CN104634903A - Method for determining content of three effective components in callicarpa nudiflora medicinal material - Google Patents
Method for determining content of three effective components in callicarpa nudiflora medicinal material Download PDFInfo
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Abstract
The invention relates to a method for determining content of three effective components in a callicarpa nudiflora medicinal material, the three effective components comprise verbascoside, luteolin and 5,4'-dihydroxy-3,7,3'-trimethoxyflavone, which belongs to the medicine field. The method is characterized by employing a high performance liquid chromatography, the chromatogram condition and system applicability are characterized in that octadecylsilane chemically bonded silica is a filler, a mobile phase is an organic solvent-acidic solution, gradient elution is employed, concentration of an acidic solution is 0-0.3%, the detection wavelength is 320-360nm, and column temperature is 25-40 DEG C. According to the invention, an analysis method for simultaneous determination of content of several effective components in the callicarpa nudiflora medicinal material can be established, method is reliable and is easy to operate, quality standard of the callicarpa nudiflora medicinal material is increased, and quality of the callicarpa nudiflora medicinal material and clinical curative effect are ensured.
Description
Technical field
The present invention relates to the assay method of three kinds of active constituent contents in callicarpa nudiflora medicinal material, be specifically related to acteoside in callicarpa nudiflora medicinal material, cyanidenon, 5,4 '-dihydroxy-3,7, the assay method of 3 '-trimethoxy flavone, three kinds of active constituent contents, belongs to field of medicaments.
Background technology
Callicarpa nudiflora (
callicarpa nudiflorahook. Et A rn.) be Verenaceae Callicarpa plant.Multitude's medicine name mends valve, main product in Hainan, Guangdong and Guangxi.Its leaf mildly bitter flavor, puckery, property is put down; There is antibacterial anti hemorrhagic, eliminating inflammation and expelling toxin, the function of eliminating stasis to subdue swelling.For purulent inflammation, acute infectious hepatitis, respiratory tract and hemorrhage of digestive tract, thrombocytopenic purpura; Burn and traumatism and bleeding are controlled in external application, are one of Nationality in Hainan Province doctor medicinal herbs most in use.
Less to the research report of callicarpa nudiflora chemical composition both at home and abroad, the composition be therefrom separated mainly contains flavonoids, terpene, volatile oil and phenols etc.Callicarpa nudiflora middle flavone compound mainly contains cyanidenon and glycocide thereof; From callicarpa nudiflora leaf, separation obtains phenolic compound and mainly contains phenolic glycoside class as acteoside, samioside, Forsythoside etc.
The method that callicarpa nudiflora quality research is commonly used has microscopical characters method, thin-layer chromatography (TLC) method, ultraviolet spectrophotometer method, high performance liquid chromatography (HPLC) method etc.Flavonoids, terpene and phenolic glycoside class is mainly contained in the active constituent content measuring method report of callicarpa nudiflora medicinal material or its Chinese medicine preparation.Content assaying method many employings high performance liquid chromatography at present for effective constituent in callicarpa nudiflora medicinal material and preparation thereof carries out assay to wherein a certain effective constituent such as cyanidenon, acteoside, oleanolic acid etc., bibliographical information is a lot, and patent is as the Chinese patent assay method of acteoside content " in the callicarpa nudiflora preparation " (application number: 201010289134.1).The quality standard that this employing single active ingredient content controls medicinal material and preparation thereof can not control quality of medicinal material comprehensively, and adopt different measuring methods to measure the content of two or more effective constituent, thing must make mensuration work heavy, determination period extends, and is unfavorable for that real work is particularly promoted in the large production of enterprise and operation.The assay method of the two or more effective constituent of a kind of condition determination of current employing Simultaneously test rarely has report.
The invention provides a kind of assay method, adopt high performance liquid chromatography can acteoside, cyanidenon and 5 in the callicarpa nudiflora medicinal material of Simultaneously test, 4 '-dihydroxy-3,7, the content of 3 '-trimethoxy flavone, three kinds of effective constituents.The analytical approach of multiple active constituent content in this Simultaneously test is callicarpa nudiflora medicinal material, the method that not only perfect callicarpa nudiflora quality of medicinal material controls, and also method is reliable, and easy to operate.
