CN102809625B - Method for determining related substances of andrographolide - Google Patents
Method for determining related substances of andrographolide Download PDFInfo
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Abstract
The invention provides a method for determining related substances of andrographolide. According to the method, HPLC (High Performance Liquid Chromatography) is used for determination; a chromatographic column with octadecylsilyl silica gel as filler is used; mobile phases A, B and C are water, acetonitrile and methyl alcohol, respectively, then gradient elution is carried out; flow velocity is 1mL/min, the detection wavelength is 200-260, the column temperature is 25-40 DEG C, the volume ratio of mobile phases at gradient 1: A:B:C is 60-75%: 25-35%:0-5%; and the volume ratio of mobile phases at gradient 2: A:B:C is 55-70%: 25-35%:5-10%. The method is simple to operate and good in stability and can be used for quickly and accurately determining contents of raw materials of andrographolide and related substances of preparations of andrographolide.
Description
Technical field
The present invention relates to technical field of analytical chemistry, especially a kind of assay method of andrographolide related substance.
Background technology
Andrographolide (Andrographolide, AND) calls andrographolide, and be the diterpene ginkgolide extracting in acanthaceous plant Herba Andrographitis and obtain, its structural formula is as follows:
。
Andrographolide is important extract and the effective active components of Herba Andrographitis, has the functions such as clearing heat and detoxicating, cool blood detumescence.Andrographolide preparation that is that gone on the market now or that be in the development phase mainly contains andrographolide tablet, ChuanxinlianNeizhi capsule and andrographolide injection.Andrographolide is raw material with Folium Andrographis, adopts the preparation raw material medicine that different extraction processes prepares.It can be used for preparing various andrographolide preparation.Andrographolide has ester class formation, in aqueous, particularly in high temperature, strong basicity environment, and facile hydrolysis, open loop, isomerization, resinification.Due to the instability of the chemical constitution of andrographolide own, in andrographolide bulk drug and preparation thereof except principal ingredient andrographolide, often there is neoandrographolide (Neoandrographolide simultaneously, NAND), deoxyandrographolide (Deoxyandro-grapholide, and the diterpene lactone impurity such as Dehydro and drographolide (Dehydroandrographolide, DDAND) DAND).Other impurity may introduced in the preparation of above-mentioned impurity and andrographolide raw material and preparation and storage and transport process are referred to as related substance.This related substance can produce certain impact to the security of andrographolide bulk drug and preparation and validity.Therefore, in Accurate Determining andrographolide raw material and preparation thereof, the content of related substance, is the important indicator correctly evaluating andrographolide bulk drug and the quality of the pharmaceutical preparations thereof.
In current detection andrographolide and preparation thereof, the Main Means of chemical composition content is high performance liquid chromatography, Deng Guihua, the people such as Lin Chaozhan disclose the content analysis method (" Pharmaceutical Analysis magazine " of 6 lactone compositions in a kind of Herba Andrographitis medicinal material and preparation thereof, 2011,31(2): 231 ~ 235), Kromasil RP-C is adopted
18(4.6mm*250 mm, 5 μm) chromatographic column, acetonitrile (A)-water (B) binary system gradient elution, elution program is as follows: 0 ~ 10 min, A phase is 30%; 10 ~ 20 min, A phase rises to 40%; 20 ~ 23 min, A phase maintains 40 %; 23 ~ 40 min, A phase rises to 50%; 40 ~ 70 min, A phase rises to 65%, flow velocity 1.0mL*min
-1, determined wavelength 226 nm, column temperature 25 DEG C.Take andrographolide, Dehydro and drographolide, deoxyandrographolide, neoandrographolide reference substance respectively in right amount, after adding methyl alcohol dissolving, be prepared into mixing reference substance solution; Take the powder of andrographolide medicinal material and tablet more respectively, be mixed with need testing solution, then according to the content of each composition above-mentioned in external standard method need testing solution.
