CN100360931C - Quality control method for red sage root and notoginseng preparation - Google Patents
Quality control method for red sage root and notoginseng preparation Download PDFInfo
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Abstract
The present invention relates to a method for identifying the compound HPLC-DAD fingerprint of red sage root and notoginseng, which belongs to the field of the quality control of natural medicines, particularly to the field of finger prints. The present invention can be used as one of the indexes for controlling the quality of compound preparations containing the medicinal materials of danshen root and notoginseng, such as danqi tablets, compound danshen tablets, compound danshen dripping pills, etc.
Description
Technical field:
The present invention relates to the field of quality control of natural drug, be specially the finger-print field, be specifically related to the HPLC-DAD finger print atlas identifying method of the red sage root and notoginseng.It can be used as one of index of the compound preparation quality control that contains the red sage root and pseudo-ginseng.
Background technology:
The preparation that contains the red sage root and pseudo-ginseng also is called as compound red sage root preparation usually, is widely used in the treatment angiocardiopathy clinically.Common have Fufang Danshen Pian, compound danshen dripping pills, DANQI PIAN, a GUANXIN DANSHEN PIAN etc.
The red sage root and pseudo-ginseng are the main medicines of forming of two of compound red sage root preparation, and wherein the red sage root is the dry root of labiate red sage root Salvia miltiorrhiza Bge., the tool stasis-dispelling and pain-killing, activating blood to promote menstruation, the effect of the relieving restlessness that clears away heart-fire is used for irregular menstruation, through closing dysmenorrhoea lumps in the chest and abdomen, chest ventral spine pain, hot numbness pain, sore swells and ache, dysphoria and insomnia, hepatosplenomegaly, angina pectoris; Pseudo-ginseng is the dry root of panax araliaceae plant Panax notoginseng (Burk.) F.H.Chen, the diffusing stasis of blood hemostasis of tool, the effect of detumescence ding-tong.Be used for spitting of blood, spit blood bleeding from five sense organs or subcutaneous tissue, traumatism and bleeding, diseases such as tumbling and swelling.
Modern study shows that the active component of the red sage root is mainly the fat-soluble and salvianolic acid aqueous soluble active constituent of diterpene quinones, and root of red-rooted salvia phenolic acid constituents tool suppresses platelet aggregation, and antithrombotic forms, effects such as anti-oxidant and protection heart microvascular endothelial cell; Liposoluble constituents such as tanshinone energy coronary artery dilator improves coronary blood flow, protection cardiac muscle and broad-spectrum antibacterial effect.The notoginsenoside constituents is the main active of pseudo-ginseng, and the tool antithrombotic forms, effects such as hemangiectasis and protection cardiac muscle.
At present about the red sage root and notoginseng preparation finger study of identification method report, mostly be the evaluation of the red sage root or pseudo-ginseng single medicinal material greatly, as red rooted salvia ethanol extract efficient liquid-phase chromatograph finger print atlas research (Chinese Pharmaceutical Journal the 39th the 8th phase of volume of August in 2004), pseudo-ginseng finger-print research (Strait PharmaceuticalJournal Vol 14 No52002).Prior art fails to identify multiclass active component in the red sage root and the pseudo-ginseng two flavor medicines simultaneously with finger-print.
Summary of the invention:
The objective of the invention is to set up a kind of finger-print of multiclass active component in the red sage root and pseudo-ginseng two flavor medicines of can identifying simultaneously in the red sage root and the notoginseng.
Another object of the present invention is to finger-print of the present invention is used to contain the quality control of the compound preparation of the red sage root and pseudo-ginseng.
The present invention is achieved in that
We have simulated the prescription (hereinafter referred to as red seven sides) of DANQI PIAN, and by to red seven side's test liquid preparation methods, chromatographic condition is selected and the chromatographic condition methodological study, has determined pellet seven side HPLC-DAD finger-prints.This finger-print detects and analyzes when can satisfy the multiclass active component of the red sage root and pseudo-ginseng among red seven sides.We further are used to this finger-print to contain the compound preparation quality control of the red sage root and pseudo-ginseng again.
