CN101502616B - Method for measuring content of Bletilla striata medicinal materials - Google Patents
Method for measuring content of Bletilla striata medicinal materials Download PDFInfo
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- CN101502616B CN101502616B CN2009103008822A CN200910300882A CN101502616B CN 101502616 B CN101502616 B CN 101502616B CN 2009103008822 A CN2009103008822 A CN 2009103008822A CN 200910300882 A CN200910300882 A CN 200910300882A CN 101502616 B CN101502616 B CN 101502616B
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Abstract
The invention discloses a method for measuring the content of common bletilla pseudobulb medical materials. The method adopts bis(4-(Beta-D-pyranoglucose oxygen) benzyl)-2-isobutylmalate as a comparison product and uses high performance liquid chromatography to measure the content of the bis(4-(Beta-D-pyranoglucose oxygen) benzyl)-2-isobutylmalate of the common bletilla pseudobulb medical materials. The method is convenient, fast and accurate and provides good standard for controlling the quality of the common bletilla pseudobulb medical materials.
Description
Technical field
The present invention relates to the method for quality control of Bletilla striata medicinal materials, particularly relate to the content assaying method of Bletilla striata medicinal materials.
Background technology
Bletilla striata medicinal materials is the dry tuber of orchid Pseudobulbus Bletillae (Rhizoma Bletillae) Bletilla striata (Thunb.) Reichb.f., bitter in the mouth, sweet, puckery, cold nature, function with astringing to arrest bleeding, detumescence and promoting granulation, be a kind of Chinese medicine medical material commonly used, be used for ermine pancreas chapstick, in the Chinese patent medicines such as bone wound medicine (gushangling) spray.Along with deepening continuously of modern pharmacology research, find that it has obvious inhibitory action to tubercule bacillus, tumor cell etc.Clinical discovery, Bletilla striata medicinal materials also have better curative effect to commonly encountered diseases such as inside and outside hemorrhage, burn and scald etc.But as the raw medicinal material of medicine field, its content of effective must reach a certain standard, otherwise, can influence the quality that it is made into medicine at the using value and the crude drug of medicine field greatly.Still there is not report at present about the content assaying method in the Bletilla striata medicinal materials method of quality control.
Summary of the invention
Technical problem to be solved by this invention provides a kind of content assaying method of Bletilla striata medicinal materials, can convenient, fast and accurately carry out assay to the effective ingredient in the Bletilla striata medicinal materials.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme:
The content assaying method of Bletilla striata medicinal materials of the present invention is that [4-(β-D-Glucopyranose. oxygen) benzyl]-2-isobutyl group malate is a reference substance with two, with the content of two [4-(β-D-Glucopyranose. oxygen) benzyl]-2-isobutyl group malates (militarine) in the high effective liquid chromatography for measuring Bletilla striata medicinal materials.
Concrete, above-mentioned high performance liquid chromatography is made up of following steps:
(1) chromatographic condition and system suitability test: octadecylsilane chemically bonded silica is a filler, methanol: water=37: 63 (volume ratio) is mobile phase, the detection wavelength is 225nm, 40 ℃ of column temperatures, theoretical cam curve calculate by two [4-(β-D-Glucopyranose. oxygen) benzyl]-2-isobutyl group malates and are not less than 5000;
(2) preparation of reference substance solution: precision takes by weighing two [4-(β-D-Glucopyranose. oxygen) benzyl]-2-isobutyl group malate reference substances, adds 70% methanol solution and makes the solution that every 1ml contains 0.15mg, promptly;
(3) preparation of need testing solution: accurate ding white ware and the medicinal powder 0.1g of claiming, the accurate 70% methanol 25ml that adds claims to decide weight, supersound process 30 minutes, merceration 12 hours, supersound process is 30 minutes again, puts to room temperature, supplies the weight that subtracts mistake with 70% methanol, shake up, filter, get subsequent filtrate, promptly;
(4) algoscopy: accurate respectively reference substance solution and each 5 μ L of need testing solution of drawing, inject high performance liquid chromatography, measure, calculate content with one point external standard method, promptly.
In the preceding method, press the Bletilla striata medicinal materials dry product and calculate, the content of two [4-(β-D-Glucopyranose. oxygen) benzyl]-2-isobutyl group malates (militarine) is no less than 1.50% (weight).
