CN106596783A - Method for determining content of garlicin content in garlicin tablets - Google Patents
Method for determining content of garlicin content in garlicin tablets Download PDFInfo
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- CN106596783A CN106596783A CN201611197737.2A CN201611197737A CN106596783A CN 106596783 A CN106596783 A CN 106596783A CN 201611197737 A CN201611197737 A CN 201611197737A CN 106596783 A CN106596783 A CN 106596783A
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- garlicin
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- liquid chromatography
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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
Abstract
The invention belongs to the technical field of quality control, and particularly relates to a method for determining the content of garlicin diallyl trisulfide in garlicin tablets. The method comprises the steps as follows: a to-be-detected sample of the garlicin tablets is mixed and dissolved with N, N-dimethylformamide, detection with high performance liquid chromatography and analysis with an external standard method are performed, and the content of diallyl trisulfide is obtained. With the adoption of the detection method, diallyl trisulfide can be fully separated from the garlicin tablets, and accordingly, the content of diallyl trisulfide in the garlicin tablets can be accurately detected. The detection method has the advantages of good linearity, repeatability and stability, high precision, low detection limit and quantification limit and high recovery rate, and blanks basically have no interference to determined results.
Description
Technical field
The invention belongs to Quality Control Technology field, and in particular to the side of Allicin Content in a kind of measure Bulbus Allii plain piece
Method, especially a kind of method for determining garlicin Diallytrisin content in Bulbus Allii plain piece.
Background technology
Garlicin (garlicin), is the thio ether compound of diallyl also known as allicin, and main component is diene
Propyl trisulfide ether and diallyl disulphide.Garlicin is naturally occurring in the bulb of liliaceous plant Bulbus Allii, blue to various leather
Family name's positive bacteria and gram negative bacteria have antibacterial action, to bacillus (dysentery bacterium, Bacillus typhi, escherichia coli, pertussis bar
Bacterium), funguses (Candida albicans, cryptococcus, Aspergillus fumigatus), viral (cytomegaloviruses), ameba, trichomonas vaginitises, pinworm
Worm etc. has suppression killing action, especially strong to the effect of the intestinal bacteria such as escherichia coli, dysentery bacterium.Clinical research discovery, greatly
Allicin has obvious preventive and therapeutic effect to the concurrent cytomegalovirus infection of bone marrow transplantation person.Garlicin also reduces cholesterolemia, glycerol
Three esters and lipoprotein and anti-platelet aggregation, antitumor action.Experiment also shows that garlicin can prevent and treat hepatic fibrosis, is antioxygen
Agent.In recent years, more and more extensive, deep to the pharmacological research of garlicin both at home and abroad, the various preparations of garlicin are facing in succession
Bed application.Such as allicin oil, garlicin powder, Bulbus Allii plain piece, capsulae allitridi.
At present garlicin common detection methods have NY/T 1497-2007, NY/T 1800-2009 and NY/T 2643-
2014.These detection methods are required for first carrying out pre-treatment to sample before detection, therefrom extract garlicin, then carry out again
The detection of content.Conventional pre-treating method includes using the means such as acetone solution, ethanol extraction, n-hexane extraction, water dissolution.
But these processing methods are not suitable for for embedding type Bulbus Allii plain piece, can not well dissolve and extract garlicin.Due to
Some adjuvants are with the addition of in Bulbus Allii plain piece, the such as conventional adjuvant of schardinger dextrin, Microcrystalline Cellulose, carboxymethylstach sodium tablet can affect greatly
The dissolution of allicin, causes the Allicin Content being dissolved out very low, affects the accuracy of follow-up content detection, it is impossible to obtain sample
In accurate Allicin Content result.
The content of the invention
In view of this, present invention aims to defect in prior art, there is provided one kind determines big in Bulbus Allii plain piece
The method of allicin Diallytrisin content.
In order to realize foregoing invention purpose, the present invention provides technical scheme below：
The invention provides a kind of method for determining Diallytrisin content in Bulbus Allii plain piece, to be measured by Bulbus Allii plain piece
Sample and DMF mixed dissolution, high performance liquid chromatography detection, external standard method analysis obtains the diallyl
The content of trithioether.
Wherein, preferably, described be dissolved as supersound process.
Preferably, the temperature of the supersound process is 4-30 DEG C, the time is 10-30min.
