CN106990198A - It is a kind of at the same determine a variety of methods about material of andrographolide - Google Patents
It is a kind of at the same determine a variety of methods about material of andrographolide Download PDFInfo
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- CN106990198A CN106990198A CN201710286299.5A CN201710286299A CN106990198A CN 106990198 A CN106990198 A CN 106990198A CN 201710286299 A CN201710286299 A CN 201710286299A CN 106990198 A CN106990198 A CN 106990198A
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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
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- G01N30/74—Optical detectors
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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
- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
- G01N30/8631—Peaks
- G01N30/8634—Peak quality criteria
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Abstract
It is especially a kind of while determining a variety of methods about material of andrographolide the present invention relates to technical field of analytical chemistry.Determined using HPLC, using octadecyl silane as the chromatographic column of filler, packing material size is 2~5 μm, average diameter of particles is 4.6mm, Detection wavelength is 220~230nm, and column temperature is that 30~35 DEG C of flow velocitys are 0.5~2.0mL/min, and sample size is 10~15 μ L.With water (A) acetonitrile (B) for mobile phase, gradient elution is carried out.The present invention is easy to operate, can quickly, efficiently and accurately determine a variety of contents about material of andrographolide.
Description
Technical field
The present invention relates to technical field of analytical chemistry, it is more particularly related to which a kind of determine in Herba Andrographitis simultaneously
A variety of methods about material in ester.
Background technology
Andrographolide (Andrographolide) system extracts two obtained from Acanthaceae punching nelumbium Herba Andrographitis
Terpene lactones compound, with functions such as clearing heat and detoxicating, cool blood detumescences.Preparation listed or in the development phase is main
There are andrographolide tablet, capsule, injection etc..Herba Andrographitis Inner esters are using Folium Andrographis as raw material, using different extraction works
The preparation raw material medicine that skill is prepared.Due to its esters structure, in aqueous, particularly in high temperature, strong basicity environment, the Yishui River
Solution, open loop, isomerization and resinification.In andrographolide bulk drug and its preparation in addition to main component andrographolide, typically
There is the diterpene lactone impurity such as neoandrographolide, deoxyandrographolide and Dehydro and drographolide simultaneously.These chemical combination
Thing is introduced in extraction process a bit, is also had by degraded or Internal reforming is formed.These impurity may influence punching
The drug effect of lotus lactone, may seriously cause adverse reaction, and this is all pole for the security, validity, quality controllability of medicine
To be unfavorable.Therefore, in Accurate Determining andrographolide raw material and its preparation about material content, be to evaluate andrographolide
The important indicator of bulk drug and its quality of the pharmaceutical preparations.
At present, it is less about the research of substance detecting method for andrographolide.Document " Herba Andrographitis medicinal material and its preparation
In 6 lactone constituents content analysis (Pharmaceutical Analysis magazine, Deng Guihua, Lin Chaozhan, Zhu Chen Gall, 2011 (2):231-
235.) a kind of method for detecting Herba Andrographitis Multiple components " is provided, but the method gradient program is more, and Testing index is only
It is limited to the detection of Inner ester impurities, and detection time is longer；Patent " a kind of assay method of andrographolide about material "
(CN102809625B) water-acetonitrile-methanol ternary system, is employed, system is complex, cumbersome, and it is detected
Simply new Herba Andrographitis Inner esters, deoxidation Herba Andrographitis Inner esters and the dehydration Inner esters molecular structures such as Herba Andrographitis Inner esters, but for other
Content is relatively low but may influence the other impurities of Product quality and safety, and evidence suggests can also detect simultaneously." one surveys document
The content for commenting method to determine 5 lactone constituents in Herba Andrographitis (more《Chinese medicine》, Wang Huan, Lin Chaozhan, Wu Runjing, Zhu Chen Gall, the 37th
Roll up in March, 2014 the 3rd phase, 448-451) " provide one and survey and comment method while determining in Herba Andrographitis medicinal material 5 Inner lactone components more
The method of content, but examined through inventor, the method is when detecting Herba Andrographitis Inner esters alkali destruction sample, it is impossible to by each relevant material
It is effectively separated and then carries out content detection.As mentioned previously, except the impurity containing each Inner esters in Herba Andrographitis Inner esters
Outside, there is other such as open loop, isomerization, the impurity of resinification, therefore, current technology still lacks a kind of easy, sensitive, efficient
Andrographolide about the assay method of material, quick and precisely and comprehensively can determine and evaluate andrographolide raw material, with
And related preparations prepare and stability test during relevant content of material.