Concrete scheme of the present invention is as follows:
Use high performance liquid chromatograph, the DAD detecting device, chromatographic work station, with the red sage root and notoginseng solution, adopt following chromatographic condition:
Chromatographic column: carbon octadecyl silane filler chromatographic column and pre-column;
Column temperature: 25-35 ℃;
Moving phase: A is the phosphoric acid water of 0.1-0.5%; B is an acetonitrile; A+B=100% adopts gradient elution: 0-10min, 7-17%B, 10-12min, 17-20%B, 12-16min, 20-21%B, 16-32min, 21%B, 32-40min, 21-29%B, 40-55min, 29-35%B, 55-65min, 35-70%B, 65-75min, 70-80%B, 75-80min, 80-97%B, 80-82min, 97-100%B, 82-85min, 100%B; Perhaps gradient is after 55 minutes: 55-65min, 35-65%B, 65-80min, 65-80%B, 80-85min, 80-100%B;
Flow velocity: 1ml/min, in the time of 22～28 minutes, flow velocity is 0.8ml/min;
Detect wavelength 203,281nm.
Preferred column temperature is 30 ℃.
The concentration of preferred phosphoric acid water is 0.1%, is percent by volume.
The preparation method of need testing solution is: get the red sage root and the pseudo-ginseng of pulverizing, add the 85-95% alcohol immersion, the water-bath refluxing extraction is put coldly, filters; Dregs of a decoction boiling is put coldly, filters, and merging filtrate is concentrated near doing, and adds the 50-90% dissolve with methanol, constant volume.
Preferred manufacturing procedure is: get the red sage root and the pseudo-ginseng of the same umber of pulverizing, add 90% alcohol immersion of 6-12 times of parts by weight, the water-bath refluxing extraction is put coldly, filters; The dregs of a decoction add poach, amount of water be medicinal material weight 10-30 doubly, put coldly, filter, merging filtrate is evaporated near doing in 50 ℃, adds 70% dissolve with methanol, constant volume.
The preferred 10 μ l of above-mentioned liquid chromatograph sample size.
Finger print atlas identifying method of the present invention, got final product at 85 minutes writing time, is used to identify DANQI PIAN, and be to get final product in 55-65 minute writing time during compound danshen dripping pills.
Be part test of the present invention below:
1. the preparation of need testing solution: the red sage root and the pseudo-ginseng of getting pulverizing are an amount of, add 90% ethanol, soak, and water-bath refluxing extraction 2h is put coldly, filters; The dregs of a decoction add suitable quantity of water and continue to decoct 2h, filter, merging filtrate, decompression recycling ethanol is settled to scale to doing, adding 70% dissolve with methanol and be transferred to volumetric flask, filtering with microporous membrane, need testing solution (0.024g crude drug/ml).Sample introduction 10 μ l carry out stratographic analysis.
2.HPLC chromatographiccondition:
Chromatographic column: carbon octadecyl silane filler chromatographic column (4.6 * 250mm ID, 5 μ m) and pre-column (4.6 * 12.5mmID, 5 μ m); Column temperature: 30 ℃; Moving phase, A is 0.1% phosphoric acid water; B is an acetonitrile; A+B=100% adopts gradient elution: 0-10min, 7-17%B, 10-12min, 17-20%B, 12-16min, 20-21%B, 16-32min, 21%B, 32-40min, 21-29%B, 40-55min, 29-35%B, 55-65min, 35-70%B, 65-75min, 70-80%B, 75-80min, 80-97%B, 80-82min, 97-100%B, 82-85min, 100%B; Perhaps gradient is after 55 minutes: 55-65min, 35-65%B, 65-80min, 65-80%B, 80-85min, 80-100%B.Flow velocity: 1ml/min (22-28min, 0.8ml/min); Detect wavelength 203,281nm.Writing time 85min.
The selection of 3 chromatographic conditions and result
3.1 the selection of elution system and result
This experiment is selected 3 kinds of flow phase system: (1) acetonitrile-water gradient elution; (2) acetonitrile-0.1%-0.5% phosphoric acid gradient elution; (3) acetonitrile-0.1% formic acid gradient elution.
The result shows that acetonitrile-0.1%-0.5% phosphoric acid gradient elution absorption peak number is many, and peak shape is good, and baseline is steady, is better than acetonitrile-0.1% formic acid, the acetonitrile-water gradient elution system.Acetonitrile-0.1%-0.5% phosphoric acid gradient elution effect is suitable, and 0.1% phosphoric acid concentration is lower, and is little to the loss of chromatographic column, thus more excellent be acetonitrile-0.1% phosphoric acid gradient elution.