In a certain specific embodiment, the temperature of the supersound process is 30 DEG C, and the time is 15min.In a certain concrete reality
In applying example, the temperature of the supersound process is 4 DEG C, and the time is 30min.In a certain specific embodiment, the supersound process
Temperature is 15 DEG C, and the time is 15min.Preferably, also including machine filter membrane filtration before the high performance liquid chromatography detection
Step.
In the embodiment that the present invention is provided, the aperture of organic filter membrane is 0.45 μm.
Preferably, the mobile phase of the high performance liquid chromatography is acetonitrile solution.
Preferably, acetonitrile and the volume ratio of water are (20-80) in the acetonitrile solution:(80-20).
In a certain specific embodiment, the acetonitrile is 70 with the volume ratio of water:30.In a certain specific embodiment, institute
It is 20 that acetonitrile is stated with the volume ratio of water:80.In another specific embodiment, the acetonitrile is 80 with the volume ratio of water:20.
Preferably, the flow velocity of the mobile phase of the high performance liquid chromatography is 0.5～1.0mL/min.
In a certain specific embodiment, the flow velocity of the mobile phase is 1.0mL/min.
Preferably, the Detection wavelength of the high performance liquid chromatography is 240-254nm.
In a certain specific embodiment, the Detection wavelength of the high performance liquid chromatography is 240nm.
Preferably, the column temperature of the high performance liquid chromatography is 30～40 DEG C.
In a certain specific embodiment, the column temperature of the high performance liquid chromatography is 30 DEG C.
Preferably, the chromatographic column of the high performance liquid chromatography is Diamonsil Plus C18.
In the embodiment that the present invention is provided, model C18 of chromatographic column, column length 250mm, internal diameter 4.6mm, the μ of particle diameter 5.0
m。
The invention provides a kind of determine Diallytrisin content method in Bulbus Allii plain piece.The method is by Bulbus Allii plain piece
Testing sample tries mixed dissolution with DMF, and high performance liquid chromatography detection, external standard method analysis obtains described two
The content of diallyl trisulfide ether.
The present invention at least has one of following advantage：
1st, the detection method that the present invention is provided can be sufficiently separated Diallytrisin from Bulbus Allii plain piece such that it is able to
Accurately detect the content of Diallytrisin in Bulbus Allii plain piece；
2nd, detection method is linear, repeatability, have good stability, and precision is high, it is blank to measurement result substantially without
Interference, detection limit, quantitative limit are low, and the response rate is high, meets GB/T27404-2008《Good Laboratory controls specification》Requirement,
Measure Diallytrisin detection method of content scientific and effective of the present invention is proved, can be to the diallyl three of Bulbus Allii plain piece
Thioether content plays the purpose of quality control.
Description of the drawings
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
The accompanying drawing to be used needed for having technology description is briefly described.
Fig. 1 shows the chromatogram of blank solution in method blank assay；
Fig. 2 shows the chromatogram of reference substance solution in method blank assay；
Fig. 3-7 is respectively the chromatogram of the reference substance of standard serial number 1-5, shows the linear relationship of detection method；
The standard work that the concentration of Diallytrisin is drawn in the reference substance that Fig. 8 shows according to standard serial number 1-5 is bent
Line；
Fig. 9 shows the detection limit chromatogram of detection method；
Figure 10-15 is the chromatogram of 6 parts of samples of replication, shows the precision of detection method；
Figure 16-21 places at room temperature the chromatogram obtained after 0h, 1h, 2h, 4h, 7h, 9h for reference substance solution, shows this
The stability of bright detection method；
Figure 22-30 is the chromatogram of the sample of serial number 1～9 in recovery test, shows the response rate of detection method.
Specific embodiment
The invention discloses a kind of method for determining Allicin Content in Bulbus Allii piece.Those skilled in the art can use for reference this
Literary content, is suitably modified technological parameter realization.Specifically, all similar replacements and change are to art technology
It is it will be apparent that they are considered as being included in the present invention for personnel.The method of the present invention has passed through preferred embodiment
It is described, related personnel substantially can be carried out in without departing from present invention, spirit and scope to method described herein
Change or suitably change with combining to realize and apply the technology of the present invention.
For a further understanding of the present invention, with reference to specific embodiment, the present invention will be described in detail, such as without special
Illustrate, involved reagent is commercially available prod in the embodiment of the present invention, can be obtained by commercial channel purchase.Wherein,
Detecting instrument includes the high performance liquid chromatograph of Agilent 1260 (attached UV-detector), Ultrasound Instrument, electronic balance etc..The detection
Reagent includes N,N-dimethylformamide (analysis is pure), acetonitrile (chromatographically pure), one-level water.Diallytrisin reference substance comes
Come from Nat'l Pharmaceutical ＆ Biological Products Control Institute's (lot number:100384-201403, purity 94.2%).The Bulbus Allii plain piece to be measured is equal
For same batch, provided by Tang Chenbeijian companies.