At present, lack a kind of assay method of andrographolide related substance of easy and simple to handle, sensitive, good stability, can measure and evaluate its related substances during andrographolide raw material and related preparations preparation and stability test quickly and accurately.
Summary of the invention
The object of this invention is to provide a kind of method of mensuration andrographolide related substance of easy and simple to handle, good stability, so that its related substances in andrographolide bulk drug and preparation thereof can be measured quickly and accurately.
For realizing the object of the invention, the technical solution adopted in the present invention is:
An assay method for andrographolide related substance, step is as follows:
A () takes andrographolide reference substance, add methyl alcohol and be mixed with the reference substance solution that Determination of Andrographolide is 5 ~ 15 μ g/mL; Take andrographolide raw material or andrographolide preparation, add methyl alcohol and be mixed with need testing solution, in described need testing solution, Determination of Andrographolide is 100 times of Determination of Andrographolide in reference substance solution;
B () adopts HPLC to measure reference substance solution in a step and need testing solution respectively, chromatographic condition is as follows: select octadecyl silane to be the C18 chromatographic column of filler, take water as mobile phase A, acetonitrile is Mobile phase B, and methyl alcohol is that mobile phase C carries out gradient elution; Flow velocity is 1 mL/min, and determined wavelength is 200 ~ 260 nm, and column temperature is 25 ~ 40 DEG C, and the volume ratio of gradient 1 mobile phase is: A:B:C=60 ~ 75%: 25 ~ 35%: 0 ~ 5%, and after sample introduction 15 ~ 20min, mobile phase is changed to gradient 2; The volume ratio of gradient 2 mobile phase is: A:B:C=55 ~ 70%: 25 ~ 35%: 5 ~ 10%, is eluted to inclusion-free peak and occurs;
The reference substance solution recorded in (c) contrast b step and the chromatogram of need testing solution, in need testing solution single impurity peaks area < reference substance solution chromatogram in the half of andrographolide peak area, the area at andrographolide peak in the area of impurity peaks and < reference substance solution chromatogram in need testing solution.
The assay method of andrographolide related substance of the present invention, in a step reference substance solution, the content of andrographolide is preferably 10 μ g/mL, in b step, determined wavelength is preferably 224nm, column temperature is preferably 30 DEG C, the volume ratio of gradient 1 mobile phase is preferably A:B:C=70%: 30%: 0%, and after sample introduction 18min, mobile phase is changed to gradient 2; The volume ratio of gradient 2 mobile phase is preferably A:B:C=65%: 30%: 5%.Under this chromatographic condition, detection sensitivity is high, speed is fast, and theoretical cam curve calculates by andrographolide and is not less than 5000, and each Related Substances degree of separation is greater than 1.8.
The assay method of andrographolide related substance of the present invention, working time is preferably 50 ~ 55min, twice or when repeatedly measuring, best interval 15 ~ 20min, can avoid indivedual unknown impuritie retention time long, cause measuring error working time.
The assay method of andrographolide related substance of the present invention, the filler octadecyl silane described in it, preferred particulates degree is 5 μm, and average diameter of particles is the octadecyl silane of 4.6mm.Its separating effect to andrographolide related substance can be ensured thus further.
The assay method of andrographolide related substance of the present invention, adopt instrument auto injection, sample size is 10 uL, can avoid the error of the improper introducing of manual operation, improves the degree of accuracy of measurement.
The present invention adopts common C18 chromatographic column to carry out gradient elution, achieves the mensuration of andrographolide related substance rapidly and accurately.In gained chromatogram, mainly contain related substance neoandrographolide, between deoxyandrographolide and Dehydro and drographolide, and between each related substance and andrographolide chromatographic peak, reach good degree of separation (being greater than 1.5).Shown by the Study on degradation of andrographolide and Method validation, this method of the present invention has the indicative effect of stability, and achieve the limit handling to each impurity of andrographolide, this method is easy and simple to handle, with low cost, there is good economic benefit and promotion prospect.