Summary of the invention
The object of the present invention is to provide acteoside, cyanidenon and 5 in the callicarpa nudiflora medicinal material of a kind of Simultaneously test, 4 '-dihydroxy-3,7, the assay method of 3 '-trimethoxy flavone, three kinds of active constituent contents.
The technical scheme realizing the object of the invention is as follows:
Adopt acteoside, cyanidenon and 5 in the callicarpa nudiflora medicinal material of high-performance liquid chromatogram determination, 4 '-dihydroxy-3,7,3 '-trimethoxy flavone, three kinds of active constituent contents.Chromatographic condition and system suitability are: be filling agent with octadecylsilane chemically bonded silica, and mobile phase is organic solvent-acid solution, adopt gradient elution, as follows:
0-10min organic solvent ratio is 10% ~ 50%;
10-20min organic solvent ratio is 20% ~ 60%;
20-30min organic solvent ratio is 25% ~ 70%;
30-40min organic solvent ratio is 30% ~ 80%;
40-50min organic solvent ratio is 35% ~ 80%;
50-60min organic solvent ratio is 40% ~ 80%,
Acid solution concentration is 0-0.3%, determined wavelength 320-360nm, column temperature 25 DEG C-40 DEG C.
Organic solvent in described mobile phase comprises the one in methyl alcohol or acetonitrile, and methyl alcohol and acetonitrile are chromatographically pure; The acid of acid solution comprises the one in phosphoric acid, acetic acid or formic acid, and it is pure that phosphoric acid, acetic acid and formic acid are analysis.
Described chromatographic condition and system suitability are preferably: be filling agent with octadecylsilane chemically bonded silica, and mobile phase is methyl alcohol-0.15% phosphate aqueous solution, adopt gradient elution, as follows:
0-5min methyl alcohol-0.15% phosphate aqueous solution 38:62;
5-14min methyl alcohol-0.15% phosphate aqueous solution 45:55;
14-23min methyl alcohol-0.15% phosphate aqueous solution 60:40;
23-30min methyl alcohol-0.15% phosphate aqueous solution 70:30;
30-35min methyl alcohol-0.15% phosphate aqueous solution 75:25,
Determined wavelength 350nm, column temperature 40 DEG C.
Prepared by reference substance solution: get acteoside, cyanidenon and 5,4 '-dihydroxy-3,7,3 '-trimethoxy flavone reference substance is appropriate, accurately weighed, add 75% methyl alcohol dissolving and about make every 1 mL respectively respectively containing acteoside 1.48 ㎎, cyanidenon 0.05 ㎎ and 5,4 '-dihydroxy-3,7, the mixing reference substance solution of 3 '-trimethoxy flavone 0.13 ㎎, miillpore filter (0.22 μm) filters and get final product.
Prepared by need testing solution: get dry callicarpa nudiflora medicinal powder and be about 1.0g, accurately weighed, is placed in 100 mL tool plug conical flasks, precision adds 75% methyl alcohol 50mL, close plug, weighed weight, ultrasonic process 30 minutes, let cool, more weighed weight, the weight of less loss is supplied with 75% methyl alcohol, shake up, 0.45 μm of filter membrane filters, and gets subsequent filtrate, to obtain final product.
Draw reference substance solution, each 5 μ L of need testing solution respectively, injection liquid chromatography, measure, to obtain final product.