The content of the invention
It is an object of the invention to provide a kind of more easy, the sensitive efficient a variety of relevant materials of measure andrographolide
Method, with can quickly and accurately, it is comprehensive while determine relevant content of material in andrographolide bulk drug and its preparation.
To realize the object of the invention, technical scheme is as follows：
A kind of a variety of methods about material of use hplc simultaneous determination Herba Andrographitis Inner esters, what the method was used
Chromatographic condition is：Stationary phase is the chromatographic column using octadecyl silane as filler；Mobile phase A is water, and Mobile phase B is second
Nitrile；Gradient elution is carried out, gradient condition is：The volume ratio of the mobile phase of gradient 1 is：A：B=75~80%：25~20%, sample introduction
It is gradient 2 that phase change is flowed after 15~20min, and the volume ratio of the mobile phase of gradient 2 is：A：B=65~70%：35~30%, always
Run time is 45~55min；220~230nm of Detection wavelength, column temperature is 30~35 DEG C；Elution flow rate is 0.5~2.0mL/
min。
In some embodiments, the preferred volume ratio of the mobile phase of gradient 1 is：A：B=77：23.
In some embodiments, the preferred volume ratio of the mobile phase of gradient 2 is：A：B=70：30.
In some embodiments, the preferred 224nm of Detection wavelength.
In some embodiments, the preferred 1.0mL/min of elution flow rate.
In some embodiments, in sample introduction sample detection process, sample injection volume is 10~15 μ L.
In some embodiments, after the 45~55min of total run time, then under the conditions of gradient 1 operation 10~
15min。
In some embodiments, the chromatographic column filler particle diameter is 2~5 μm；Average diameter of particles is 4.6mm.
In some embodiments, the packing material size of the chromatographic column is 3 μm.
In some embodiments, in the process for preparation of andrographolide reference substance and testing sample, from good solvent
Andrographolide is dissolved, the good solvent be to andrographolide raw material, preparation and reference substance dissolubility preferably and
The solvent compatible with system, is methanol or acetonitrile, or the two mixture, preferably methanol.
The assay method that the present invention is mentioned, its elution flow rate is set as general knowledge known to those skilled in the art, common model
Enclose generally 0.5mL/min to 2mL/min, the present invention preferably 0.9~1.1mL/min, more preferably 1.0mL/min.
The method of the present invention has the advantages that compared with prior art：
(1) water-acetonitrile binary system is used, two sections of elutions are easier, more efficient.
(2) present invention carries out the sieve of chromatographic condition using the larger alkali destruction andrographolide of destructiveness as test sample
Choosing, in addition to andrographolide, 9 kinds of relevant materials can be detected simultaneously, and each separating degree about between material can be more than
1.5, therefore the scope of application of the present invention is wider.
Brief description of the drawings
Fig. 1 is the HPLC chromatogram after andrographolide reference substance destroys (destructiveness 6%) through highly basic；
Fig. 2 is the HPLC chromatogram after andrographolide reference substance destroys (destructiveness 47%) through highly basic；
Fig. 3 is the HPLC chromatogram after andrographolide reference substance is destroyed through strong acid；
Fig. 4 is relevant material detection HPLC colors under the chromatographic condition of embodiment 4 after andrographolide reference substance is destroyed through highly basic
Spectrogram；
Fig. 5 is relevant material detection HPLC colors under the chromatographic condition of embodiment 5 after andrographolide reference substance is destroyed through highly basic
Spectrogram；
Fig. 6 is the HPLC chromatogram of 0.001mg/mL andrographolide bulk drug methanol solutions；
Fig. 7 is the HPLC chromatogram of 1mg/mL andrographolide bulk drug methanol solutions.
Fig. 8 is the trial of chromatographic condition in document " one surveys the contents for commenting method to determine 5 lactone constituents in Herba Andrographitis more "；
Fig. 9 is that chromatographic condition is tasted in document " content analysis of 6 lactone constituents in Herba Andrographitis medicinal material and its preparation "
Examination.
Specific embodiment
Following is that the present invention is expanded on further in conjunction with specific embodiments.But these embodiments be only limitted to explanation the present invention without
It is to be used to limit the scope of the present invention.The experimental method of unreceipted specific experiment condition in the following example, generally according to routine
Condition.
In following embodiments, the andrographolide bulk drug comes from Yu Xin pharmaceutcal corporation, Ltds of Sichuan Province, and purity is more than
99.0%.Andrographolide reference substance is purchased from National Institute for Food and Drugs Control, purity 98.7%.
In following embodiments, detect the instrument and equipment that uses for：Agilent 1260Infinity high performance liquid chromatographs
(G1362A) (Agilent company of the U.S.)；DAD detectors (Agilent company of the U.S.).
