CN102379934A - High efficiency liquid chromatography detection method for content of raddeanin A in rhizoma anemones raddeanae - Google Patents
High efficiency liquid chromatography detection method for content of raddeanin A in rhizoma anemones raddeanae Download PDFInfo
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- CN102379934A CN102379934A CN2010102750926A CN201010275092A CN102379934A CN 102379934 A CN102379934 A CN 102379934A CN 2010102750926 A CN2010102750926 A CN 2010102750926A CN 201010275092 A CN201010275092 A CN 201010275092A CN 102379934 A CN102379934 A CN 102379934A
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Abstract
The invention relates to a high efficiency liquid chromatography detection method for the content of raddeanin A in rhizoma anemones raddeanae, belonging to a detection method of rhizoma anemones raddeanae. In the method, an evaporative light-scattering detector is adopted, an external standard two-point method is used for quantifying, octadecylsilane bonded silica is taken as a filler, a mixed solution of methanol or acetonitrile and water is taken as a flowing phase, and the flow speed of the flowing phase is 0.2-1 ml per minute; and a methanol ultrasonic treatment method is adopted for sample pretreatment. The method has the advantages of high sensitivity, stability, high reproducibility and capability of effectively controlling the qualities of the rhizoma anemones raddeanae and a preparation thereof.
Description
Invention field
The present invention relates to the biapiculate detection method of Chinese medicine, particularly the detection method of content of Chinese medicine Rhizoma Anemones Raddeanae and preparation thereof.
Background technology
Rhizoma Anemones Raddeanae has another name called Radde Anemone Rhizome, is the dry rhizome of cohosh anemone raddeana Regel Anemone raddeanaRegel for Rhizoma Anemones Raddeanae.Mainly be distributed in ground such as three provinces in the northeast of China and Shandong, Hebei, Shanxi, maximum with Jilin Province's output.Medical material is excavated many summers, removes residual stem and fibrous root, dries.This medicine head is stated from safe show " Bencao Pinhui Jingyao " of the Liu Wen of the Ming Dynasty.Effect with " expelling wind and removing dampness, subduing inflammation ".As far back as the Qing Dynasty, " deciding cancer looses " of Wang Xugao is once with Rhizoma Anemones Raddeanae treatment breast carcinoma.The present clinical anemofrigid-damp arthralgia that is used for, contracture of the limbs, arthralgia, ulcer sore pain.Many and other medicines compatibility, folk prescription is not used as medicine, and is the primary raw material of famous Chinese patent medicine " HUOLUO DAN " and " restorative bolus ".These article are rich in triterpene saponin, and wherein the triterpenoid saponin anemonin A is one of main effective ingredient of antineoplastic.
About the anemonin A detection method in the Rhizoma Anemones Raddeanae medical material, be in the prior art and adopt HPLC to use UV-detector detection carrying out assay, owing to be saponin component; On ultra-violet absorption spectrum, have only end absorption, ultraviolet wavelength is chosen as about 206nm as measuring wavelength usually; Therefore the chromatographic peak response value is low, poor sensitivity, and mobile phase and impurity disturb more serious; Thereby make the entire method repeatability bad, it is very big to measure resultant error.Under Rhizoma Anemones Raddeanae item of version Chinese Pharmacopoeia in 2010; The sample treatment that adopts methanol Suo Shi extraction, ether defatting, water-saturated n-butanol to extract repeatedly; And be aided with acetonitrile and 0.1% phosphoric acid solution gradient elution mode is the chromatographic condition of mobile phase; Just be accomplished the content that HPLC-UV-detector detects anemonin A, about 10～15 hours of sample treatment time is because the test sample processing method is loaded down with trivial details; Be prone to cause measuring resultant error, the mobile phase of gradient elution mode very easily makes chromatographic peak separate unstability of base line again.And adopt above-mentioned existing method to Rhizoma Anemones Raddeanae medical material anemonin A assay in the patent medicine, almost can't carry out.
Summary of the invention
The present invention provides Raddeanin A content high-efficiency liquid chromatography method for detecting in a kind of Chinese medicine Rhizoma Anemones Raddeanae; To solve the low problem of complicated operation, poor reproducibility, sensitivity that exists in the prior art, this method is applicable to the quality control of Rhizoma Anemones Raddeanae medical material, Rhizoma Anemones Raddeanae preparation.The technical scheme that the present invention takes is: adopt evaporative light scattering detector; Quantitative with the external standard two-point method; The employing octadecylsilane chemically bonded silica is a filler, and as mobile phase, the flow velocity of mobile phase is per minute 0.2～1ml with the mixed liquor of methanol or acetonitrile and water; Methanol supersound process method is adopted in sample pretreatment.