The method can measure acteoside in callicarpa nudiflora medicinal material, cyanidenon and 5 accurately and effectively, 4 '-dihydroxy-3,7, the content of 3 '-trimethoxy flavone, three kinds of effective constituents, can further improve the quality standard of callicarpa nudiflora medicinal material, guarantee quality and the clinical efficacy of callicarpa nudiflora medicinal material.1. linear relationship is investigated
Precision measures acteoside respectively, cyanidenon and 5,4 '-dihydroxy-3,7,3 '-trimethoxy flavone reference substance mixed solution is that 0.2mL, 0.5mL, 1.0mL, 2.0mL, 5.0mL, 10.0mL are placed in 10 mL volumetric flasks, add 75% methanol dilution to scale, shake up and obtain control series and savor mixed liquor 1., 2., 3., 4., 5., 6..Measure under above-mentioned chromatographic condition, accurate draw 5 μ L sample introductions, measure peak area, with concentration (X, μ g.mL-1) for horizontal ordinate, peak area (Y) carries out linear regression, drawing standard curve for ordinate.Result shows, in this concentration range, 3 constituent concentrations and peak area are good linear relationship.
Table 1 linear relationship test findings
| Composition | Linear equation | Scope (μ g.mL -1） | r |
| Acteoside | Y=51348x-589450 | 29.6～1490.0 | 1.0000 |
| Cyanidenon | Y=387318x-150674 | 1.0～50.0 | 1.0000 |
| 5,4 '-dihydroxy-3,7,3 '-trimethoxy flavone | Y=224565x-167797 | 2.6～130.0 | 1.0000 |
2. precision test
Draw reference substance mixed liquor 4. (acteoside mass concentration is 296 μ g.mL-1, and cyanidenon mass concentration is 10 μ g.mL-1,5,4 '-dihydroxy-3,7,3 '-trimethoxy flavone mass concentration is 26.0 μ g.mL-1) continuous sample introduction 6 times, sample size 5 μ L.The relative standard deviation RSD of result three components relative retention time is respectively 1.48%, 0.66% and 0.46%, is all less than 2.0%.The relative standard deviation RSD of peak area is respectively 0.77%, 1.10% and 1.37%.The results are shown in Table 2
Table 2 Precision test result (n=6)
3. replica test
Get with a collection of fine medicinal material powder, parallelly prepare need testing solution 6 parts, every part of about 1.0 g, accurately weighed, prepare need testing solution by aforementioned need testing solution preparation method, respectively sample introduction, each sample introduction 5 μ L.Calculate, the RSD of result three components is respectively 1.71%, 1.69% and 1.62%.The results are shown in Table 3 ~ 5
Table 3 acteoside replica test result (n=6)
Table 4 cyanidenon replica test result (n=6)
Table 55,4 '-dihydroxy-3,7,3 '-trimethoxy flavone replica test result (n=6)
4. stability test
Get with a collection of fine medicinal material powder, parallelly prepare need testing solution 6 parts, every part of about 1.0g, accurately weighed, prepare need testing solution by aforementioned need testing solution preparation method, measure at each sample introduction of 0h, 2h, 4h, 8h, 12h, 24h respectively, survey 6 times altogether, each sample introduction 5 μ L, investigate stability in its solution, result acteoside, cyanidenon and 5,4 '-dihydroxy-3,7, the RSD of 3 '-trimethoxy flavone is respectively 1.42%, 1.83% and 1.59%.Show that need testing solution is stable in 24h.The results are shown in Table 6
Table 6 stability test result (n=6)
5. average recovery test
Get with criticizing containing acteoside, cyanidenon, 5,4 '-dihydroxy-3,7,3 '-trimethoxy flavone massfraction is respectively 2.5605 ㎎ g-1,0.1727 ㎎ g-1,0.4252 ㎎ g-1 medicinal powder is about 0.5g, 9 parts, 3 parts one group, 3 groups add appropriate reference substance solution respectively, by need testing solution preparation and mensuration.Calculate acteoside, cyanidenon and 5,4 '-dihydroxy-3,7,3 '-trimethoxy flavone average recovery rate be respectively 98.81%, 99.38% and 100.79%, RSD be respectively 1.49%, 1.46% and 1.17%.The results are shown in Table 7 ~ 9
Table 7 acteoside average recovery is tested
Table 8 cyanidenon average recovery is tested
Table 95,4 '-dihydroxy-3,7,3 '-trimethoxy flavone average recovery is tested
6. sample size measures
Get respectively and often criticize callicarpa nudiflora medicinal material sample (see table 10) powder (No. four sieves), about 1.0g, accurately weighed.Prepare need testing solution by aforementioned need testing solution preparation method, adopt acteoside, cyanidenon, 5 in one point external standard method calculation sample, 4 '-dihydroxy-3,7,3 '-trimethoxy flavone content.