After the andrographolide reference substance of embodiment 1 destroys (destructiveness 6%) through highly basic, it is tested about the detection of material
(1) andrographolide reference substance about 10mg is taken, it is accurately weighed, put in 10mL measuring bottles, plus methanol about 3mL, make its molten
Solution, adds 0.01mol/L NaOH solution 0.4mL, plus methanol dilution is to scale, shakes up.It is sub-packed in 2mL in cillin bottle, gland.
Adjusted after being placed in 65 DEG C of water-baths placement 15min with 0.01mol/L HCl to neutrality to be used as alkali to destroy solution to be measured.
(2) the alkali destruction solution in (1) step is determined using HPLC, chromatographic condition is as follows：Chromatographic column is Thermo C18
(150mm × 4.6mm, 3 μm, power ＆ light company)；Detection wavelength is 224nm；Column temperature is 30 DEG C, and flow velocity is 1.0mL/min；Sample size
For 10 μ L.With water (A)-acetonitrile (B) for mobile phase, gradient elution is carried out.The volume ratio of the mobile phase of gradient 1 is：A：B=77%：
It is gradient 2 that phase change is flowed after 23%, sample introduction 20min；The volume ratio of the mobile phase of gradient 2 is：A：B=70%：30%.Total operation
Time is 50min, and 15min is run afterwards.Chromatogram is recorded, Fig. 1 is seen.
In Fig. 1, retention time is that 12.716min chromatographic peaks are andrographolide chromatographic peak.As a result show, alkali destruction sample
In the liquid chromatogram of product, the separating degree between catabolite is all higher than 1.5, and andrographolide palliating degradation degree is about 6%.
HPLC chromatogram graph parameter after the andrographolide reference substance of table 1 destroys (destructiveness 6%) through highly basic
After the andrographolide reference substance of embodiment 2 destroys (destructiveness 47%) through highly basic, it is tried about the detection of material
Test
Andrographolide reference substance about 10mg is taken, it is accurately weighed, put in 10mL measuring bottles, plus methanol about 3mL, it is dissolved,
0.01mol/L NaOH solution 0.4mL are added, plus methanol dilution is to scale, shakes up.It is sub-packed in 2mL in cillin bottle, gland.It is placed in
70 DEG C of water-baths, which are placed, to be adjusted after 1h with 0.01mol/L HCl to neutrality to destroy solution to be measured as alkali.
Except above-mentioned condition changes other chromatographic conditions and specific steps be the same as Example 1.As a result Fig. 2 is seen.
In Fig. 2, retention time is that 12.714min chromatographic peaks are andrographolide chromatographic peak.As a result show, alkali destruction sample
Liquid chromatogram in, the separating degree between catabolite is all higher than 1.5, and andrographolide degradation rate is about 47%.As a result show, increase
Havoc intensity, each catabolite still can be separated well.
HPLC chromatogram graph parameter after the andrographolide bulk drug of table 2 destroys (destructiveness 47%) through highly basic
After the andrographolide reference substance of embodiment 3 is destroyed through strong acid, it is tested about the detection of material
(1) andrographolide reference substance about 10mg is taken, it is accurately weighed, put in 10mL measuring bottles, plus methanol about 3mL, make its molten
Solution, adds 0.01mol/L watery hydrochloric acid 0.4mL, plus methanol dilution is to scale, shakes up.It is sub-packed in 2mL in cillin bottle, gland.It is placed in
75 DEG C of water-baths, which are placed, to be adjusted after 1h with 0.01mol/L NaOH to neutrality to be used as acid destruction solution to be measured.
Except above-mentioned condition changes other chromatographic conditions and specific steps be the same as Example 1.As a result Fig. 3 is seen.
In Fig. 3, retention time is that 12.771min chromatographic peaks are andrographolide chromatographic peak.As a result show, acid destruction sample
Liquid chromatogram in, the separating degree between catabolite is all higher than 1.5, and andrographolide degradation rate is about 5%.
HPLC chromatogram graph parameter after the andrographolide bulk drug of table 3 is destroyed through strong acid
After the andrographolide reference substance of embodiment 4 is destroyed through highly basic, relevant agent detection test under different chromatographic conditions
Because the dopant species produced in highly basic failure test are more than acid destruction species, therefore with highly basic brokenization andrographolide
Bulk drug carries out relevant agent detection test under different chromatographic conditions.