The inventor has carried out great deal of experimental and method validation, has obtained technique scheme, and is specific as follows:
One, assay research:
(1) assay index choice: the inventor has carried out experimental study to the chemical constituent of Bletilla striata medicinal materials, the result therefrom separates and prepares two [4-(β-D-Glucopyranose. oxygen) the benzyl]-2-isobutyl group malates (militarine) of the chemical compound with active anticancer that content is higher, specificity is stronger, and [4-(β-D-Glucopyranose. oxygen) benzyl]-2-isobutyl group malate (militarine) is the assay index so selection is two.
(2) instrument and reagent: Agilent 1100 highly effective liquid phase chromatographic systems comprise quaternary gradient pump, variable-wavelenght detector, diode array detector, automatic sampler, 7725i hand sampling valve and Chemstation work station; The TCQ-250 ultrasonic cleaner; Chromatographic column, Symmetry C
18(5 μ m, 150mm * 4.6mm, Waters company); Two [4-(β-D-Glucopyranose. oxygen) benzyl]-2-isobutyl group malate (militarine) reference substances (Guizhou Province's Chinese medicine, the preparation of ethnic drug research and development centre, purity is greater than 98%); Methanol is that chromatographically pure, water are double distilled water.
(3) experimental condition is selected:
Extracting method: adopting 70% methanol is solvent, carries out ultrasonic, dipping, supersound extraction again.Through the methodology checking, this method is feasible.
Two, assay condition
Detect the selection of wavelength: according to the result that the HPLC-DAD of two [4-(β-D-Glucopyranose. oxygen) benzyl]-2-isobutyl group malate (militarine) reference substances measures, it has absorption maximum at 225nm place, so selection 225nm is as the detection wavelength.
Chromatographic condition is selected and the system suitability test: Hypersil C has been selected in test for use
18(5 μ m, 150mm * 4.6mm, Dalian Yi Lite), Diamonsil (diamond) C
18(5 μ m, 250mm * 4.6mm, Di Ma company) and Symmetry C
18(5 μ m, 150mm * 4.6mm, Waters company) chromatographic column, guard column is SecurityGuard C
18(5 μ m, 4.0mm * 3mm, Phenomenex inc.), with the methanol-water is mobile phase, the above-mentioned three kinds of chromatographic columns of result all can be separated two [4-(β-D-Glucopyranose. oxygen) benzyl]-2-isobutyl group malates (militarine) in the Pseudobulbus Bletillae (Rhizoma Bletillae) preferably, take all factors into consideration factors such as post pressure, disengaging time and separation case again, the main C that adopts of test
18Chromatographic column is tested, and determines that column temperature is 40 ℃.Under this chromatographic condition, the retention time of reference substance is about 16.2 minutes, and theoretical cam curve is calculated as 7200 by militarine, should be not less than 5000 (as Fig. 1) so the regulation theoretical cam curve is calculated by militarine.
Three, linear relationship is investigated and the working curve drafting
Linear relationship is investigated: accurate respectively reference substance storing solution (every 1ml contains 0.2158mg) 1 μ l, 2 μ l, 4 μ l, 6 μ l, the 12 μ l of drawing, inject liquid chromatograph, the record chromatograph, with peak area (Y) is vertical coordinate, sample size (X) is an abscissa, draw out working curve, the calculating regression equation is: Y=1505.91X-3.94, r=0.9999 (Fig. 2).The linear equation that fitted to initial point is Y=1503.64X, to calculate respectively in two equations more than the peak area substitution of minimum sample introduction concentration and maximum sample introduction concentration gained respectively, the relative deviation of low concentration sample introduction measurement result is respectively 0.23%, 1.30% as a result, the relative deviation of high concentration sample introduction measurement result is respectively 0.03%, 0.02%, illustrate that the working curve intercept is approximately zero, so adopt one point external standard method to calculate content.Under this experiment condition, the militarine sample size is in linear relation in 0.216～2.59 μ g scope.