Table 10 acteoside, cyanidenon and 5,4 '-dihydroxy-3,7,3 '-trimethoxy flavone
Assay result (㎎/g) (n=3)
Accompanying drawing explanation
Fig. 1 is acteoside, cyanidenon and 5,4 '-dihydroxy-3,7, and 3 '-trimethoxy flavone reference substance HPLC schemes.
Fig. 2 is that callicarpa nudiflora medicinal material sample HPLC schemes.
Fig. 3 is blank solvent HPLC figure.
Embodiment
embodiment 1:
Chromatographic condition and system suitability are: be filling agent with octadecylsilane chemically bonded silica, and mobile phase is methyl alcohol-0.15% phosphate aqueous solution, adopt gradient elution, as follows:
0-5min methyl alcohol-0.15% phosphate aqueous solution 38:62;
5-14min methyl alcohol-0.15% phosphate aqueous solution 45:55;
14-23min methyl alcohol-0.15% phosphate aqueous solution 60:40;
23-30min methyl alcohol-0.15% phosphate aqueous solution 70:30;
30-35min methyl alcohol-0.15% phosphate aqueous solution 75:25,
Determined wavelength 350nm, column temperature 40 DEG C.
Prepared by reference substance solution: get acteoside, cyanidenon and 5,4 '-dihydroxy-3,7,3 '-trimethoxy flavone reference substance is appropriate, accurately weighed, add 75% methyl alcohol dissolving and about make every 1mL respectively respectively containing acteoside 1.48 ㎎, cyanidenon 0.05 ㎎ and 5,4 '-dihydroxy-3,7, the mixing reference substance solution of 3 '-trimethoxy flavone 0.13 ㎎, miillpore filter (0.22 μm) filters and get final product.
Prepared by need testing solution: get dry callicarpa nudiflora medicinal powder and be about 1.0g, accurately weighed, is placed in 100 mL tool plug conical flasks, precision adds 75% methyl alcohol 50mL, close plug, weighed weight, ultrasonic process 30 minutes, let cool, more weighed weight, the weight of less loss is supplied with 75% methyl alcohol, shake up, 0.45 μm of filter membrane filters, and gets subsequent filtrate, to obtain final product.
Determination method: draw reference substance solution, each 5 μ L of need testing solution respectively, injection liquid chromatography, measures, to obtain final product.
Acteoside in callicarpa nudiflora medicinal material, cyanidenon and 5,4 '-dihydroxy-3,7,3 '-trimethoxy flavone content is respectively 2.49 ㎎/g, 0.18 ㎎/g, 0.44 ㎎/g.
embodiment 2:
Chromatographic condition and system suitability are: be filling agent with octadecylsilane chemically bonded silica, and mobile phase is acetonitrile-0.1% acetic acid aqueous solution, adopt gradient elution, as follows:
0-8min acetonitrile-0.1% acetic acid aqueous solution 18:82;
8-26min acetonitrile-0.1% acetic acid aqueous solution 25:75;
26-44min acetonitrile-0.1% acetic acid aqueous solution 35:65;
44-55min acetonitrile-0.1% acetic acid aqueous solution 40:60;
55-60min acetonitrile-0.1% acetic acid aqueous solution 50:50,
Determined wavelength 320nm, column temperature 25 DEG C.
Prepared by reference substance solution: get acteoside, cyanidenon and 5,4 '-dihydroxy-3,7,3 '-trimethoxy flavone reference substance is appropriate, accurately weighed, add 75% methyl alcohol dissolving and about make every 1mL respectively respectively containing acteoside 1.48 ㎎, cyanidenon 0.05 ㎎ and 5,4 '-dihydroxy-3,7, the mixing reference substance solution of 3 '-trimethoxy flavone 0.13 ㎎, miillpore filter (0.22 μm) filters and get final product.