(1) andrographolide reference substance about 10mg is taken, it is accurately weighed, put in 10mL measuring bottles, plus methanol about 3mL, make its molten
Solution, adds 0.01mol/LNaOH solution 0.4mL, plus methanol dilution is to scale, shakes up.It is sub-packed in 2mL in cillin bottle, gland.Put
Place and adjusted after 30min with 0.01mol/L HCl to neutrality to destroy solution to be measured as alkali in 65 DEG C of water-baths.
(2) need testing solution in (1) step is determined using HPLC, chromatographic condition is as follows：Detection wavelength is 230nm；Post
Temperature is that 35 DEG C of flow velocitys are 1mL/min；Sample size is 15 μ L.With water (A)-acetonitrile (B) for mobile phase, gradient elution is carried out.Gradient 1
The volume ratio of mobile phase is：A：B=80%：It is gradient 2 that phase change is flowed after 20%, sample introduction 20min；The body of the mobile phase of gradient 2
Accumulating ratio is：A：B=65%：35%.Total run time is 45min, and 10min is run afterwards.
In Fig. 4, retention time is that 13.248min chromatographic peaks are separating degree between andrographolide chromatographic peak, catabolite
1.5 are all higher than, andrographolide degradation rate is about 12%.
After the andrographolide bulk drug of table 4 is destroyed through highly basic, HPLC chromatogram graph parameter is detected under different chromatographic conditions
After the andrographolide reference substance of embodiment 5 is destroyed through highly basic, relevant agent detection test under different chromatographic conditions
Because the dopant species produced in highly basic failure test are more than check variety class, therefore with highly basic brokenization andrographolide
Bulk drug carries out relevant agent detection test under different chromatographic conditions.
(1) andrographolide raw material about 10mg is taken, it is accurately weighed, put in 10mL measuring bottles, plus methanol about 3mL, it is dissolved,
0.01mol/L NaOH solution 0.4mL are added, plus methanol dilution is to scale, shakes up.It is sub-packed in 2mL in cillin bottle, gland.It is placed in
65 DEG C of water-baths, which are placed, to be adjusted after 30min with 0.01mol/L HCl to neutrality to destroy solution to be measured as alkali.
(2) the alkali destruction solution in (1) step is determined using HPLC, chromatographic condition is as follows：Detection wavelength is 220nm；Post
Temperature is that 30 DEG C of flow velocitys are 1.0mLmin-1；Sample size is 15 μ L.With water (A)-acetonitrile (B) for mobile phase, gradient elution is carried out.
The volume ratio of the mobile phase of gradient 1 is：A：B=75%：It is gradient 2 that phase change is flowed after 25%, sample introduction 20min；The mobile phase of gradient 2
Volume ratio be：A：B=70%：30%.Total run time is 55min, and 10min is run afterwards.
In Fig. 5, retention time is that 11.653min chromatographic peaks are separating degree between andrographolide chromatographic peak, catabolite
1.5 are all higher than, andrographolide degradation rate is about 12%.
After the andrographolide bulk drug of table 5 is destroyed through highly basic, HPLC chromatogram graph parameter is detected under different chromatographic conditions
The andrographolide bulk drug of embodiment 6 its about material it is qualified degree detect
(1) andrographolide bulk drug is weighed, plus methanol is configured to the control that Determination of Andrographolide is 0.001mg/mL
Solution；Andrographolide raw material is weighed, plus methanol is configured to Determination of Andrographolide in need testing solution, the need testing solution
For 1000 times of Determination of Andrographolide in contrast solution.
(2) reference substance solution and need testing solution in (1) step, chromatographic condition and specific step are determined respectively using HPLC
Rapid be the same as Example 1.As a result Fig. 6 and Fig. 7 is seen.
In Fig. 6, the chromatographic peak that retention time is 12.805min is andrographolide chromatographic peak, and its peak area is
26.51258.In Fig. 7, the area of single impurity peaks is respectively less than andrographolide in reference substance solution chromatogram in need testing solution
Peak area.The apparent content of andrographolide bulk drug impurity is below 0.1%, without carrying out impurity structural identification.
Comparative example 1
Alkali is carried out using the chromatographic condition of document " one surveys the contents for commenting method to determine 5 lactone constituents in Herba Andrographitis more " to break
Bad Related substances separation.
(1) andrographolide reference substance about 10mg is taken, it is accurately weighed, put in 10mL measuring bottles, plus methanol about 3mL, make its molten
Solution, adds 0.01mol/L NaOH solution 0.4mL, plus methanol dilution is to scale, shakes up.It is sub-packed in 2mL in cillin bottle, gland.
Adjusted after being placed in 65 DEG C of water-baths placement 40min with 0.01mol/L HCl to neutrality to be used as alkali to destroy solution to be measured.
