46%, the benzoyl of 6 capsules to be measured
The relative standard deviation (RSD)=1.12% of peoniflorin dissolution；The dissolution of Paeonol in Guizhi Fuling Capsule be 95.16～
97.48%, the relative standard deviation (RSD)=0.58% of the paeonol dissolution of 6 capsules to be measured；Meat in GUIZHI FULING JIAONANG
The dissolution of cinnamic acid is 95.16～97.48%, the relative standard deviation (RSD) of the cinnamic acid dissolution of 6 capsules to be measured=
0.86%；In GUIZHI FULING JIAONANG, the dissolution of cinnamic aldehyde is 83.83～85.83%, the cinnamic aldehyde dissolution of 6 capsules to be measured
Relative standard deviation (RSD)=1.01%；In GUIZHI FULING JIAONANG, the dissolution of amygdaloside is 97.99～99.78%, 6
The relative standard deviation (RSD)=0.69% of the amygdaloside dissolution of grain capsule to be measured.
Embodiment 3
GUIZHI FULING JIAONANG dissolution detects
Taking 6 GUIZHI FULING JIAONANG (20130601), by dissolution method, (" Chinese Pharmacopoeia " version the 4th in 2015 is led to
Then 0,931 first method), with 0.1mol/L hydrochloric acid 500ml as dissolution medium, design temperature 37 DEG C, rotating speed 50r/min, treats that temperature reaches
In each turn of basket, put into a seed lac capsule after to, sample after 45min, through 0.22 μm filtering with microporous membrane, use Agilent
1290 ultrahigh-pressure liquid chromatograph sample is carried out chromatograph detection (each active component be given in chromatographic condition and embodiment 1
Testing conditions is consistent), calculate the dissolution of each active component, the results are shown in Table 5:
Table 5 GUIZHI FULING JIAONANG (20130601) dissolution determination result
By table 5 it can be seen that in GUIZHI FULING JIAONANG the dissolution of gallic acid be 93.47～95.83%, treat for 6
Survey the relative standard deviation (RSD)=0.93% of the gallic acid dissolution of capsule；The dissolution of peoniflorin be 92.33～
94.81%, the relative standard deviation (RSD)=1.07% of the peoniflorin dissolution of 6 capsules to be measured；Benzene in GUIZHI FULING JIAONANG
The dissolution of formic acid is 83.94～86.69%, the relative standard deviation (RSD) of the benzoic acid dissolution of 6 capsules to be measured=
1.11%；In GUIZHI FULING JIAONANG, the dissolution of benzoylpaeoniflorin is 92.28～94.15%, the benzoyl of 6 capsules to be measured
The relative standard deviation (RSD)=0.80% of peoniflorin dissolution；The dissolution of Paeonol in Guizhi Fuling Capsule be 92.79～
94.53%, the relative standard deviation (RSD)=0.64% of the paeonol dissolution of 6 capsules to be measured；Meat in GUIZHI FULING JIAONANG
The dissolution of cinnamic acid is 89.79～91.37%, the relative standard deviation (RSD) of the cinnamic acid dissolution of 6 capsules to be measured=
0.68%；In GUIZHI FULING JIAONANG, the dissolution of cinnamic aldehyde is 79.64～81.11%, the cinnamic aldehyde dissolution of 6 capsules to be measured
Relative standard deviation (RSD)=0.73%；In GUIZHI FULING JIAONANG, the dissolution of amygdaloside is 93.49～94.81%, 6
The relative standard deviation (RSD)=0.56% of the amygdaloside dissolution of grain capsule to be measured.