Embodiment 1
1st, chromatographic condition
Chromatographic column：Diamonsil Plus C18 (column length 250mm, internal diameter 4.6mm, 5.0 μm of particle diameter)；
Column temperature：30℃；
Flow velocity：1.0ml/min；
Wavelength：240nm；
Mobile phase：Acetonitrile：Water=70:30
2nd, prepared by reference substance solution：Precision weighs garlicin (Diallytrisin) reference substance 8mg, is placed in 25ml browns
In volumetric flask, add appropriate DMF to dissolve in 30 DEG C of ultrasound 15min, add N, N- dimethyl formyls to be settled to
Volumetric flask scale, shakes up, and obtains final product.
3rd, prepared by sample test liquid：Bulbus Allii plain piece to be measured 20 (about 10g) is taken, finely ground into powder, precision weighs 50mg extremely
In 25ml volumetric flasks, appropriate DMF is added to dissolve in 30 DEG C of ultrasound 15min, DMF is fixed
Hold to volumetric flask scale, shake up, cross 0.45 μm of organic filter membrane, obtain final product.
4th, determine
It is accurate respectively to draw the control μ l of test liquid 1,2 μ l, 3 μ l, 4 μ l, the 5 μ l and μ l of sample test liquid 20, inject efficient liquid
Chromatography, sets up calibration curve equation.Sample test liquid chromatographic peak should be presented and compare test liquid chromatographic peak retention time phase
Same chromatographic peak.
5th, result is calculated
X=C × V/M × K
In formula：The content of X-sample garlicin (Diallytrisin), g/100g；
The quality of M-sample, g；
K-unit conversion factor (K=0.1)；
The extension rate of V-sample, ml；
The concentration of garlicin (Diallytrisin), mg/ml in C-sample solution.
6th, Method validation
(1) method blank experiment
Sample is weighed, the method prepared by above-mentioned sample test liquid processes blank solution, determine empty by above-mentioned chromatographic condition
White solution, contrasts with the appearance time of Diallytrisin reference substance solution.As a result Fig. 1 and Fig. 2 is seen.Fig. 1 and Fig. 2 results show
Show, blank solution, without absworption peak, shows blank noiseless to measurement result at the appearance time of Diallytrisin.
(2) range of linearity confirms
Test data is shown in Table 1, and chromatogram is shown in Fig. 3-7.
The range of linearity validation test result of table 1
With concentration as abscissa, peak area is vertical coordinate, draws standard working curve as shown in Figure 8.
Linear test conclusion：The dependency of the Diallytrisin of garlicin is 1.000, so determining big with the method
The Diallytrisin of allicin is presented good linear between concentration 0.01458mg/ml to 0.07290mg/ml, meets
GB/T27404-2008《Good Laboratory controls specification》Requirement (GB/T27404-2008 require dependency >=0.99).
(3) detection limit and quantitative limit
The qualitative detection limit DL and quantitative detection limit QL of analysis method is calculated by signal to noise ratio (S/N).DL be S/N=3 when pair
The concentration to be analyzed answered, corresponding concentration to be analyzed when QL is S/N=10.
Detection limit chromatogram is shown in 9.
Qualitative detection limit：When signal to noise ratio (S/N) is 3, the qualitative detection of the Diallytrisin of garlicin is limited to
0.17 μ g/ml, the qualitative detection of method for obtaining the Diallytrisin of garlicin is limited to 42.5 μ g/g.
Quantitative detection limit：When signal to noise ratio (S/N) is 10, the Diallytrisin of garlicin is quantitatively limited to 0.51 μ
G/ml, the method for obtaining the Diallytrisin of garlicin is quantitatively limited to 140.2 μ g/g.
(4) precision test
Test method：6 parts of samples are weighed, the method process sample prepared by above-mentioned sample test liquid, detection sample content,
Calculate its RSD (%).
Test data is shown in Table 2, and chromatogram is shown in Figure 10-15.
The Precision test result of table 2
Conclusion (of pressure testing)：The RSD (%) of 6 parts of sample garlicin (Diallytrisin) contents is 1.2%, shows the method
There is preferable precision, meet GB/T27404-2008《Good Laboratory controls specification》Requirement (GB/T27404-2008 will
Seek RSD (%)≤2.7%).