The inventive method may further comprise the steps:
1, chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler; Mobile phase is 80～93: 20～7 acetonitrile-water or 82～95: 18～5 methanol-water; Evaporative light scattering detector detects; The flow velocity of mobile phase is per minute 0.2～1ml; The drift tube temperature that evaporative light scattering detector detects: 60～130 ℃, air velocity: 1.0～3.1L/min.
2, the preparation of reference substance solution: it is an amount of that precision takes by weighing the Raddeanin A reference substance, adds methanol and process the solution that every 1ml contains 0.4mg, promptly gets;
3, the preparation of need testing solution: get Radde Anemone 2～8g, put in the tool plug conical flask, the accurate methanol 50ml that adds, close plug is claimed decide weight, and supersound process 0.5～1 hour is put coldly, claims to decide weight again, adds methanol and supplies the weight that subtracts mistake, shakes up filtration; Measure subsequent filtrate 10ml, water bath method, residue add methanol makes dissolving, is transferred to the 10ml measuring bottle and is diluted to scale, shakes up, and the microporous filter membrane filtration with 0.45 μ m promptly gets;
4, algoscopy: accurate reference substance solution 5 μ l, the 15 μ l of drawing, need testing solution 10 μ l inject chromatograph of liquid, measure, and calculate with the two points external standard method logarithmic equation, promptly get;
Beneficial effect: the present invention adopts HPLC-evaporative light scattering detection method to measure the content of Raddeanin A in the Chinese medicine Rhizoma Anemones Raddeanae, and it is very simple that operational approach is compared existing method.The methodology checking shows, this method good separation, and methodological studies such as method linearity, stability, repeatability, average recovery all meet the requirement of quantitative assay.Can more effectively control the product quality of Chinese medicine Rhizoma Anemones Raddeanae and preparation thereof.About 0.5 hour of sample treatment time, improved detection efficiency greatly, reduced environmental pollution, practiced thrift the detection cost, method is easy, quick, accurate.
The present invention also is fit to comprise clinical or pharmaceutically acceptable common formulations such as tablet, granule with the preparation of Rhizoma Anemones Raddeanae as one of crude drug or crude drug.
Description of drawings
Fig. 1 is that reference substance Raddeanin A evaporative light scattering detector detects collection of illustrative plates;
Fig. 2 is that Rhizoma Anemones Raddeanae medical material evaporative light scattering detector detects collection of illustrative plates;
Fig. 3 is that the QIANLIETONG PIAN evaporative light scattering detector detects collection of illustrative plates.
The specific embodiment
Instrument: day island proper Tianjin LC-10Atvp high performance liquid chromatograph, Zhejiang University's 2010 dual pathways chromatographic work stations; The U.S.'s safe ELSD2000ES evaporative light scattering detector difficult to understand; The prunus mume (sieb.) sieb.et zucc. Teller. holder benefit AB265-S electronic balance.
Reagent: the Raddeanin A chemical reference substance, assay usefulness, Nat'l Pharmaceutical & Biological Products Control Institute, purity meets the specification requirement of assay with chemical reference substance on inspection, and content is >=98%; Methanol: chromatographically pure, water: self-control distilled water;
Sample: Chinese medicine Rhizoma Anemones Raddeanae medical material.QIANLIETONG PIAN, lot number: 20100225 (Guangzhou Zhongyi Medicine Industry Co., Ltd)
Embodiment 1
(1), chromatographic condition and system suitability test: think filler; Mobile phase: acetonitrile-water 80: 20; Evaporative light scattering detector detects; Flow velocity: 0.2ml/min; The drift tube temperature that evaporative light scattering detector detects: 60 ℃, air velocity: 1.0L/min.