Embodiment 4
GUIZHI FULING JIAONANG dissolution detects
Taking 6 GUIZHI FULING JIAONANG (20141101), by dissolution method, (" Chinese Pharmacopoeia " version the 4th in 2015 is led to
Then 0,931 first method), with 0.1mol/L hydrochloric acid 500ml as dissolution medium, design temperature 37 DEG C, rotating speed 50r/min, treats that temperature reaches
In each turn of basket, put into a seed lac capsule after to, sample after 45min, through 0.22 μm filtering with microporous membrane, use Agilent
1290 ultrahigh-pressure liquid chromatograph sample is carried out chromatograph detection (each active component be given in chromatographic condition and embodiment 1
Testing conditions is consistent), calculate the dissolution of each active component, the results are shown in Table 6:
Table 6 GUIZHI FULING JIAONANG (20141101) dissolution determination result
By table 6 it can be seen that in GUIZHI FULING JIAONANG the dissolution of gallic acid be 96.55～99.28%, treat for 6
Survey the relative standard deviation (RSD)=1.08% of the gallic acid dissolution of capsule；The dissolution of peoniflorin be 96.32～
98.88%, the relative standard deviation (RSD)=0.96% of the peoniflorin dissolution of 6 capsules to be measured；Benzene in GUIZHI FULING JIAONANG
The dissolution of formic acid is 89.44～91.23%, the relative standard deviation (RSD) of the benzoic acid dissolution of 6 capsules to be measured=
0.69%；In GUIZHI FULING JIAONANG, the dissolution of benzoylpaeoniflorin is 96.82～98.15%, the benzoyl of 6 capsules to be measured
The relative standard deviation (RSD) 0.57% of peoniflorin dissolution；The dissolution of Paeonol in Guizhi Fuling Capsule be 96.73～
98.98%, the relative standard deviation (RSD)=0.87% of the paeonol dissolution of 6 capsules to be measured；Meat in GUIZHI FULING JIAONANG
The dissolution of cinnamic acid is 95.52～96.32%, the relative standard deviation (RSD) of the cinnamic acid dissolution of 6 capsules to be measured=
0.36%；In GUIZHI FULING JIAONANG, the dissolution of cinnamic aldehyde is 83.94～85.28%, the cinnamic aldehyde dissolution of 6 capsules to be measured
Relative standard deviation (RSD)=0.74%；In GUIZHI FULING JIAONANG, the dissolution of amygdaloside is 96.45～98.34%, 6
The relative standard deviation (RSD)=0.67% of the amygdaloside dissolution of grain capsule to be measured.
Embodiment 5
The specificity experiment of detection method
1, adjuvant interference experiment
Taking beta cyclodextrin 60mg, add 0.1mol/L hydrochloric acid 500ml, ultrasonic, after fully dissolving, sampling, through 0.22 μm micropore
Membrane filtration, uses Agilent 1290 ultrahigh-pressure liquid chromatograph that sample carries out chromatograph detection (chromatographic condition and embodiment 1
In the testing conditions of each active component that is given consistent), result does not detects each work in GUIZHI FULING JIAONANG in chromatogram spectrogram
Property composition characteristic peak, illustrate adjuvant on the dissolution of effective ingredient each in GUIZHI FULING JIAONANG without impact.
2, capsule shells interference experiment
Take GUIZHI FULING JIAONANG 1, content is poured out, clean with cotton swab, add 0.1mol/L hydrochloric acid 500ml,
Ultrasonic, after fully dissolving, sampling, through 0.22 μm filtering with microporous membrane, use Agilent1290 ultrahigh-pressure liquid chromatograph to sample
Product carry out chromatograph detection (chromatographic condition is consistent with the testing conditions of each active component provided in embodiment 1), and result is in chromatograph
Spectrogram does not detects the characteristic peak of each active component in GUIZHI FULING JIAONANG, illustrates that capsule shells is respectively arranged with in GUIZHI FULING JIAONANG
The dissolution of effect composition is without impact.
3, solvent interference experiment
Take 0.1mol/L hydrochloric acid, through 0.22 μm filtering with microporous membrane, use Agilent 1290 ultrahigh-pressure liquid chromatograph
Sample carries out chromatograph detection (chromatographic condition is consistent with the testing conditions of each active component be given in embodiment 1), and result exists
Chromatogram spectrogram does not detects the characteristic peak of each active component in GUIZHI FULING JIAONANG, illustrates that solvent is to each in GUIZHI FULING JIAONANG
The dissolution of effective ingredient is without impact.
Embodiment 6
The Precision Experiment of detection method
1, preparation reference substance solution
Precision weighs gallic acid, peoniflorin, benzoic acid, benzoylpaeoniflorin, paeonol, cinnamic acid, cinnamic aldehyde respectively
In right amount, add 50vol% methanol and dissolve, dilution, prepare mixing reference substance solution, the concentration of the most each composition is respectively as follows: Galla Turcica (Galla Helepensis)
Acid 4.878 μ g/ml, peoniflorin 4.8551 μ g/ml, benzoic acid 1.0524 μ g/ml, benzoylpaeoniflorin 1.0591 μ g/ml, Cortex Moutan
Phenol 5.4126 μ g/ml, cinnamic acid 1.001 μ g/ml, cinnamic aldehyde 1.0473 μ g/ml；It is appropriate that another precision weighs amygdaloside, same to method
Preparing amygdaloside reference substance solution, concentration is 9.6558 μ g/ml.
2, detection process
Take above-mentioned reference substance solution, use Agilent 1290 ultrahigh-pressure liquid chromatograph that sample is carried out chromatograph detection
(chromatographic condition is consistent with the testing conditions of each active component be given in embodiment 1), continuous sample introduction 6 times, record peak area, knot
Fruit is shown in Table 7:
Table 7 Precision Experiment result
By table 7 it can be seen that gallic acid, peoniflorin, benzoic acid, benzoylpaeoniflorin, paeonol, cinnamic acid, osmanthus
Skin aldehyde, amygdaloside relative standard deviation (RSD) be respectively 0.30%, 0.73%, 0.44%, 1.62%, 1.61%,
0.67%, 1.54%, 1.15%, show that this method precision is good.