Accompanying drawing explanation
Fig. 1 is the HPLC chromatic graph spectrum of system suitability sample;
In figure, retention time 9.74 min is AND(andrographolide) chromatographic peak; 23.08min is NAND chromatographic peak (neoandrographolide) relative retention time is 2.38); 31.49 min are DDAND chromatographic peak (Dehydro and drographolide) (relative retention time is 3.25); 33.77 min are DAND chromatographic peak (deoxyandrographolide) (relative retention time is 3.48).
Fig. 2 is the HPLC chromatogram of andrographolide preparation after high temperature;
In figure, retention time is 9.79 min chromatographic peaks is AND chromatographic peak, and 33.60 min are DAND chromatographic peak (relative retention time is 3.46).
Fig. 3 is the HPLC chromatogram of andrographolide bulk drug after highly basic destroys;
In figure, retention time is 9.82 min chromatographic peaks is AND chromatographic peak.Result shows, and alkali destroys in the liquid chromatography of sample, and the degree of separation that catabolite is shown in all is greater than 1.5, and the recovery of Study on degradation is 97.5%.
Embodiment
Further illustrate content of the present invention with specific embodiment below, but and mean never in any form and limit the invention.
In following embodiment, described andrographolide bulk drug is from Yu Xin pharmaceutcal corporation, Ltd of Sichuan Province, and wherein, Determination of Andrographolide is 98.7%.Described andrographolide preparation is andrographolide tablet.The impurity that the impurity that may exist in described andrographolide bulk drug and andrographolide preparation includes neoandrographolide, deoxyandrographolide, Dehydro and drographolide and introduces in preparation or storage and transport process.
Andrographolide reference substance is purchased from Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 110797-201108, neoandrographolide reference substance is purchased from Chun You bio tech ltd, Shanghai, lot number: 11082301, deoxyandrographolide reference substance is purchased from Chun You bio tech ltd, Shanghai, lot number: 11063001, Dehydro and drographolide reference substance is purchased from Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 110854-201007.
The instrument and equipment adopted during detection is: Agilent 1200 high performance liquid chromatograph, DAD detecting device, Chemstation Data Processing in Chromatography Workstation (Chinese edition), chromatographic column: Féraud door Genini C18,250 × 4.6 mm, 5 μm.The filler of described chromatographic column is octadecyl silane, and its granularity is 5 μm, and average diameter of particles is 4.6mm.During mensuration, adopt instrument auto injection, sample size is 10 μ L, twice or when repeatedly measuring, interval 15 ~ 20min.
Embodiment 1
System suitability
It is appropriate that precision takes andrographolide reference substance, neoandrographolide reference substance, deoxyandrographolide reference substance and Dehydro and drographolide reference substance, dissolves and be diluted to mixing reference substance solution after mixing with methyl alcohol.Wherein, the concentration of andrographolide, neoandrographolide, deoxyandrographolide and Dehydro and drographolide is followed successively by 35 μ g/mL, 100 μ g/mL, 75 μ g/mL, 50 μ g/mL.
Get mixing reference substance solution 10 μ L injection liquid chromatography, chromatographic condition is as follows: take water as mobile phase A, and acetonitrile is Mobile phase B, and methyl alcohol is that mobile phase C carries out gradient elution; Flow velocity is 1 mL/min, and determined wavelength is 224 nm, and column temperature is 30 DEG C, and the volume ratio of gradient 1 mobile phase is: A:B:C=70%: 30%: 0%, and after sample introduction 18min, mobile phase is changed to gradient 2; The volume ratio of gradient 2 mobile phase is: A:B:C=65%: 30%: 5%, regulates detection sensitivity, makes major component chromatogram peak height be about 20% ~ 25% of full scale, is eluted to inclusion-free peak and occurs, run 50 min.Chromatogram is shown in Fig. 1.
Result shows: between each peak, degree of separation is greater than 1.8, meets mensuration requirement, shows that the inventive method can be used for detecting the related substance in andrographolide raw material thus.