(2), the preparation of reference substance solution: it is an amount of that precision takes by weighing the Raddeanin A reference substance, adds methanol and process the solution that every 1ml contains 0.4mg, promptly gets;
(3), the preparation of need testing solution: get Radde Anemone 2g, put in the tool plug conical flask, the accurate methanol 50ml that adds, close plug is claimed decide weight, supersound process 0.5 hour is put coldly, claims to decide weight again, adds methanol and supplies the weight that subtracts mistake, shakes up filtration; Measure subsequent filtrate 10ml, water bath method, residue add methanol makes dissolving, is transferred to the 10ml measuring bottle and is diluted to scale, shakes up, and the microporous filter membrane filtration with 0.45 μ m promptly gets;
(4), algoscopy: precision is drawn reference substance solution 5 μ l, 15 μ l, and need testing solution 10 μ l inject chromatograph of liquid, measure, and calculate with the two points external standard method logarithmic equation, promptly get;
Embodiment 2
(1), chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler; Mobile phase: acetonitrile-water 86: 14; Evaporative light scattering detector detects; Flow velocity: 0.6ml/min; The drift tube temperature that evaporative light scattering detector detects: 90 ℃, air velocity: 2.0L/min.
(2), the preparation of reference substance solution: it is an amount of that precision takes by weighing the Raddeanin A reference substance, adds methanol and process the solution that every 1ml contains 0.4mg, promptly gets;
(3), the preparation of need testing solution: get Radde Anemone 5g, put in the tool plug conical flask, the accurate methanol 50ml that adds, close plug is claimed decide weight, supersound process 0.8 hour is put coldly, claims to decide weight again, adds methanol and supplies the weight that subtracts mistake, shakes up filtration; Measure subsequent filtrate 10ml, water bath method, residue add methanol makes dissolving, is transferred to the 10ml measuring bottle and is diluted to scale, shakes up, and the microporous filter membrane filtration with 0.45 μ m promptly gets;
(4), algoscopy: precision is drawn reference substance solution 5 μ l, 15 μ l, and need testing solution 10 μ l inject chromatograph of liquid, measure, and calculate with the two points external standard method logarithmic equation, promptly get;
Embodiment 3
(1), chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler; Mobile phase: acetonitrile-water 93: 7; Evaporative light scattering detector detects; Flow velocity: 1ml/min; The drift tube temperature that evaporative light scattering detector detects: 130 ℃, air velocity: 3.1L/min.
(2), the preparation of reference substance solution: it is an amount of that precision takes by weighing the Raddeanin A reference substance, adds methanol and process the solution that every 1ml contains 0.4mg, promptly gets;
(3), the preparation of need testing solution: get Radde Anemone 8g, put in the tool plug conical flask, the accurate methanol 50ml that adds, close plug is claimed decide weight, supersound process 1 hour is put coldly, claims to decide weight again, adds methanol and supplies the weight that subtracts mistake, shakes up filtration; Measure subsequent filtrate 10ml, water bath method, residue add methanol makes dissolving, is transferred to the 10ml measuring bottle and is diluted to scale, shakes up, and the microporous filter membrane filtration with 0.45 μ m promptly gets;
(4), algoscopy: precision is drawn reference substance solution 5 μ l, 15 μ l, and need testing solution 10 μ l inject chromatograph of liquid, measure, and calculate with the two points external standard method logarithmic equation, promptly get;
Embodiment 4
(1), chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler; Mobile phase: methanol-water 82: 18; Evaporative light scattering detector detects; Flow velocity: 0.2ml/min; The drift tube temperature that evaporative light scattering detector detects: 60 ℃, air velocity: 1.0L/min.
(2), the preparation of reference substance solution: it is an amount of that precision takes by weighing the Raddeanin A reference substance, adds methanol and process the solution that every 1ml contains 0.4mg, promptly gets;
(3), the preparation of need testing solution: get Radde Anemone 2g, put in the tool plug conical flask, the accurate methanol 50ml that adds, close plug is claimed decide weight, supersound process 0.5 hour is put coldly, claims to decide weight again, adds methanol and supplies the weight that subtracts mistake, shakes up filtration; Measure subsequent filtrate 10ml, water bath method, residue add methanol makes dissolving, is transferred to the 10ml measuring bottle and is diluted to scale, shakes up, and the microporous filter membrane filtration with 0.45 μ m promptly gets;
(4), algoscopy: precision is drawn reference substance solution 5 μ l, 15 μ l, and need testing solution 10 μ l inject chromatograph of liquid, measure, and calculate with the two points external standard method logarithmic equation, promptly get;
(1), chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler; Mobile phase: methanol-water 95: 5; Evaporative light scattering detector detects; Flow velocity: 1ml/min; The drift tube temperature that evaporative light scattering detector detects: 130 ℃, air velocity: 3.1L/min.