(2) the alkali destruction solution in (1) step is determined using HPLC, chromatographic condition is as follows：Chromatographic column：Thermo C18
(4.6mm × 250mm, 5 μm)；Detection wavelength is 226nm；Column temperature is that 25 DEG C of flow velocitys are 0.8mL/min；Sample size is 10 μ L.With
Water (A)-acetonitrile (B) is mobile phase, carries out gradient elution.0~15min, A：B=90%：10%；15~25min, A：B=
75%：25%；25~40min, A：B=60%：40%；40~50min, A：B=60%：40%；50~70min, A：B=
20%：80%.HPLC chromatogram is shown in Fig. 8.
In Fig. 8, retention time is that 23.640min chromatographic peaks are andrographolide chromatographic peak, and appearance time is later, and impurity
Peak is clearly separated bad.Therefore this literature method is not suitable for andrographolide Related substances separation.
Comparative example 2
Alkali is carried out using the chromatographic condition of document " content analysis of 6 lactone constituents in Herba Andrographitis medicinal material and its preparation "
Destroy Related substances separation.
(1) alkali destroys solution to be measured and prepared with comparative example 1.
(2) need testing solution in (1) step is determined using HPLC, chromatographic condition is as follows：Chromatographic column：Thermo C18
(4.6mm × 250mm, 5 μm)；Detection wavelength is 226nm；Column temperature is 25 DEG C；Flow velocity is 1.0mLmin-1；Sample size is 10 μ L.
With water (A)-acetonitrile (B) for mobile phase, gradient elution is carried out.0~10min, A：B=70%：30%；10~20min, A：B=
60%：40%；20~25min, A：B=60%：40%；25~40min, A：B=50%：50%；40~70min, A：B=
35%：65%.HPLC chromatogram is shown in Fig. 9.
In Fig. 9, retention time is that 8.600min chromatographic peaks are andrographolide chromatographic peak, impurity peaks 23.986min,
24.873min, 25.260min chromatographic peak separating degree are respectively less than 1.5.Therefore not to be suitable for andrographolide relevant for this literature method
Material is checked.
It should be understood that after the above-mentioned instruction content of the present invention has been read, those skilled in the art can be to present invention work
Various changes or modification, these equivalent form of values equally fall within the application appended claims limited range.
Claims (10)
1. a kind of a variety of methods about material of use hplc simultaneous determination andrographolide, it is characterised in that
The chromatographic condition used for：Stationary phase is the chromatographic column using octadecyl silane as filler；Mobile phase A is water, Mobile phase B
It is acetonitrile；Gradient elution is carried out, gradient condition is：The volume ratio of the mobile phase of gradient 1 is：A：B=75~80%：25~20%,
It is gradient 2 that phase change is flowed after 15~20min of sample introduction, and the volume ratio of the mobile phase of gradient 2 is：A：B=65~70%：35~
30%, total run time is 45~55min；220~230nm of Detection wavelength, column temperature is 30~35 DEG C；Elution flow rate be 0.5~
2.0mL/min。
2. according to the method described in claim 1, it is characterised in that the volume ratio of the described mobile phase of gradient 1 is：A：B=77：
23。
3. method according to claim 2, it is characterised in that the volume ratio of the described mobile phase of gradient 2 is：70：30.
4. method according to claim 3, it is characterised in that the Detection wavelength is 224nm.
5. method according to claim 4, it is characterised in that the elution flow rate is 1.0mL/min.
6. method according to claim 5, it is characterised in that during sample detection, sample injection volume is 10~15 μ L.
7. the method according to claim 1~6 any one, it is characterised in that in the 45~55min of total run time
Afterwards, then under the conditions of gradient 1 10~15min is run.
8. the method according to claim 1~6 any one, it is characterised in that the particle diameter of the filler of the chromatographic column is 2
~5 μm；Average diameter of particles is 4.6mm.
9. method according to claim 8, it is characterised in that the particle diameter of the filler is 3 μm.
10. method according to claim 9, it is characterised in that methods described includes andrographolide reference substance and treats test sample
Product match somebody with somebody processing procedure, andrographolide are dissolved from good solvent in process for preparation, the good solvent is methanol or acetonitrile,
Or the two mixture.
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Cited By (1)
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| CN109568264A (en) * | 2017-09-28 | 2019-04-05 | 神威药业集团有限公司 | A kind of andrographolide nano suspension |
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| CN102809625A (en) * | 2012-08-23 | 2012-12-05 | 神威药业集团有限公司 | Method for determining related substances of andrographolide |
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| CN109568264B (en) * | 2017-09-28 | 2021-09-28 | 神威药业集团有限公司 | Andrographolide nanosuspension |
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