Embodiment 2
System suitability
It is appropriate that precision takes andrographolide reference substance, neoandrographolide reference substance, deoxyandrographolide reference substance and Dehydro and drographolide reference substance, dissolves and be diluted to mixing reference substance solution after mixing with methyl alcohol.Wherein, the concentration of andrographolide, neoandrographolide, deoxyandrographolide and Dehydro and drographolide is followed successively by 35 μ g/mL, 100 μ g/mL, 75 μ g/mL, 50 μ g/mL.
Get mixing reference substance solution 10 μ L injection liquid chromatography, chromatographic condition is as follows: take water as mobile phase A, and acetonitrile is Mobile phase B, and methyl alcohol is that mobile phase C carries out gradient elution; Flow velocity is 1 mL/min, and determined wavelength is 200 nm, and column temperature is 25 DEG C, and the volume ratio of gradient 1 mobile phase is: A:B:C=60%: 35%: 5%, and after sample introduction 15min, mobile phase is changed to gradient 2; The volume ratio of gradient 2 mobile phase is: A:B:C=55%: 35%: 10%, regulates detection sensitivity, makes major component chromatogram peak height be about 20% ~ 25% of full scale, is eluted to inclusion-free peak and occurs, run 55 min.Result shows: between each peak, degree of separation is greater than 1.5, and the degree of separation of deoxyandrographolide and Dehydro and drographolide chromatographic peak is greater than 1.8, meets mensuration requirement, shows that the inventive method can be used for detecting the related substance in andrographolide thus.
Embodiment 3
It is appropriate that precision takes andrographolide reference substance, neoandrographolide reference substance, deoxyandrographolide reference substance and Dehydro and drographolide reference substance, dissolves and be diluted to mixing reference substance solution after mixing with methyl alcohol.Wherein, the concentration of andrographolide, neoandrographolide, deoxyandrographolide and Dehydro and drographolide is followed successively by 35 μ g/mL, 100 μ g/mL, 75 μ g/mL, 50 μ g/mL.
Get mixing reference substance solution 10 μ L injection liquid chromatography, chromatographic condition is as follows: take water as mobile phase A, and acetonitrile is Mobile phase B, and methyl alcohol is that mobile phase C carries out gradient elution; Flow velocity is 1 mL/min, and determined wavelength is 260 nm, and column temperature is 40 DEG C, and the volume ratio of gradient 1 mobile phase is: A:B:C=75%: 25%: 0%, and after sample introduction 18min, mobile phase is changed to gradient 2; The volume ratio of gradient 2 mobile phase is: A:B:C=70%: 25%: 5%, regulates detection sensitivity, makes major component chromatogram peak height be about 20% ~ 25% of full scale, is eluted to inclusion-free peak and occurs, run 53 min.Result shows: between each peak, degree of separation is greater than 1.5, meets mensuration requirement.
The detection of related substance in embodiment 4 andrographolide bulk drug
A () takes andrographolide raw material, add methyl alcohol and be mixed with need testing solution, and in described need testing solution, Determination of Andrographolide is 1mg/mL;
B () employing HPLC measures the need testing solution in a step respectively, chromatographic condition is as follows: take water as mobile phase A, and acetonitrile is Mobile phase B, and methyl alcohol is that mobile phase C carries out gradient elution; Flow velocity is 1 mL/min, and determined wavelength is 224nm, and column temperature is 30 DEG C, and the volume ratio of gradient 1 mobile phase is: A:B:C=70%: 30%: 0%, and after sample introduction 18min, mobile phase is changed to gradient 2; The volume ratio of gradient 2 mobile phase is: A:B:C=65%: 30%: 5%, is eluted to inclusion-free peak and occurs; Degree of separation in gained chromatogram between each impurity chromatographic peak and between impurity and andrographolide chromatographic peak is greater than 1.8, meets the requirements, and shows that the inventive method can be used for detecting the related substance in andrographolide raw material thus.