(2), the preparation of reference substance solution: it is an amount of that precision takes by weighing the Raddeanin A reference substance, adds methanol and process the solution that every 1ml contains 0.4mg, promptly gets;
(3), the preparation of need testing solution: get Radde Anemone 8g, put in the tool plug conical flask, the accurate methanol 50ml that adds, close plug is claimed decide weight, supersound process 1 hour is put coldly, claims to decide weight again, adds methanol and supplies the weight that subtracts mistake, shakes up filtration; Measure subsequent filtrate 10ml, water bath method, residue add methanol makes dissolving, is transferred to the 10ml measuring bottle and is diluted to scale, shakes up, and the microporous filter membrane filtration with 0.45 μ m promptly gets;
(4), algoscopy: precision is drawn reference substance solution 5 μ l, 15 μ l, and need testing solution 10 μ l inject chromatograph of liquid, measure, and calculate with the two points external standard method logarithmic equation, promptly get;
(1), chromatographic condition and system suitability test: chromatographic column: octadecylsilane chemically bonded silica chromatographic column Diamonsil C
18, 250 * 4.6mm; 5 μ; Mobile phase: methanol-water 85: 15; Flow velocity: 0.8ml/min; The drift tube temperature that evaporative light scattering detector detects: 80 ℃, air velocity: 2.0L/min; Column temperature: room temperature.
(2), that the preparation precision of reference substance solution takes by weighing the Raddeanin A reference substance is an amount of, adds methanol and processes the solution that every 1ml contains 0.42mg, promptly get.
(3), the preparation of need testing solution gets Chinese medicine Radde Anemone 5g, crosses sieve No. three, accurately claims surely, puts in the tool plug conical flask the accurate methanol 50ml that adds; Close plug is claimed to decide weight, and supersound process 30 minutes is put cold; Claim again to decide weight, add methanol and supply the weight that subtracts mistake, shake up, filter; Measure subsequent filtrate 10ml, water bath method, residue add methanol makes dissolving, is transferred to the 10ml measuring bottle and is diluted to scale, shakes up, and the microporous filter membrane filtration with 0.45 μ m promptly gets;
(4), algoscopy: accurate respectively each 5 μ l of absorption reference substance solution, 15 μ l, need testing solution 10 μ l inject chromatograph of liquid.
Raddeanin A and other component reach baseline separation under this condition, separating degree R＞1.5, and theoretical cam curve is pressed Raddeanin A and is calculated greater than 6000, and the Raddeanin A retention time is about 14 minutes.
Different mobile phase ratio and different mobile phase flow velocitys such as methanol-water and acetonitrile-water have been investigated; 20～7) or methanol-water (82～95: 18～5) mobile phase is acetonitrile-water (80～93: as a result; Flow velocity is per 1 minute 0.2ml to 1ml, and Raddeanin A all can separate; With mobile phase be acetonitrile-water (80～93: 20～7) or methanol-water (82～95: 18～5), flow velocity is per 1 minute 0.2ml to 0.8ml, and effect is more excellent.
Linear relationship is investigated: it is an amount of that precision takes by weighing the Raddeanin A reference substance, adds methanol and process the solution that contains Raddeanin A 0.42mg among every 1ml, as reference substance solution.Accurate respectively 4,8,12,16, the 20 μ l that draw; Injecting high performance liquid chromatograph, measure by above-mentioned condition, is vertical coordinate with the natural logrithm of peak area; The natural logrithm of Raddeanin A sample size is an abscissa; Linear regression must regression equation be: LnA=60243LnC+1.531, r=0.9993.Available external standard two-point method logarithmic equation is measured and is calculated.
The precision test: get same reference substance solution, continuous sample introduction 5 times, the record peak area calculates precision.
Stability test: accurate draw same need testing solution, at regular intervals sample introduction once, comparative measurements result's stability.
Repeatability test: get same lot number sample, carry out 5 parallel tests (being n=5), calculate relative standard deviation (RSD%), relatively repeatability.
Recovery test: the application of sample absorption method is adopted in this test, and precision takes by weighing 5 parts in the sample of known content, accurately respectively adds a certain amount of Raddeanin A reference substance, measures by determination, calculates the response rate of Raddeanin A.
The result: experimental result shows that the detection of Raddeanin A is limited to 10ng, and the range of linearity of Raddeanin A is 1.68～8.4 μ g; Precision is 0.23%; Raddeanin A is stable in 12 hours, and RSD is 1.21%; This assay method has good repeatability, and RSD is 1.02%; The average recovery of Raddeanin A is 99.01%, and RSD is 1.55%; Raddeanin A content is 0.34% in the Chinese medicine Rhizoma Anemones Raddeanae medical material through measuring.