Embodiment 7
The stability experiment of detection method
1, reference substance solution Detection of Stability
Precision weighs reference substance in right amount respectively, makes mixing reference substance solution (gallic acid, peoniflorin, benzoic acid, benzene first
Acyl peoniflorin, paeonol, cinnamic acid, cinnamic aldehyde concentration be respectively 4.878 μ g/ml, 4.8551 μ g/ml, 1.0524 μ g/ml,
1.0591μg/ml、5.4126μg/ml、1.001μg/ml、1.0473μg/ml)；Separately weigh appropriate amygdaloside and make reference substance
Solution (4.8279 μ g/ml), uses Agilent 1290 ultrahigh-pressure liquid chromatograph that above-mentioned reference substance solution is carried out chromatograph inspection
Survey (chromatographic condition is consistent with the testing conditions of each active component be given in embodiment 1), in 0h, 2h, 4h, 6h, 8h, 12h,
24h sample introduction, records peak area, calculates RSD, the results are shown in Table 8:
Table 8 reference substance solution stability
By table 8 it can be seen that gallic acid, peoniflorin, benzoic acid, benzoylpaeoniflorin, paeonol, cinnamic acid, osmanthus
Skin aldehyde, the RSD of amygdaloside be respectively 0.72%, 1.84%, 1.38%, 1.48%, 1.07%, 0.76%, 1.06%,
1.67%, show that dissolution fluid is stable in 24h.
2, GUIZHI FULING JIAONANG Detection of Stability
Take GUIZHI FULING JIAONANG one, add 0.1mol/L hydrochloric acid 500ml, ultrasonic to being completely dissolved, centrifugal, through 0.22 μm
Filtering with microporous membrane, uses Agilent 1290 ultrahigh-pressure liquid chromatograph that sample carries out chromatograph detection (chromatographic condition and reality
The testing conditions executing each active component provided in example 1 is consistent), in 0h, 2h, 4h, 6h, 8h, 12h, 24h sample introduction, record face, peak
Long-pending, calculate RSD, the results are shown in Table 9:
Dissolution fluid stability result in table 9 0.1mol/L hydrochloric acid
By table 9 it can be seen that branch Indian buead capsule is stable in 24h in 0.1mol/L hydrochloric acid.
Embodiment 8
The repeated experiment of detection method
Take GUIZHI FULING JIAONANG (20130501), by dissolution method (the 4th general rule of " Chinese Pharmacopoeia " version in 2015
0931 first method), with 0.1mol/L hydrochloric acid 500ml as dissolution medium, design temperature 37 DEG C, rotating speed 50r/min, treats that temperature reaches
After in each turn of basket, put into a seed lac capsule, after 45min, in same stripping rotor, take out 6 parts of samples as test liquid, centrifugal,
Through 0.22 μm filtering with microporous membrane, use Agilent 1290 ultrahigh-pressure liquid chromatograph that sample carries out chromatograph detection (chromatograph
Condition is consistent with the testing conditions of each active component be given in embodiment 1), record peak area, calculate RSD, the results are shown in Table 10:
Table 10 repeated experiment result
By table 10 it can be seen that gallic acid, peoniflorin, benzoic acid, benzoylpaeoniflorin, paeonol, cinnamic acid, osmanthus
Skin aldehyde, the RSD of amygdaloside be respectively 0.86%, 0.46%, 1.79%, 1.47%, 0.58%, 1.80%, 0.92%,
0.99%, show the method repeatability preferably.