3.2 gradient, column temperature, and the selection and the result of flow velocity
To 5 gradient, column temperature (25-35 ℃) and flow velocity are investigated.The result determines:
Gradient: 0-10min, 7-17%B, 10-12min, 17-20%B, 12-16min, 20-21%B, 16-32min, 21%B, 32-40min, 21-29%B, 40-55min, 29-35%B, 55-65min, 35-70%B, 65-75min, 70-80%B, 75-80min, 80-97%B, 80-82min, 97-100%B, 82-85min, (mobile phase A is 0.1% phosphoric acid water to 100%B; B is an acetonitrile; A+B=100%).Perhaps gradient is after 55 minutes: 55-65min, 35-65%B, 65-80min, 65-80%B, 80-85min, 80-100%B.Preferred column temperature: 30 ℃
3.3 detection wavelength determination
The principal ingredient of pseudo-ginseng is the notoginsenoside class in red seven side's extracts; The principal ingredient of the red sage root is the water-soluble and red sage root quinones liposoluble constituent of salvianolic acid.According to the characteristic ultraviolet absorption of these compositions, be provided with 203,254,270,281 and five wavelength of 286nm chromatographic condition is investigated, the result shows that the notoginsenoside constituents only goes out the peak at the low wavelength place of 203nm; Red sage root chemical constitution all has different the absorption at each wavelength, 281nm than 254,270 and 286nm can better take into account salvia-soluble and liposoluble constituent.Take all factors into consideration, select 203nm and two wavelength of 281nm.
3.4 the method and the result of red seven side's need testing solutions preparation
This test is optimized red seven sides' technology, is intended to make red seven side's test liquids can reflect its effective constituent comprehensively, reduces the interference of impurity such as carbohydrate, tannin simultaneously.
Test liquid 1: get the red sage root 0.6g of pulverizing, pseudo-ginseng 0.6g adds 30ml water logging bubble 1h, decocts 2h, puts coldly, filters, and filtrate is evaporated near doing in 50 ℃, adds 70% dissolve with methanol and is transferred to 50ml volumetric flask constant volume.
Test liquid 2: the red sage root 0.6g that gets pulverizing, pseudo-ginseng 0.6g adds 30ml water logging bubble 1h, decocts 2h, put cold, filter, filtrate is evaporated to 2ml in 50 ℃, adds 3 times of amount 95% ethanol alcohol precipitations, refrigerator left standstill liquid, filter, filtrate is evaporated near dried in 50 ℃, add 70% dissolve with methanol and be transferred to 50ml volumetric flask constant volume.
Test liquid 3: get the red sage root 0.6g of pulverizing, pseudo-ginseng 0.6g adds 90% ethanol 10ml and soaks 1h, and water-bath refluxing extraction 2h is put coldly, filters, and filtrate is evaporated near doing in 50 ℃, adds 70% dissolve with methanol and is transferred to 50ml volumetric flask constant volume.
Test liquid 4: the red sage root 0.6g that gets pulverizing, pseudo-ginseng 0.6g, add 70% ethanol 10ml and soak 1h, water-bath refluxing extraction 2h is put coldly, filters, the dregs of a decoction continue with 70% alcohol extract 1 time, merging filtrate, filtrate is evaporated near dried in 50 ℃, add 70% dissolve with methanol and be transferred to 50ml volumetric flask constant volume.
Test liquid 5: get the red sage root 0.6g of pulverizing, pseudo-ginseng 0.6g adds 90% ethanol 10ml and soaks 1h, and water-bath refluxing extraction 2h is put coldly, filters; The dregs of a decoction add 50% ethanol 10ml to be continued to extract 1 time, merging filtrate, and filtrate is evaporated near dried in 50 ℃, add 70% dissolve with methanol and be transferred to 50ml volumetric flask constant volume.
Test liquid 6: get the red sage root 0.6g of pulverizing, pseudo-ginseng 0.6g adds 90% ethanol 10ml and soaks 1h, and water-bath refluxing extraction 2h is put coldly, filters; The dregs of a decoction add water 30ml and decoct 2h, put coldly, filter, and filtrate is evaporated to 2ml in 50 ℃, add 3 times of amount 95% ethanol alcohol precipitations, refrigerator left standstill liquid, filtered, filtrate merges with 90% alcohol extract filtrate, is evaporated to closely in 50 ℃ and does, and adds 70% dissolve with methanol and is transferred to 50ml volumetric flask constant volume.
Test liquid 7: get the red sage root 0.6g of pulverizing, pseudo-ginseng 0.6g adds 90% ethanol 10ml and soaks 1h, and water-bath refluxing extraction 2h is put coldly, filters; The dregs of a decoction add water 30ml and decoct 2h, put coldly, filter, and merging filtrate is evaporated near doing in 50 ℃, adds 50% dissolve with methanol and is transferred to 50ml volumetric flask constant volume.