Four, precision test
Replica test: get same lot number test sample, press 9 parts of test liquids of preparation method preparation of need testing solution, the difference sample introduction, the record chromatograph, the results are shown in Table 1, the militarine average content is 2.76%, and RSD is 1.10%, the result shows that the repeatability of militarine content assaying method is good in the preparation.。
Militarine assay replica test in table 1 need testing solution
| Numbering | Weighing (mg) | Content (%) | Meansigma methods (%) | ?RSD(％) |
| 1 | 79.1 | 2.76 | 2.76 | ?1.10 |
| 2 | 80.7 | 2.71 | ||
| 3 | 80.0 | 2.74 | ||
| 4 | 102.1 | 2.81 | ||
| 5 | 103.4 | 2.79 | ||
| 6 | 102.6 | 2.77 | ||
| 7 | 122.6 | 2.73 | ||
| 8 | 121.3 | 2.76 | ||
| 9 | 121.0 | 2.77 |
Middle precision test: at same date not, press the preparation of need testing solution preparation method with different analysts molten for examination, mensuration the results are shown in Table 2 respectively.
Precision test result relatively in the middle of the table 2
Five, accuracy test
Average recovery test: accurate weighing m ilitarine reference substance 27.92mg, put in the 50ml measuring bottle, add 70% dissolve with methanol and be diluted to scale, shake up, promptly, precision is measured above-mentioned solution 5 respectively, 10,15ml is in 3 100ml measuring bottles, be diluted to scale with 70% methanol respectively, shake up, get every 1ml and contain 0.02792,0.05584,0.08376mg the reference substance solution of three concentration, precision takes by weighing 9 parts in same lot number sample measuring militarine content (2.76%) respectively, accurate respectively each 25ml of solution of measuring above-mentioned 3 concentration adds conduct extraction solvent in the sample, prepares test liquid by the need testing solution preparation method, measures, the militarine average recovery rate is 98.7% as a result, and RSD is 1.90% (table 3).
Militarine recovery test result in table 3 Bletilla striata medicinal materials
| Numbering | Weighing (mg) | Content (mg) | Addition (mg) | The amount of recording (mg) | The response rate (%) | Meansigma methods (%) | ?RSD(％) |
| 1 2 3 4 5 6 7 8 9 | 51.9 52.0 53.8 49.2 50.5 52.3 53.3 54.1 50.8 | 1.4324 1.4352 1.4849 1.3579 1.3938 1.4435 1.4711 1.4932 1.4021 | 0.698 0.698 0.698 1.396 1.396 1.396 2.094 2.094 2.094 | 2.1248 2.1110 2.1795 2.7161 2.8006 2.8202 3.5172 3.6289 3.4207 | 99.2 96.8 99.5 97.3 100.8 98.6 97.7 102.0 96.4 | 98.7 | ?1.90 |
Six, serviceability test
Be to investigate the ruggedness of analytical method, compare example, different column temperature, the different wavelength that detects and respectively need testing solution is measured with the chromatographic column of three kinds of different trades mark, different flowing respectively, the result shows that the ruggedness of method is better.
Different chromatogram column analysis results compare: because the chromatographic column of different brands has certain difference in separation, therefore under same ratio mobile phase condition, the brand chromatographic column that has is bad to the separation of militarine in the Pseudobulbus Bletillae (Rhizoma Bletillae), therefore to adapt to each chromatographic column militarine in the Pseudobulbus Bletillae (Rhizoma Bletillae) is reached separation preferably by regulating the mobile phase ratio, same lot number test sample is measured, from table 4 result as seen, three kinds of brand chromatographic columns are to the measurement result unanimity of militarine in the Pseudobulbus Bletillae (Rhizoma Bletillae).
The different chromatographic column measurement results of table 4 relatively
Seven, different flowing compared routine measurement result relatively: use Symmetry C
18Chromatographic column is a mobile phase with the methanol-water, and by analyzing of different proportion, the mobile phase minor variations is to measurement result influence little (table 5) as a result.
Different the flowing of table 5 compared routine measurement result relatively
| Methanol: water | Content (%) | Meansigma methods (%) | ?RSD(％) | Overall average (%) | ?RSD(％) |
| 34∶66 | 2.80 2.75 2.76 | 2.77 | ?0.96 | 2.83 | ?2.5 |
| 37∶63 | 2.72 2.81 2.74 | 2.76 | ?1.71 | ||
| 40∶60 | 2.93 2.91 2.91 | 2.92 | ?0.40 |
Eight, different column temperature measurement results relatively: use Symmetry C
18Chromatographic column is measured with different chromatogram column temperatures, the results are shown in Table 6.
