CN103091441A - Quality detecting method of alpinia zerumbet medicinal material - Google Patents
Quality detecting method of alpinia zerumbet medicinal material Download PDFInfo
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- CN103091441A CN103091441A CN201310056136XA CN201310056136A CN103091441A CN 103091441 A CN103091441 A CN 103091441A CN 201310056136X A CN201310056136X A CN 201310056136XA CN 201310056136 A CN201310056136 A CN 201310056136A CN 103091441 A CN103091441 A CN 103091441A
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Abstract
The invention discloses a quality detecting method of an alpinia zerumbet medicinal material. The quality detecting method comprises the following steps of: preparation of a test solution and preparation of a comparison solution, wherein the chromatographic conditions are as follows: a chromatographic column is an AgilentEclipseXDB-C18 column (150mm*4.6mm, 5 microns); a volume ratio of (flowing phases) water to acetonitrile equals to 80:20; a flow rate is 1mL/min; the detecting wavelength is 345nm, the column temperature is 25 DEG C; and the feeding quantity is 10 microliters. A content determination method comprises the steps of: respectively and accurately absorbing 10 microliters of comparison solution and 10 microliters of test solution, injecting the comparison solution and the test solution into a liquid chromatograph, and determining the solutions according to a high performance liquid chromatography, wherein the content of demethoxyyangonin is not less than 5mg/g by taking anhydrous substance as a reference. The quality detecting method of the alpinia zerumbet medicinal material is high in accuracy, reliable, easy to operate, good in reproducibility, and capable of effectively controlling the quality of the alpinia zerumbet medicinal material.
Description
Technical field
The invention belongs to technical field of traditional Chinese medicines, particularly a kind of quality determining method of shellflower medicinal material.
Background technology
Shellflower be the zingiberaceous plant shellflower (
Alpinia zerumbet(Pers.) Burtt.et Smith) fresh or dry mature fruit.
Proterties: this product is spherical in shape, and two ends are point slightly, is about 2cm, diameter 1.5cm, and yellowish-brown, slightly glossy, the vertical rib of ten several protuberances is arranged, tool one projection in top is the perianth residue, the tool carpopodium mark of break that base portion has.Seed group's lobe is arranged loose, easily is scattered, and aril is membranous, white.Seed is polyhedron, long 0.4～0.5cm, diameter 0.3～0.4cm.Gas is little, lightly seasoned, little suffering.
Differentiate:
1. seed square section: it is square to plant epidermis chrotoplast class.Be 2～3 row cells under epidermis, rectangle or class are square, and tangential the arrangement includes the tawny material, and uvea is the brown cell of ordered series of numbers, and wherein faling apart has the similar round oil droplet; Endotesta is 1 row palisade lithocyte, brown color, and inwall and sidewall are extremely thick, and cell is little, includes siliceous.The perisperm cell contains the calcium oxalate prismatic crystal.
The powder taupe brown.The aril cell is larger, Chang Chengtuan; Individual cells is spindle, some ovalizes, and end expands more, contains granular substance in the born of the same parents of chamber.Plant the epidermis chrotoplast and be polygon, common lower epidermis cell is overlapping with it, and the lower epidermis cell is thin, lithocyte cerioid or similar round.Eleocyte is larger, and oval contains brown thing.
2. get this product meal 1g, add sherwood oil (60～90 ℃) 10mL, dipping spends the night, and filters, and filtrate is brown color, puts under ultraviolet lamp (365nm) and observes, aobvious yellow-white fluorescence.Drip 5% vanillic aldehyde sulfuric acid solution, aobvious purple is to mulberry.
Shellflower is now included in " Guizhou Province's Chinese medicine, ethnic drug standard " (2003 editions), only includes the proterties of medicinal material in standard and differentiates, therefore, the quality of shellflower medicinal material can't be effectively controlled.Contain in the shellflower water extract and have bioactive pyrone compound de-methoxy kawain, this compound can antagonistic experiment gastric and duodenal ulcer, is one of effective substance of shellflower.
Summary of the invention
A kind of accuracy that the object of the invention is to overcome above-mentioned shortcoming and provide is high, reliable, easy operating, favorable reproducibility, can effectively control the quality determining method of the shellflower medicinal material of shellflower quality of medicinal material.