Test liquid 8: get the red sage root 0.6g of pulverizing, pseudo-ginseng 0.6g adds 90% ethanol 10ml and soaks 1h, and water-bath refluxing extraction 2h is put coldly, filters; The dregs of a decoction add water 30ml and decoct 2h, put coldly, filter, and merging filtrate is evaporated near doing in 50 ℃, adds 60% dissolve with methanol and is transferred to 50ml volumetric flask constant volume.
Test liquid 9: get the red sage root 0.6g of pulverizing, pseudo-ginseng 0.6g adds 90% ethanol 10ml and soaks 1h, and water-bath refluxing extraction 2h is put coldly, filters; The dregs of a decoction add water 30ml and decoct 2h, put coldly, filter, and merging filtrate is evaporated near doing in 50 ℃, adds 70% dissolve with methanol and is transferred to 50ml volumetric flask constant volume.
Red each need testing solution of seven sides of preparation, liquid chromatograph auto injection 10 μ l carry out stratographic analysis.The result shows: simple water is carried, and 70% ethanol and 90% alcohol extract all can not well be taken into account the water-soluble and liposoluble constituent of red seven sides; 90% ethanol extracts to combine with water and combines effective than 90% ethanol with 50% alcohol extract, but water is put forward part and through alcohol precipitation protocatechualdehyde is slightly lost, so can be without alcohol precipitation: sample with 70% dissolve with methanol than taking into account water-soluble and liposoluble constituent with 50% and 60% dissolve with methanol.To sum up, choose the preparation technology of optimum test liquid 9.
3.5 the methodological study of detection method
3.5.1 need testing solution stability and instrument precision experiment
Be equipped with red seven side's need testing solutions by " 1 " below legal system, detected finger-print respectively at 0,2,4,12,18,24 hour and (see Fig. 1-1,1-2), investigate the stability of red seven side's need testing solutions and the precision of high performance liquid chromatograph.The result shows that red seven side's test liquids are stable in 24 hours, and the precision of high performance liquid chromatograph also meets the requirements.
3.5.2 the repeated experiment that need testing solution is measured
Get with a collection of red sage root and pseudo-ginseng meal (40 order), by 3 parts of pellets of the parallel preparation of method, seven side's test solutions under " 1 " item, detecting the HPLC finger-print (sees Fig. 2-1,2-2), investigates the stability of red seven sides' extracting method and fingerprint atlas detection method and repeated.The result shows that red seven side's test liquid preparation methods are reliable and stable, has good reappearance.
3.5.3 determining of writing time
2 hour record figures and the blank figure of red seven side's test liquids under " 2 " chromatographic condition (sees Fig. 3-1,3-2), investigates the best titime time.The result shows, the composition in the later on basic n.s. of 80min, thereby definite best titime time be 85min.
3.5.4 standard control experiment:
Adopting protocatechualdehyde, tanshin polyphenolic acid B, Cryptotanshinone, tanshinone IIA, notoginsenoside R, ginsenoside Rg1, ginsenoside Rb1 is object of reference, and accurate title is fixed an amount of, uses 70% dissolve with methanol, makes standard solution, record chromatogram (see figure 4).Conclusion:
By to red seven side's test liquid preparation methods, chromatographic condition is selected and the chromatographic condition methodological study, and definite existing red seven side's chromatographicconditions detect and analysis when can satisfy the multiclass active component of the red sage root and pseudo-ginseng among red seven sides.
We are further used for this finger-print condition to contain the quality control of the compound preparation of the red sage root and pseudo-ginseng.Specific as follows:
1. the test liquid of compound red sage root preparation preparation:
It is an amount of to get DANQI PIAN (desaccharification clothing), Fufang Danshen Pian and compound danshen dripping pills (removal film-coating), and pulverize is with 70% dissolve with methanol and transfer to constant volume in the volumetric flask.Ultrasonic Extraction is put coldly, adds 70% methyl alcohol and supplies weight.Solution is crossed 0.45 μ m filter membrane, promptly.
2. with finger-print condition of the present invention the test liquid of compound red sage root preparation is carried out the HPLC-DAD stratographic analysis, promptly get the compound red sage root preparation finger-print.