The different column temperature measurement results of table 6 relatively
| Chromatogram column temperature (℃) | Content (%) | Meansigma methods (%) | RSD(％) |
| 35 | 2.71 2.72 2.74 | 2.72 | 0.56 |
| 40 | 2.81 2.78 2.79 | 2.79 | 0.55 |
| 45 | 2.79 2.80 2.78 | 2.79 | 0.36 |
Nine, the different wavelength measurement results that detect compare: except that detecting wavelength change, all the other chromatographic conditions are constant, and same lot number test sample measurement result is seen Table 7.
Table 7 is different to detect the wavelength measurement result relatively
| Detect wavelength (nm) | Content (%) | Meansigma methods (%) | ?RSD(％) |
| 215 | 2.75 2.81 2.77 | 2.78 | ?1.10 |
| 225 | 2.78 2.76 2.74 | 2.76 | ?0.72 |
| 235 | 2.79 2.82 2.72 | 2.78 | ?1.85 |
Ten, need testing solution study on the stability: get same test sample, prepare test liquid by the need testing solution preparation method, respectively at 0,1,2,4,8 hour sample introduction, militarine peak area meansigma methods is 847.874 as a result, RSD is 0.33%, shows need testing solution stable (table 8) in 8 hours.
Table 8 need testing solution study on the stability
| Sample injection time (h) | 0 | 1 | 2 | 4 | 8 | Meansigma methods | ?RSD(％) |
| Peak area | 843.726 | 850.389 | 846.437 | 849.740 | 849.078 | 847.874 | ?0.33 |
11, sample determination
Get the Bletilla striata medicinal materials test sample, prepare need testing solution, cofabrication reference substance solution by the preparation method of need testing solution, sample introduction 5 μ l write down chromatograph respectively, measure peak area, calculate militarine content, 10 batches of Bletilla striata medicinal materials measurement results are 1.62%, 2.02%, 1.85%, 2.37%, 1.69%, 2.37%, 3.46%, 1.77%, 1.91%, 3.10%.
According to measurement result, this product is pressed dry product and is calculated, and contains militarine and must not be less than 1.50%.
Compared with prior art, the present invention selects two [4-(β-D-Glucopyranose. oxygen) benzyl]-2-isobutyl group malates (militarine) to measure the content of Bletilla striata medicinal materials for reference substance, this method is convenient, fast, accurate, for the quality control of Bletilla striata medicinal materials provides good standard.
Description of drawings
Fig. 1 is system suitability test HPLC figure;
Fig. 2 is the militarine working curve.
The specific embodiment
Measure the content of two [4-(β-D-Glucopyranose. oxygen) benzyl]-2-isobutyl group malates (militarine) in the Bletilla striata medicinal materials according to high performance liquid chromatography (" appendix VID of Chinese pharmacopoeia).
Instrument and reagent: Agilent 1100 highly effective liquid phase chromatographic systems comprise quaternary gradient pump, variable-wavelenght detector, diode array detector, automatic sampler, 7725i hand sampling valve and Chemstation work station; The TCQ-250 ultrasonic cleaner; Chromatographic column, Symmetry C
18(5 μ m, 150mm * 4.6mm, Waters company); Two [4-(β-D-Glucopyranose. oxygen) benzyl]-2-isobutyl group malate (militarine) reference substances (Guizhou Province's Chinese medicine, the preparation of ethnic drug research and development centre, purity is greater than 98%); Methanol is chromatographically pure, and water is double distilled water, and other reagent are analytical pure.