(5) stability test
Test method：Garlicin (Diallytrisin) reference substance working solution is placed at room temperature respectively 0h, 1h,
After 2h, 4h, 7h, 9h, peak area is determined by above-mentioned chromatographic condition, calculate its RSD (%).
Test data is shown in Table 3, and chromatogram is shown in Figure 16-21.
The stability test result of table 3
Conclusion (of pressure testing)：Garlicin (Diallytrisin) reference substance working solution place at room temperature respectively 0h, 1h,
After 2h, 4h, 7h, 9h, RSD (%) is 0.3%, shows garlicin (Diallytrisin) stablizing in 9 hours at room temperature
Property is good.
(6) recovery test
Test method：
Mark-on：Precision weighs 9 parts of about 50mg samples, and (the Diallytrisin content of known garlicin is：0.976g/
100g), it is divided into 3 groups, 3 parts per group, in being placed in 25ml volumetric flasks, each group is accurate respectively to add garlicin (Diallytrisin)
Reference substance solution (0.2916mg/ml) 1.6ml, 2.0ml, 2.4ml, then add DMF appropriate, 30 DEG C of ultrasounds
15min, with DMF volumetric flask scale is settled to, and is shaken up, and crosses the organic filter membranes of 0.45um, obtains final product mark-on for examination
Liquid.
Test data such as table 4, chromatogram is shown in accompanying drawing 22-30.
The recovery test result table of table 4
Measure addition=mark-on sample measured amount-sample measured amount
The response rate (%)=measure addition/theoretical addition amount
Conclusion (of pressure testing)：Garlicin (Diallytrisin) average recovery rate is：97.34%, relative standard deviation (RSD)
For 0.6%, meet GB/T27404-2008《Good Laboratory controls specification》Requirement (GB/T27404-2008 require the response rate
For 95%-105%).
Conclusion：
Linear, repeated, stability, sky are carried out by the method for the Diallytrisin content to determining garlicin
In vain, detection limit, quantitative limit, recovery test, meet GB/T27404-2008《Good Laboratory controls specification》Requirement, card
The bright methodological science for determining content effectively, can play quality control to the content of the Diallytrisin of garlicin in Bulbus Allii plain piece
The purpose of system.
Embodiment 2
The method and conventional common detection methods (NY/T 1497-2007, NY/T 1800- of embodiment 1 is respectively adopted
2009 and NY/T 2643-2014) detect content (the known garlicin of Diallytrisin in same batch Bulbus Allii plain piece
Diallytrisin content is 1.0%), to the results are shown in Table 5 in piece.
The content of Diallytrisin in the distinct methods of table 5 detection allicin tablet
| Detection method | The content (%) of garlicin in garlicin |
| NY/T 1497-2007 | Do not detect |
| NY/T 1800-2009 | 0.68% |
| NY/T 2643-2014 | 0.05% |
| Embodiment 1 | 0.96% |
Embodiment 3
1st, chromatographic condition
Chromatographic column：Diamonsil Plus C18 (column length 250mm, internal diameter 4.6mm, 5.0 μm of particle diameter)；
Column temperature：40℃；
Flow velocity：0.5ml/min；
Wavelength：240nm；
Mobile phase：Acetonitrile：Water=80:20
2nd, the preparation of reference substance solution：Precision weighs garlicin (Diallytrisin) reference substance 5mg, is placed in 10ml brown
In color tolerance measuring bottle, add appropriate DMF to dissolve in 4 DEG C of ultrasound 30min, add N, N- dimethyl formyl constant volumes
To volumetric flask scale, shake up, obtain final product.
3rd, the preparation of sample test liquid：Bulbus Allii plain piece to be measured 20 (about 10g) is taken, finely ground into powder, precision weighs 30mg
Into 10ml volumetric flasks, appropriate DMF is added to dissolve in 4 DEG C of ultrasound 30min, DMF
Volumetric flask scale is settled to, is shaken up, cross 0.45 μm of organic filter membrane, obtained final product.
4th, determine
It is accurate respectively to draw the control μ l of test liquid 1,2 μ l, 3 μ l, 4 μ l, the 5 μ l and μ l of sample test liquid 20, inject efficient liquid
Chromatography, injects high performance liquid chromatograph, under above-mentioned chromatographic condition, sets up calibration curve equation, is analyzed measure.