The detection of related substance in embodiment 5 andrographolide tablet
A () gets andrographolide tablet, pulverize last, adds methyl alcohol and is mixed with need testing solution, and in described need testing solution, Determination of Andrographolide is 1mg/mL;
B () employing HPLC measures the need testing solution in a step respectively, chromatographic condition is as follows: take water as mobile phase A, and acetonitrile is Mobile phase B, and methyl alcohol is that mobile phase C carries out gradient elution; Flow velocity is 1 mL/min, and determined wavelength is 224nm, and column temperature is 30 DEG C, and the volume ratio of gradient 1 mobile phase is: A:B:C=70%: 30%: 0%, and after sample introduction 20min, mobile phase is changed to gradient 2; The volume ratio of gradient 2 mobile phase is: A:B:C=65%: 30%: 5%, is eluted to inclusion-free peak and occurs; Degree of separation in gained chromatogram between each impurity chromatographic peak and between impurity and andrographolide chromatographic peak is greater than 1.8, meets the requirements, and shows that the inventive method can be used for detecting the related substance in andrographolide tablet thus.
Under embodiment 6 andrographolide preparation high temperature storage condition, the detection experiment of its related substance
A () gets andrographolide parenteral solution, be positioned over 40 ± 2 DEG C, under 75 ± 5%RH condition, in sampling in 3rd month, precision is got in right amount (about containing andrographolide 25 mg), accurately weighed, puts in 25 mL measuring bottles, add methyl alcohol dissolve and be diluted to scale, shake up, as need testing solution.
B () employing HPLC measures the need testing solution in a step respectively, chromatographic condition is as follows: take water as mobile phase A, and acetonitrile is Mobile phase B, and methyl alcohol is that mobile phase C carries out gradient elution; Flow velocity is 1 mL/min, and determined wavelength is 224nm, and column temperature is 28 DEG C, and the volume ratio of gradient 1 mobile phase is: A:B:C=70%: 30%: 0%, and after sample introduction 18min, mobile phase is changed to gradient 2; The volume ratio of gradient 2 mobile phase is: A:B:C=65%: 30%: 5%, and be eluted to inclusion-free peak and occur, working time is 50min.Record chromatogram, is shown in Fig. 2.
In Fig. 2, retention time is 9.79 min chromatographic peaks is AND chromatographic peak, and 33.60 min are DAND chromatographic peak (relative retention time is 3.46).Result shows: the degree of separation between each impurity chromatographic peak and between impurity and andrographolide chromatographic peak is greater than 1.8.Show thus, being separated between each impurity and between impurity with main peak is good, meets the requirements, can be used for the determination of foreign matter of andrographolide preparation.
Embodiment 7 andrographolide preparation through highly basic destroy after, the detection experiment of its related substance
A () precision takes about 25 mg andrographolide reference substances and puts in 25 mL measuring bottles, the methyl alcohol adding about 10 mL makes it dissolve, then adds about 0.1 mol/L NaOH solution 3 mL, room temperature is placed, in sampling in the 5th day, with methanol dilution to scale, filter, subsequent filtrate is as need testing solution.
B () employing HPLC measures the need testing solution in a step respectively, chromatographic condition is as follows: take water as mobile phase A, and acetonitrile is Mobile phase B, and methyl alcohol is that mobile phase C carries out gradient elution; Flow velocity is 1 mL/min, and determined wavelength is 224nm, and column temperature is 28 DEG C, and the volume ratio of gradient 1 mobile phase is: A:B:C=70%: 30%: 0%, and after sample introduction 18min, mobile phase is changed to gradient 2; The volume ratio of gradient 2 mobile phase is: A:B:C=65%: 30%: 5%, and be eluted to inclusion-free peak and occur, working time is 50min.Record chromatogram, is shown in Fig. 3.
In Fig. 3, retention time is 9.82 min chromatographic peaks is AND chromatographic peak.Result shows, and alkali destroys in the liquid chromatography of sample, and the degree of separation between catabolite is all greater than 1.5, and the recovery of Study on degradation is 97.5%, meets the requirements.Show thus, the inventive method can be used for the inspection of andrographolide preparation related substance in process of production.