Prepared by need testing solution: get dry callicarpa nudiflora medicinal powder and be about 1.0g, accurately weighed, is placed in 100 mL tool plug conical flasks, precision adds 75% methyl alcohol 50mL, close plug, weighed weight, ultrasonic process 30 minutes, let cool, more weighed weight, the weight of less loss is supplied with 75% methyl alcohol, shake up, 0.45 μm of filter membrane filters, and gets subsequent filtrate, to obtain final product.
Determination method: draw reference substance solution, each 5 μ L of need testing solution respectively, injection liquid chromatography, measures, to obtain final product.
Acteoside in callicarpa nudiflora medicinal material, cyanidenon and 5,4 '-dihydroxy-3,7,3 '-trimethoxy flavone content is respectively 1.12 ㎎/g, 0.11 ㎎/g, 0.27 ㎎/g.
embodiment 3:
Chromatographic condition and system suitability are: be filling agent with octadecylsilane chemically bonded silica, and mobile phase is methyl alcohol-0.15% aqueous formic acid, adopt gradient elution, as follows:
0-5min methyl alcohol-0.15% aqueous formic acid 30:70;
5-15min methyl alcohol-0.15% aqueous formic acid 37:63;
15-25min methyl alcohol-0.15% aqueous formic acid 43:57;
25-35min methyl alcohol-0.15% aqueous formic acid 52:48;
35-45min methyl alcohol-0.15% aqueous formic acid 57:43;
45-55min methyl alcohol-0.15% aqueous formic acid 60:40;
55-60min methyl alcohol-0.15% aqueous formic acid 75:25,
Determined wavelength 340nm, column temperature 35 DEG C.
Prepared by reference substance solution: get acteoside, cyanidenon and 5,4 '-dihydroxy-3,7,3 '-trimethoxy flavone reference substance is appropriate, accurately weighed, add 75% methyl alcohol dissolving and about make every 1mL respectively respectively containing acteoside 1.48 ㎎, cyanidenon 0.05 ㎎ and 5,4 '-dihydroxy-3,7, the mixing reference substance solution of 3 '-trimethoxy flavone 0.13 ㎎, miillpore filter (0.22 μm) filters and get final product.
Prepared by need testing solution: get dry callicarpa nudiflora medicinal powder and be about 1.0g, accurately weighed, is placed in 100 mL tool plug conical flasks, precision adds 75% methyl alcohol 50mL, close plug, weighed weight, ultrasonic process 30 minutes, let cool, more weighed weight, the weight of less loss is supplied with 75% methyl alcohol, shake up, 0.45 μm of filter membrane filters, and gets subsequent filtrate, to obtain final product.
Determination method: draw reference substance solution, each 5 μ L of need testing solution respectively, injection liquid chromatography, measures, to obtain final product.
Acteoside in callicarpa nudiflora medicinal material, cyanidenon and 5,4 '-dihydroxy-3,7,3 '-trimethoxy flavone content is respectively 0.68 ㎎/g, 0.09 ㎎/g, 0.30 ㎎/g.
embodiment 4:
Chromatographic condition and system suitability are: be filling agent with octadecylsilane chemically bonded silica, and mobile phase is methyl alcohol-0.3% phosphate aqueous solution, adopt gradient elution, as follows:
0-20min methyl alcohol-0.3% phosphate aqueous solution 38:62;
20-30min methyl alcohol-0.3% phosphate aqueous solution 45:55;
30-40min methyl alcohol-0.3% phosphate aqueous solution 48:52;
40-48min methyl alcohol-0.3% phosphate aqueous solution 55:45;
48-55min methyl alcohol-0.3% phosphate aqueous solution 60:40;
55-60min methyl alcohol-0.3% phosphate aqueous solution 75:25,
Determined wavelength 360nm, column temperature 40 DEG C.