Embodiment 7: the QIANLIETONG PIAN assay
(1), chromatographic condition and system suitability test: chromatographic column: octadecylsilane chemically bonded silica chromatographic column Diamonsil C
18, 250 * 4.6mm; 5 μ; Mobile phase: methanol-water 85: 15, the flow velocity of mobile phase: 0.8ml/min; The drift tube temperature that evaporative light scattering detector detects: 80 ℃, air velocity: 2.0L/min; Column temperature: room temperature.
(2), that the preparation precision of reference substance solution takes by weighing the Raddeanin A reference substance is an amount of, adds methanol and processes the solution that every 1ml contains 0.42mg, promptly get.
(3), the preparation of need testing solution, get QIANLIETONG PIAN, porphyrize, mixing is got about 6g, accurate claim fixed; Put in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, supersound process 0.5 hour; Put coldly, claim again decide weight, add methanol and supply the weight that subtracts mistake, shake up filtration; Measure subsequent filtrate 10ml, water bath method, residue add methanol makes dissolving, is transferred to the 10ml measuring bottle and is diluted to scale, shakes up, and the microporous filter membrane filtration with 0.45 μ m promptly gets.
The preparation negative sample solution of negative sample solution is to take by weighing all the other adjuvants except that the Chinese medicine Rhizoma Anemones Raddeanae in the prescription ratio; Process Chinese medicine Rhizoma Anemones Raddeanae negative sample by method for making, get this negative sample again and do not contain the biapiculate negative sample solution of Chinese medicine by the preparation of above-mentioned " preparation of need testing solution " method.
(4), algoscopy: accurate respectively absorption reference substance solution 5 μ l, 15 μ l, need testing solution reach and do not contain the biapiculate negative sample solution 10 μ l of Chinese medicine, inject chromatograph of liquid.Raddeanin A and other component reach baseline separation under this condition; Separating degree R＞1.5, theoretical cam curve are pressed Raddeanin A and are calculated greater than 6000, and the Raddeanin A retention time is about 14 minutes; Negative sample solution chromatograph does not have absworption peak in the relevant position, and is visible negative noiseless.
Testing result: Raddeanin A content is the 2.92mg/ sheet in the QIANLIETONG PIAN through measuring.
Claims (3)
1. the method that the HPLC of Raddeanin A content detects in the Chinese medicine Rhizoma Anemones Raddeanae; It is characterized in that adopting evaporative light scattering detector; Quantitative with the external standard two-point method; The employing octadecylsilane chemically bonded silica is a filler, and as mobile phase, the flow velocity of mobile phase is per minute 0.2～1ml with the mixed liquor of methanol or acetonitrile and water; Methanol supersound process method is adopted in sample pretreatment.
2. the method that the HPLC of Raddeanin A content detects in the Chinese medicine Rhizoma Anemones Raddeanae as claimed in claim 1 is characterized in that mobile phase is 80～93: 20～7 acetonitrile-water or 82～95: 18～5 methanol-water.
3. the method that the HPLC of Raddeanin A content detects in the Chinese medicine Rhizoma Anemones Raddeanae as claimed in claim 1, the flow velocity that it is characterized in that mobile phase is per minute 0.2～1ml; The drift tube temperature that evaporative light scattering detector detects: 60～130 ℃, air velocity: 1.0～3.1L/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105616552A (en) * | 2014-11-28 | 2016-06-01 | 天津耀宇生物技术有限公司 | Preparation method and application of Rhizoma Anemones Raddeanae extract |
| CN109738545A (en) * | 2019-02-20 | 2019-05-10 | 江西医学高等专科学校 | Wine processs the processing procedure optimization method of medicinal material pointed at both ends |
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Non-Patent Citations (2)
| Title |
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| 刘大有: "两头尖地上部分化学成分及其含量测定分析", 《长春中医学院学报》 * |
| 李顺意: "高效液相色谱-质谱-质谱法快速鉴定中药竹节香附的皂苷", 《湖北大学学报(自然科学版)》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105616552A (en) * | 2014-11-28 | 2016-06-01 | 天津耀宇生物技术有限公司 | Preparation method and application of Rhizoma Anemones Raddeanae extract |
| CN105616552B (en) * | 2014-11-28 | 2019-10-15 | 天津耀宇生物技术有限公司 | The preparation method and applications of Radde anemone rhizome extract |
| CN109738545A (en) * | 2019-02-20 | 2019-05-10 | 江西医学高等专科学校 | Wine processs the processing procedure optimization method of medicinal material pointed at both ends |
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