The quality determining method of a kind of shellflower medicinal material of the present invention comprises the following steps:
(1) preparation of need testing solution: precision takes 0.5g medicinal powder (crossing 60 mesh sieves), and precision adds 30mL methyl alcohol, and precise weighing is bathed refluxing extraction 2h at 80 ℃ of Water Unders, take off and let cool, precise weighing is mended weight loss with methyl alcohol, shake up, miillpore filter (0.45 μ m) filters, and get final product;
(2) preparation of reference substance solution: precision takes the de-methoxy kawain reference substance that is dried to constant weight through phosphorus pentoxide and adds the methyl alcohol dissolving, make the reference substance solution that every 1mL contains de-methoxy kawain 0.204mg, it is 0.122(mg/ml that this solution dilution is become concentration) reference substance solution and get final product;
(3) chromatographic condition: chromatographic column: Agilent Eclipse XDB-C18 post (150mm * 4.6 mm, 5 μ m) post; Water-acetonitrile (80: 20) is mobile phase; Flow velocity is 1mL/min; Detect wavelength 345nm, column temperature: 25 ℃; Sample size: 10 μ L;
(4) content assaying method: precision is drawn reference substance solution and each 10 μ L of need testing solution respectively, and the injection liquid chromatography is according to high effective liquid chromatography for measuring.
The quality determining method of above-mentioned shellflower medicinal material, the wherein preparation of (2) step reference substance solution: precision takes the de-methoxy kawain reference substance 5.1mg that is dried to constant weight through phosphorus pentoxide and puts in the 25mL volumetric flask, adding methyl alcohol dissolves and is diluted to scale, shake up, make the reference substance solution that every 1mL contains de-methoxy kawain 0.204mg, it is 0.122(mg/ml that this solution dilution is become concentration) reference substance solution and get final product.
The quality determining method of above-mentioned shellflower medicinal material, wherein: de-methoxy kawain content must not be lower than 5mg/g(in dry product).
The quality determining method of above-mentioned shellflower medicinal material, wherein: the shellflower medicinal material is shellflower medicinal material and various various preparations take the shellflower medicinal material as raw material.
The present invention compared with prior art, has obvious beneficial effect, by above technical scheme as can be known: through literature survey research, contain in the shellflower water extract and have bioactive pyrone compound de-methoxy kawain, this compound energy antagonistic experiment gastric and duodenal ulcer, one of effective substance of shellflower, therefore determine to adopt the content of de-methoxy kawain in high effective liquid chromatography for measuring shellflower medicinal material.The results showed, de-methoxy kawain and other component degree of separation are good, and linear relationship, reappearance, precision, stability, the recovery are all better.The preparation method of need testing solution can access testing result preferably, and therefore, method accuracy of the present invention and sensitivity all higher, advanced technology, operation are fast and convenient, can make the quality of shellflower medicinal material and preparation thereof obtain more effective control.
Embodiment
Below further illustrate the beneficial effect of the inventive method by concrete experimental example.
Embodiment 1
A kind of quality determining method of shellflower medicinal material comprises the following steps:
(1) preparation of need testing solution: precision takes 0.5g medicinal powder (crossing 60 mesh sieves), precision adds 30mL methyl alcohol, precise weighing, bathe refluxing extraction 2h at 80 ℃ of Water Unders, take off and let cool, precise weighing, mend weight loss with methyl alcohol, shake up, miillpore filter (0.45 μ m) filters, and get final product;
Take respectively two Duplicate Samples S
1, S
2:
(2) preparation of reference substance solution: precision takes the de-methoxy kawain reference substance 5.1mg that is dried to constant weight through phosphorus pentoxide and puts in the 25mL volumetric flask, adding methyl alcohol dissolves and is diluted to scale, shake up, make the reference substance solution that every 1mL contains de-methoxy kawain 0.204mg.It is 0.122(mg/ml that above-mentioned storing solution solution dilution is become concentration) reference substance solution, standby.
(3) chromatographic condition: chromatographic column: Agilent Eclipse XDB-C18 post (150mm * 4.6 mm, 5 μ m) post; Water-acetonitrile (80: 20) is mobile phase; Flow velocity is 1mLmin
-1Detect wavelength 345nm, column temperature: 25 ℃; Sample size: 10 μ L.