(1) chromatographic condition and system suitability test: octadecylsilane chemically bonded silica is a filler, methanol: water=37: 63 (volume ratio) is mobile phase, the detection wavelength is 225nm, 40 ℃ of column temperatures, theoretical cam curve calculate by two [4-(β-D-Glucopyranose. oxygen) benzyl]-2-isobutyl group malates and are not less than 5000;
(2) preparation of reference substance solution: precision takes by weighing two [4-(β-D-Glucopyranose. oxygen) benzyl]-2-isobutyl group malate reference substances, adds 70% methanol solution and makes the solution that every 1ml contains 0.15mg, promptly;
(3) preparation of need testing solution: accurate ding white ware and medicinal powder (the crossing sieve No. three) 0.1g of claiming, the accurate 70% methanol 25ml that adds claims to decide weight, supersound process 30 minutes, merceration 12 hours, supersound process is 30 minutes again, puts to room temperature, supplies the weight that subtracts mistake with 70% methanol, shake up, filter, get subsequent filtrate, promptly;
(4) algoscopy: accurate respectively reference substance solution and each 5 μ L of need testing solution of drawing, inject high performance liquid chromatography, measure, calculate content with one point external standard method, promptly.
This product is pressed dry product and is calculated, and contains two [4-(β-D-Glucopyranose. oxygen) benzyl]-2-isobutyl group malates (militarine) and is no less than 1.50% (weight).
Claims (2)
1. the content assaying method of a Bletilla striata medicinal materials, it is characterized in that: described high performance liquid chromatography is made up of following steps:
(1) chromatographic condition and system suitability test: octadecylsilane chemically bonded silica is a filler, the volume ratio of methanol and water be 37: 63 for mobile phase, the detection wavelength is 225nm, 40 ℃ of column temperatures, theoretical cam curve calculate by two [4-(β-D-Glucopyranose. oxygen) benzyl]-2-isobutyl group malates and are not less than 5000;
(2) preparation of reference substance solution: precision takes by weighing two [4-(β-D-Glucopyranose. oxygen) benzyl]-2-isobutyl group malate reference substances, adds 70% methanol solution and makes the solution that every 1ml contains 0.15mg, promptly;
(3) preparation of need testing solution: accurate ding white ware and the medicinal powder 0.1g of claiming, the accurate 70% methanol 25ml that adds claims to decide weight, supersound process 30 minutes, merceration 12 hours, supersound process is 30 minutes again, puts to room temperature, supplies the weight that subtracts mistake with 70% methanol, shake up, filter, get subsequent filtrate, promptly;
(4) algoscopy: accurate respectively reference substance solution and each 5 μ L of need testing solution of drawing, inject high performance liquid chromatography, measure, calculate content with one point external standard method, promptly.
2. according to the content assaying method of the described Bletilla striata medicinal materials of claim 1, it is characterized in that: press dry product and calculate, the content of two [4-(β-D-Glucopyranose. oxygen) benzyl]-2-isobutyl group malates is no less than 1.50% (weight).
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101863935B (en) * | 2010-06-04 | 2013-01-02 | 北京工业大学 | Preparation method of 1,4-di-[4-(glucosyloxy) benzyl]-2-isobutyl malate comparison product |
| CN103293261A (en) * | 2012-03-05 | 2013-09-11 | 贵州益佰制药股份有限公司 | Content determination method of rhizoma bletillae |
| CN105954411B (en) * | 2016-05-09 | 2019-01-11 | 贵州医科大学 | The measuring method of six kinds of ingredient absorption and transport amounts in Caco-2 cell model in bletilla |
| CN106924273B (en) * | 2017-02-23 | 2020-04-07 | 贵州医科大学 | Application of Militarine in preparation of heparin antagonist drugs |
| CN107340348B (en) * | 2017-06-07 | 2020-05-12 | 贵阳中医学院 | Method for establishing HPLC (high Performance liquid chromatography) fingerprint spectrum of rhizoma bletillae medicinal material |
| CN108606971A (en) * | 2018-03-28 | 2018-10-02 | 贵州医科大学 | Application of the bletilla glycosides in terms of preparing haemostatic medicament |
| CN109709225B (en) * | 2018-12-28 | 2022-02-18 | 贵州医科大学 | Qualitative and quantitative analysis method for milearine and metabolites thereof in plasma |
| CN111679015A (en) * | 2020-07-24 | 2020-09-18 | 张家港清蓝生物医药科技有限公司 | Bletilla striata small molecule characteristic fingerprint spectrum analysis method |
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| CN1895551A (en) * | 2006-06-15 | 2007-01-17 | 贵州太和制药有限公司 | Preparation of common bletilla tuber capsules |
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