Prepared by reference substance solution: get acteoside, cyanidenon and 5,4 '-dihydroxy-3,7,3 '-trimethoxy flavone reference substance is appropriate, accurately weighed, add 75% methyl alcohol dissolving and about make every 1mL respectively respectively containing acteoside 1.48 ㎎, cyanidenon 0.05 ㎎ and 5,4 '-dihydroxy-3,7, the mixing reference substance solution of 3 '-trimethoxy flavone 0.13 ㎎, miillpore filter (0.22 μm) filters and get final product.
Prepared by need testing solution: get dry callicarpa nudiflora medicinal powder and be about 1.0g, accurately weighed, is placed in 100 mL tool plug conical flasks, precision adds 75% methyl alcohol 50mL, close plug, weighed weight, ultrasonic process 30 minutes, let cool, more weighed weight, the weight of less loss is supplied with 75% methyl alcohol, shake up, 0.45 μm of filter membrane filters, and gets subsequent filtrate, to obtain final product.
Determination method: draw reference substance solution, each 5 μ L of need testing solution respectively, injection liquid chromatography, measures, to obtain final product.
Acteoside in callicarpa nudiflora medicinal material, cyanidenon and 5,4 '-dihydroxy-3,7,3 '-trimethoxy flavone content is respectively 1.67 ㎎/g, 0.20 ㎎/g, 0.35 ㎎/g.
Claims (4)
1. acteoside, cyanidenon, 5 in callicarpa nudiflora medicinal material, 4 '-dihydroxy-3,7, the assay method of 3 '-trimethoxy flavone, three kinds of active constituent contents, adopt high performance liquid chromatography, it is characterized in that: chromatographic condition and system suitability are: be filling agent with octadecylsilane chemically bonded silica, mobile phase is organic solvent-acid solution, adopt gradient elution, as follows:
0-10min organic solvent ratio is 10% ~ 50%;
10-20min organic solvent ratio is 20% ~ 60%;
20-30min organic solvent ratio is 25% ~ 70%;
30-40min organic solvent ratio is 30% ~ 80%;
40-50min organic solvent ratio is 35% ~ 80%;
50-60min organic solvent ratio is 40% ~ 80%,
Acid solution concentration is 0-0.3%, determined wavelength 320-360nm, column temperature 25 DEG C-40 DEG C.
2. assay method as claimed in claim 1, wherein in mobile phase, organic solvent is methyl alcohol or acetonitrile, and acid solution is phosphoric acid or acetic acid or formic acid.
3. assay method as claimed in claim 1, wherein acid solution concentration is 0.15%.
4. assay method as claimed in claim 1, its chromatographic condition and system suitability are preferably following condition: be filling agent with octadecylsilane chemically bonded silica, and mobile phase is methyl alcohol-0.15% phosphate aqueous solution, employing gradient elution, as follows:
0-5min methyl alcohol-0.15% phosphate aqueous solution 38:62;
5-14min methyl alcohol-0.15% phosphate aqueous solution 45:55;
14-23min methyl alcohol-0.15% phosphate aqueous solution 60:40;
23-30min methyl alcohol-0.15% phosphate aqueous solution 70:30;
30-35min methyl alcohol-0.15% phosphate aqueous solution 75:25,
Determined wavelength 350nm, column temperature 40 DEG C.
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| CN109596767A (en) * | 2017-09-30 | 2019-04-09 | 海南九芝堂药业有限公司 | A kind of detection method of callicarpa nudiflora preparation |
| CN110568113A (en) * | 2019-07-19 | 2019-12-13 | 江西普正制药股份有限公司 | Active characteristic fingerprint chromatogram of callicarpa nudiflora and rapid identification method thereof |
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| CN110568113A (en) * | 2019-07-19 | 2019-12-13 | 江西普正制药股份有限公司 | Active characteristic fingerprint chromatogram of callicarpa nudiflora and rapid identification method thereof |
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