Embodiment 9
The average recovery experiment of detection method
Precision weighs GUIZHI FULING JIAONANG (20130501) the about 0.24g of known content, average 9 parts, 3 parts one group, puts tool
In plug volumetric flask, each group is sequentially added into a certain amount of gallic acid, peoniflorin, benzoic acid, benzoylpaeoniflorin, paeonol, meat
Cinnamic acid, cinnamic aldehyde and amygdaloside, add the 0.1mol/L hydrochloric acid solution of 500ml, ultrasonic to being completely dissolved, centrifugal, through 0.22 μ
M filtering with microporous membrane, uses Agilent 1290 ultrahigh-pressure liquid chromatograph that sample carries out chromatograph detection (chromatographic condition and reality
The testing conditions executing each active component provided in example 1 is consistent), the content of each active component before and after calculating mark-on, and calculate back
Yield, the results are shown in Table 11～table 18:
Table 11 gallic acid average recovery experimental result
Table 12 peoniflorin average recovery experimental result
Table 13 benzoic acid average recovery experimental result
Table 14 benzoylpaeoniflorin average recovery experimental result
Table 15 paeonol average recovery experimental result
Table 16 cinnamic acid average recovery experimental result
Table 17 cinnamic aldehyde average recovery experimental result
Table 18 amygdaloside average recovery experimental result
By table 11～18 it can be seen that gallic acid, peoniflorin, benzoic acid, benzoylpaeoniflorin, paeonol, Cortex Cinnamomi
Acid, cinnamic aldehyde, amygdaloside average recovery rate is respectively 102.34%, 97.28%, 99.27%, 97.90%, 97.80%,
95.83%, 96.98%, 100.35%, RSD be respectively 1.54%, 0.59%, 1.03%, 1.43%, 1.33%, 1.08%,
1.40%, 1.49%.Show that the method accuracy rate is good.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For Yuan, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1., based on a method for active component dissolution in Rotating shaker detection GUIZHI FULING JIAONANG, comprise the following steps:
A), adding 500～900mL hydrochloric acid solutions in the stripping rotor of medicament dissolution instrument, the concentration of described hydrochloric acid solution is 0.05
～0.15mol/L；To turning of medicament dissolution instrument, basket adds a GUIZHI FULING JIAONANG；
B) in stripping rotor, by said spin basket soak more than 30min, obtain dissolution fluid；Basket rotating speed is turned during described immersion
It is 50～100r/min；
C), use chromatography that the active component in described dissolution fluid is carried out content detection, obtain osmanthus according to chromatograph testing result
The dissolution of active component in branch Indian buead capsule.
Method the most according to claim 1, it is characterised in that in step a), the addition of hydrochloric acid solution in described stripping rotor
Amount is 500mL；The concentration of described hydrochloric acid solution is 0.1mol/L.
Method the most according to claim 1, it is characterised in that in step b), the temperature of described immersion is 37 ± 1 DEG C；Institute
State and turn basket in stripping rotor, soak 30～60min；The rotating speed of said spin basket is 50r/min.
Method the most according to claim 1, it is characterised in that containing gallic acid, Radix Paeoniae in described GUIZHI FULING JIAONANG
Glycosides, benzoic acid, benzoylpaeoniflorin, paeonol, cinnamic acid, cinnamic aldehyde and amygdaloside.
Method the most according to claim 4, it is characterised in that in step c), the device that described chromatography uses is superelevation
Pressure liquid chromatography instrument.
Method the most according to claim 5, it is characterised in that in step c), is using chromatography in described dissolution fluid
Gallic acid, peoniflorin, benzoic acid, benzoylpaeoniflorin, paeonol, cinnamic acid and cinnamic aldehyde in one or more carry out
During content detection, the flowing of employing is acetonitrile and 0.02vol% trifluoroacetic acid aqueous solution mutually；
In step c), when using chromatography that the amygdaloside in described dissolution fluid is carried out content detection, the flowing phase of employing
For first alcohol and water.
Method the most according to claim 6, it is characterised in that in step c), the type of elution that described chromatography uses is
Gradient elution.
Method the most according to claim 7, it is characterised in that in step c), is using chromatography in described dissolution fluid
Gallic acid, peoniflorin, benzoic acid, benzoylpaeoniflorin, paeonol, cinnamic acid and cinnamic aldehyde in one or more carry out
During content detection, the elution program of described gradient elution is set to:
When 0～2min, 0.02vol% trifluoroacetic acid aqueous solution is 95:5 with the volume ratio of acetonitrile；During 8min, 0.02vol% tri-
Fluoroethanoic acid aqueous solution is 83:17 with the volume ratio of acetonitrile；During 12min, 0.02vol% trifluoroacetic acid aqueous solution and the volume of acetonitrile
Ratio is 81:19；During 16min, 0.02vol% trifluoroacetic acid aqueous solution is 74:26 with the volume ratio of acetonitrile；24～28min,
0.02vol% trifluoroacetic acid aqueous solution is 12:88 with the volume ratio of acetonitrile；
In step c), when using chromatography that the amygdaloside in described dissolution fluid is carried out content detection, described gradient elution
Elution program be set to:
When 0～7min, methanol is 20:80 with the volume ratio of water；During 13min, methanol is 80:20 with the volume ratio of water.
Method the most according to claim 5, it is characterised in that in step c), is using chromatography in described dissolution fluid
Gallic acid, peoniflorin, benzoic acid, benzoylpaeoniflorin and paeonol in one or more when carrying out content detection, adopt
Detection wavelength be 230nm；
In step c), when using chromatography that the cinnamic acid in described dissolution fluid and/or cinnamic aldehyde are carried out content detection, use
Detection wavelength be 275nm；
In step c), when using chromatography that the amygdaloside in described dissolution fluid is carried out content detection, the detection ripple of employing
A length of 218nm.
Method the most according to claim 1, it is characterised in that in step c), the active component in described dissolution fluid is carried out
Before content detection, also include:
Described dissolution fluid is filtered；The filter sizes of described filtration is 0.2～0.25 μm.
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