The qualified degree of its related substance of embodiment 8 andrographolide bulk drug detects
A () takes andrographolide reference substance, add methyl alcohol and be mixed with the reference substance solution that Determination of Andrographolide is 10 μ g/mL; Take andrographolide raw material, add methyl alcohol and be mixed with need testing solution, in described need testing solution, Determination of Andrographolide is 100 times of Determination of Andrographolide in reference substance solution;
B () adopts HPLC to measure reference substance solution in a step and need testing solution respectively, chromatographic condition is as follows: select octadecyl silane to be the chromatographic column of filler, take water as mobile phase A, acetonitrile is Mobile phase B, and methyl alcohol is that mobile phase C carries out gradient elution; Flow velocity is 1 mL/min, and determined wavelength is 224 nm, and column temperature is 30 DEG C, and the volume ratio of gradient 1 mobile phase is: A:B:C=70%: 30%: 0%, and after sample introduction 15 ~ 20min, mobile phase is changed to gradient 2; The volume ratio of gradient 2 mobile phase is: A:B:C=65%: 30%: 5%, is eluted to inclusion-free peak and occurs;
C, in () need testing solution, degree of separation is all greater than 1.5 between each impurity chromatographic peak and between impurity and andrographolide chromatographic peak.The reference substance solution recorded in contrast b step and the chromatogram of need testing solution, in need testing solution, the area of single impurity peaks is less than the half of andrographolide peak area in reference substance solution chromatogram, in need testing solution impurity peaks area and be less than the area at andrographolide peak in reference substance solution chromatogram.Therefore, the method for the invention accurately reflects the content of related substance in test sample, meets bound requirements.
Claims (2)
1. an assay method for andrographolide related substance, is characterized in that comprising the following steps: (a) takes andrographolide reference substance, adds methyl alcohol and is mixed with the reference substance solution that Determination of Andrographolide is 10 μ g/mL; Take andrographolide raw material or andrographolide preparation, add methyl alcohol and be mixed with need testing solution, in described need testing solution, Determination of Andrographolide is 100 times of Determination of Andrographolide in reference substance solution;
B () adopts HPLC to measure reference substance solution in a step and need testing solution respectively, chromatographic condition is as follows: select filler to be octadecyl silane, granularity is 5 μm, average diameter of particles is the C18 chromatographic column of 4.6mm, take water as mobile phase A, acetonitrile is Mobile phase B, and methyl alcohol is that mobile phase C carries out gradient elution; Flow velocity is 1 mL/min, and determined wavelength is 224nm, and column temperature is 30 DEG C, and the volume ratio of gradient 1 mobile phase is A:B:C=70%: 30%: 0%, and after sample introduction 18min, mobile phase is changed to gradient 2; The volume ratio of gradient 2 mobile phase is A:B:C=65%: 30%: 5%, and its working time is 50 ~ 55min, twice or repeatedly minute interval 15 ~ 20min, is eluted to inclusion-free peak and occurs;
The reference substance solution recorded in (c) contrast b step and the chromatogram of need testing solution, in need testing solution single impurity peaks area < reference substance solution chromatogram in the half of andrographolide peak area, the area at andrographolide peak in the area of impurity peaks and < reference substance solution chromatogram in need testing solution.
2. assay method according to claim 1, it is characterized in that described sample introduction adopts instrument auto injection, sample size is 10 uL.
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| CN105021723A (en) * | 2015-07-06 | 2015-11-04 | 广西壮族自治区药用植物园 | Method for simultaneous determination of content of geniposide, andrographolide and dehydroandrographolide in Zhimai tablets for clearing heat |
| CN105699546A (en) * | 2016-04-25 | 2016-06-22 | 广西壮族自治区梧州食品药品检验所 | Method for measuring content of effective components in herba andrographitis tablets through liquid mass series method |
| CN106990198A (en) * | 2017-04-27 | 2017-07-28 | 沈阳药科大学 | It is a kind of at the same determine a variety of methods about material of andrographolide |
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