Content assaying method: accurate reference substance solution and two parts of each 10 μ L injection liquid chromatographies of need testing solution drawn respectively, according to high effective liquid chromatography for measuring, record chromatogram, measure peak area, with the content of de-methoxy kawain in the following formula calculation sample:
As: the peak area of need testing solution; Ar: the peak area of reference substance solution;
Cs: reference substance concentration (mg/ml);
Ms: test sample sampling amount (g); V: constant volume (ml)
Measurement result:
| Sample introduction | Reference substance solution | S 1 | S 2 |
| Retention time (min) | 12.73 | 12.70 | 12.76 |
| Peak area | 1508.7 | 1081.3 | 1092.7 |
2. calculate: (average content 5.2mg/g)
Embodiment 2
A kind of quality determining method of shellflower medicinal material comprises the following steps:
(1) preparation of need testing solution: precision takes 0.5g medicinal powder (crossing 60 mesh sieves), precision adds 30mL methyl alcohol, precise weighing, bathe refluxing extraction 2h at 80 ℃ of Water Unders, take off and let cool, precise weighing, mend weight loss with methyl alcohol, shake up, miillpore filter (0.45 μ m) filters, and get final product.；
Take respectively two Duplicate Samples S
1, S
2:
All the other are with embodiment 1
Measurement result:
| Sample introduction | Reference substance solution | Sample 1 | Sample 2 |
| Retention time (min) | 12.73 | 12.70 | 12.76 |
| Peak area | 1528.7 | 1120.5 | 1132.1 |
2. calculate: (average content 3.0270g/ bag)
Embodiment 3-12
Ten batches of test sample measurement results of embodiment 3-12 see the following form (method is with embodiment 1):
| Embodiment | Batch | De-methoxy kawain content (mg/g) |
| 3 | 201107255 | 5.42 |
| 4 | 201107262 | 5.01 |
| 5 | 201107261 | 9.60 |
| 6 | 201107254 | 5.81 |
| 7 | 201107234 | 6.65 |
| 8 | 201107231 | 5.32 |
| 9 | 201108102 | 5.55 |
| 10 | 201108042 | 6.34 |
| 11 | 201108092 | 9.02 |
| 12 | 201108091 | 5.05 |
According to the above embodiment 1-12 assay result of totally 12 batch samples, and consider the difference of the medicinal material place of production, collecting period and quality, determine that this medicinal material de-methoxy kawain content must not be lower than 5mg/g(in dry product).
Test example
1, sample pre-treatments
(1) proterties: see above-mentioned shellflower quality of medicinal material standard, 12 batch samples are all described consistent therewith.
(2) differentiate: according to " Guizhou Province's Chinese medicine, ethnic drug standard " (2003 editions) regulation.
(3) assay: in " Guizhou Province's Chinese medicine, ethnic drug standard " (2003 editions) to there is no the assay index in shellflower quality of medicinal material control method, but the pyrone compound de-methoxy kawain in medicinal material has biologically active, this compound energy antagonistic experiment gastric and duodenal ulcer, one of effective substance of shellflower, so this method has been set up the assay method of HPLC method mensuration to the de-methoxy kawain in the shellflower medicinal material.
(4) medicine and medicament: de-methoxy kawain reference substance (Baoji time bio tech ltd, lot number: 20101029, purity＞98%); Shellflower medicinal material (Yuanchen Pharmaceutical Co., Ltd., Guizhou Prov. provides); Acetonitrile (chromatographically pure, U.S. world reagent company), methyl alcohol, hydrochloric acid, phosphoric acid (analyzing pure), water (ultrapure water).
(5) instrumental analysis condition: instrument is Agilent 1100 high performance liquid chromatographs, VWD detecting device, Agilent 1100 chem workstations.
(6) chromatographic condition: Agilent Eclipse XDB-C18 post (150mm * 4.6 mm, 5 μ m) post; Water-acetonitrile (80: 20) is mobile phase; Flow velocity is 1mLmin
-1Detect wavelength 345nm, column temperature: 25 ℃; Sample size: 10 μ L.
(7) selection processed of need testing solution: the effects the extraction effect of heating and refluxing extraction and ultrasonic extraction, find that heating and refluxing extraction method extraction efficiency is better than ultrasonic extraction, therefore adopt the heating and refluxing extraction method.Simultaneously, investigated extraction solvent and extraction time, methyl alcohol is optimum extraction condition as extracting solvent, adding hot reflux 2h.
2, methodological study
2.1 the range of linearity
It is 0.204 mgmL that precision measures concentration
-1Reference substance solution 2,4,6,8 ml put in 10 mL volumetric flasks, add methyl alcohol and are diluted to scale, shake up, and forming together concentration range with mother liquor is 0.0408-0.204 mgmL
-1The series reference substance solution.Precision measures this series reference substance solution 10 μ L respectively, the injection liquid chromatography, measure peak area by above-mentioned chromatographic condition, and take the sample size X (μ g) of reference substance as horizontal ordinate, peak area integrated value Y is ordinate, carry out linear regression, the regression equation that gets the de-methoxy kawain is: Y=10757.6X+151.4 r=0.9993.
2.2 sample introduction precision test
Precision measures above-mentioned de-methoxy kawain reference substance solution 10 μ L, by above-mentioned chromatographic condition, continuous sample introduction 6 times, measures peak area, and calculating RSD is 1.7%, illustrates that this instrument has good precision.
2.3 stability test
Get same need testing solution, measure 10 μ L sample introductions respectively at 0,1,2,3,4 h precisions, the RSD that records de-methoxy kawain peak area is 1.7%.Result shows, need testing solution is stable in 4 h at least.