5th, result is calculated：
X=C × V/M × K
In formula：The content of X-sample garlicin (Diallytrisin), g/100g；
The quality of M-sample, g；
K-unit conversion factor (K=0.1)；
The extension rate of V-sample, ml；
The concentration of garlicin (Diallytrisin), mg/ml in C-sample solution.
6th, content detection result：
The Diallytrisin content detection result of the garlicin of table 6
Embodiment 4
1st, chromatographic condition
Chromatographic column：Diamonsil Plus C18 (column length 250mm, internal diameter 4.6mm, 5.0 μm of particle diameter)；
Column temperature：30℃；
Flow velocity：0.8ml/min；
Wavelength：240nm；
Mobile phase：Acetonitrile：Water=20:80
2nd, the preparation of reference substance solution：Precision weighs garlicin (Diallytrisin) reference substance 10mg, is placed in 50ml
In brown volumetric flask, add appropriate DMF to dissolve in 15 DEG C of ultrasound 15min, add N, N- dimethyl formyl to determine
Hold to volumetric flask scale, shake up, obtain final product.
3rd, the preparation of sample test liquid：Bulbus Allii plain piece to be measured 20 (about 10g) is taken, finely ground into powder, precision weighs 100mg
Into 50ml volumetric flasks, appropriate DMF is added to dissolve in 15 DEG C of ultrasound 15min, DMF
Volumetric flask scale is settled to, is shaken up, cross 0.45 μm of organic filter membrane, obtained final product.
4th, determine
It is accurate respectively to draw the control μ l of test liquid 1,2 μ l, 3 μ l, 4 μ l, the 5 μ l and μ l of sample test liquid 20, inject efficient liquid
Chromatography, injects high performance liquid chromatograph, under above-mentioned chromatographic condition, sets up calibration curve equation, is analyzed measure.
5th, result is calculated
X=C × V/M × K
In formula：The content of X-sample garlicin (Diallytrisin), g/100g；
The quality of M-sample, g；
K-unit conversion factor (K=0.1)；
The extension rate of V-sample, ml；
The concentration of garlicin (Diallytrisin), mg/ml in C-sample solution.
6th, content detection result：
The Diallytrisin content detection result of the garlicin of table 7
Claims (10)
1. it is a kind of determine Bulbus Allii plain piece in Diallytrisin content method, it is characterised in that by Bulbus Allii plain piece sample to be measured
Product and DMF mixed dissolution, high performance liquid chromatography detection, external standard method analysis obtains the diallyl three
The content of thioether.
2. method according to claim 1, it is characterised in that described to be dissolved as supersound process.
3. method according to claim 2, it is characterised in that the temperature of the supersound process is 4-30 DEG C, and the time is 10-
30min。
4. method according to claim 1, it is characterised in that also include machine filter before the high performance liquid chromatography detection
The step of membrane filtration.
5. detection method according to claim 1, it is characterised in that the mobile phase of the high performance liquid chromatography is acetonitrile
Aqueous solution.
6. detection method according to claim 5, it is characterised in that the volume ratio of acetonitrile and water in the acetonitrile solution
For (20-80):(80-20).
7. detection method according to claim 1, it is characterised in that the flow velocity of the mobile phase of the high performance liquid chromatography
For 0.5～1.0mL/min.
8. detection method according to claim 1, it is characterised in that the Detection wavelength of the high performance liquid chromatography is
240-254nm。
9. detection method according to claim 1, it is characterised in that the chromatographic column of the high performance liquid chromatography is
Diamonsil Plus C18。
10. detection method according to claim 1, it is characterised in that the column temperature of the high performance liquid chromatography is 30～
40℃。
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| CN201611197737.2A CN106596783A (en) | 2016-12-19 | 2016-12-19 | Method for determining content of garlicin content in garlicin tablets |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113029983A (en) * | 2021-03-10 | 2021-06-25 | 沈阳建筑大学 | Method for determining content of allicin in garlic wastewater |
| CN115267001A (en) * | 2022-08-05 | 2022-11-01 | 赣南师范大学 | Detection method of allicin in rhizosphere soil of tillered onion |
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| CN105319314A (en) * | 2015-12-09 | 2016-02-10 | 河南省奥林特药业有限公司 | Method for testing content of garlic oil in composite garlic oil capsule |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113029983A (en) * | 2021-03-10 | 2021-06-25 | 沈阳建筑大学 | Method for determining content of allicin in garlic wastewater |
| CN115267001A (en) * | 2022-08-05 | 2022-11-01 | 赣南师范大学 | Detection method of allicin in rhizosphere soil of tillered onion |
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Application publication date: 20170426 |