2.4 replica test
6 parts of sample thiefs (Ecological effect), accurately weighed, by 2.3 below legal system available test solutions, recording de-methoxy kawain average content is 5.4 mgg respectively
-1, RSD is 2.4%.Result shows, the repeatability of method is good
2.5 recovery test
Get sample (Ecological effect) 0.25g (theoretical content 5.4 mg/g) of known content, accurately weighed, precision adds a certain amount of de-methoxy kawain respectively, press need testing solution preparation below legal system available test sample solution, measure by the said determination method, calculate recovery rate the results are shown in Table 1.Average recovery rate (n=6) is 99.15%.
The above, it is only preferred embodiment of the present invention, be not that the present invention is done any pro forma restriction, any technical solution of the present invention content that do not break away from,, all still belong in the scope of technical solution of the present invention any simple modification, equivalent variations and modification that above embodiment does according to technical spirit of the present invention.
Claims (4)
1. the quality determining method of a shellflower medicinal material comprises the following steps:
(1) preparation of need testing solution: precision takes the 0.5g medicinal powder, crosses 60 mesh sieves, and precision adds 30mL methyl alcohol, and precise weighing is bathed refluxing extraction 2h at 80 ℃ of Water Unders, take off and let cool, precise weighing is mended weight loss with methyl alcohol, shake up, 0.45 μ m filtering with microporous membrane, and get final product;
(2) preparation of reference substance solution: precision takes the de-methoxy kawain reference substance that is dried to constant weight through phosphorus pentoxide and adds the methyl alcohol dissolving, make the reference substance solution that every 1mL contains de-methoxy kawain 0.204mg, to become concentration be the reference substance solution of 0.122mg/ml and get final product with this solution dilution;
(3) chromatographic condition: chromatographic column: Agilent Eclipse XDB-C18 post 150mm * 4.6 mm, 5 μ m posts; Water: the acetonitrile volume ratio is=80: 20 for mobile phase; Flow velocity is 1mL/min; Detect wavelength 345nm, column temperature: 25 ℃; Sample size: 10 μ L;
(4) content assaying method: precision is drawn reference substance solution and each 10 μ L of need testing solution respectively, and the injection liquid chromatography is according to high effective liquid chromatography for measuring.
2. the quality determining method of shellflower medicinal material as claimed in claim 1, the wherein preparation of (2) step reference substance solution: precision takes the de-methoxy kawain reference substance 5.1mg that is dried to constant weight through phosphorus pentoxide and puts in the 25ml volumetric flask, adding methyl alcohol dissolves and is diluted to scale, shake up, make the reference substance solution that every 1mL contains de-methoxy kawain 0.204mg, to become concentration be the reference substance solution of 0.122mg/ml and get final product with this solution dilution.
3. the quality determining method of shellflower medicinal material as claimed in claim 1 or 2, wherein: de-methoxy kawain content must not be lower than 5mg/g in dry product.
4. the quality determining method of shellflower medicinal material as claimed in claim 3, wherein: the shellflower medicinal material is shellflower medicinal material and various various preparations take the shellflower medicinal material as raw material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110658274A (en) * | 2019-09-27 | 2020-01-07 | 宁夏医科大学 | Quantitative detection method for effective components in kava pepper medicinal material |
| CN110658273A (en) * | 2019-09-27 | 2020-01-07 | 宁夏医科大学 | Method for rapidly detecting effective components in kava pepper medicinal material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000184867A (en) * | 1998-11-27 | 2000-07-04 | Minoru Kuniyoshi | Medicinal drink of shell-flower |
| US20060251715A1 (en) * | 2001-10-03 | 2006-11-09 | Robert Gow | Oral delivery of a botanical |
-
2013
- 2013-02-22 CN CN201310056136XA patent/CN103091441A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000184867A (en) * | 1998-11-27 | 2000-07-04 | Minoru Kuniyoshi | Medicinal drink of shell-flower |
| US20060251715A1 (en) * | 2001-10-03 | 2006-11-09 | Robert Gow | Oral delivery of a botanical |
Non-Patent Citations (1)
| Title |
|---|
| 乔春峰等: "HPLC法分析山姜属植物中的8种活性成分", 《天然产物研究与开发》, vol. 20, no. 3, 15 June 2008 (2008-06-15), pages 422 - 426 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110658274A (en) * | 2019-09-27 | 2020-01-07 | 宁夏医科大学 | Quantitative detection method for effective components in kava pepper medicinal material |
| CN110658273A (en) * | 2019-09-27 | 2020-01-07 | 宁夏医科大学 | Method for rapidly detecting effective components in kava pepper medicinal material |
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Application publication date: 20130508 |