Description of drawings
Fig. 1-1 need testing solution stability and instrument precision experiment chromatogram (203nm), wherein chromatogram WDQ00135～WDQ00140 is respectively 0～24 hour chromatogram
Fig. 1-2 need testing solution stability and instrument precision experiment chromatogram (281nm), wherein chromatogram WDQ00135～WDQ00140 is respectively 0～24 hour chromatogram
The repeated experiment chromatogram (203nm) that Fig. 2-1 need testing solution is measured
The repeated experiment chromatogram (281nm) that Fig. 2-2 need testing solution is measured
(203nm: wherein WDQ00120 is blank to the chromatogram that Fig. 3-1 tests writing time; WDQ00121 is a test sample)
(281nm: wherein WDQ00120 is blank to the chromatogram that Fig. 3-2 tests writing time; WDQ00121 is a test sample)
The chromatogram of Fig. 4 standard control test
Fig. 5 is the pellet seven side's finger-prints among the embodiment 1
Fig. 6 is the finger-print of commercially available DANQI PIAN among the embodiment 2
Fig. 7 is that commercially available lot number is the finger-print of 040602 Fufang Danshen Pian among the embodiment 3
Fig. 8 is that commercially available lot number is the finger-print of 050308 Fufang Danshen Pian among the embodiment 3
Fig. 9 is that commercially available lot number is the finger-print of 03121024 Fufang Danshen Pian among the embodiment 3
Figure 10 is that lot number is the finger-print of 20020921 compound danshen dripping pills among the embodiment 4
Figure 11 is that lot number is the finger-print of 20030604 compound danshen dripping pills among the embodiment 4
Figure 12 is that lot number is the finger-print of 20040303 compound danshen dripping pills among the embodiment 4
Figure 13 is the finger-print of red seven sides among the embodiment 5.
Figure 14 is the finger-print of DANQI PIAN among the embodiment 5.
Figure 15 is the finger-print of Fufang Danshen Pian among the embodiment 5.
Figure 16 is the finger-print of compound danshen dripping pills among the embodiment 5.
Figure 17 is the finger-print of DANQI PIAN among the embodiment 6.
Figure 18 is the finger-print of compound danshen dripping pills among the embodiment 6.
Each numeral is in the above accompanying drawing: 1. protocatechualdehyde 2. notoginsenoside Rs 3. ginsenoside Rg1s 4. tanshin polyphenolic acid Bs 5. ginsenoside Rb1s 6. Cryptotanshinones 7. tanshinone IIAs
Embodiment:
Embodiment 1
1 experiment material
1.1 instrument and equipment:
Agilent 1100 type series of high efficiency liquid chromatographs comprise G1312A quaternary gradient pump, G1313A automatic sampler, G1316A column oven, G1315A DAD detecting device, HP Chemstation chromatographic work station (U.S. Hui Pu company); Rotating thin film evaporimeter (Switzerland B ü chi company).
1.2 reagent and reagent:
Medicinal material: the red sage root (sky, Shaanxi scholar's power plant pharmaceutcal corporation, Ltd, Shanglou, Shaanxi) is accredited as the dry root of labiate red sage root Salvia miltiorrhiza Bge. through professor Li Ping; Pseudo-ginseng (Yunnan mountain of papers) is accredited as the dry root of panax araliaceae plant Panax notoginseng (Burk.) F.H.Chen through professor Li Ping.
2. experimental technique
2.1 chromatographic condition
Chromatographic column: C18 chromatographic column (ZORBAX ODS 4.6 * 250mm ID, 5 μ m) and C18 pre-column (4.6 * 12.5mmID, 5 μ m); Column temperature: 30 ℃; Moving phase, A is 0.1% phosphoric acid water; B is an acetonitrile; A+B=100% adopts gradient elution: 0-10min, 7-17%B, 10-12min, 17-20%B, 12-16min, 20-21%B, 16-32min, 21%B, 32-40min, 21-29%B, 40-55min, 29-35%B, 55-65min, 35-70%B, 65-75min, 70-80%B, 75-80min, 80-97%B, 80-82min, 97-100%B, 82-85min, 100%B; Flow velocity: 1ml/min (22-28min, 0.8ml/min); Detect wavelength 203,281nm.Writing time 85min.
2.2 the preparation of need testing solution
Get the red sage root 1.2g of pulverizing, pseudo-ginseng 1.2g adds 90% ethanol 25ml, soaks 1h, and water-bath refluxing extraction 2h is put coldly, filters; The dregs of a decoction add the continuation of 40ml water and decoct 2h, filter, and merging filtrate is settled to scale in 50 ℃ of decompression recycling ethanols to doing, adding 70% dissolve with methanol and be transferred to the 100ml volumetric flask, and filtering with microporous membrane gets need testing solution.
3. experimental result: 10 μ l carry out stratographic analysis with the need testing solution sample introduction, promptly get red seven side's finger-prints, and be 85min writing time.See Fig. 5.
Embodiment 2
Get commercially available DANQI PIAN (the Hunan Pharmaceutical Co that stablizes the country, lot number: 040803) 20, desaccharification clothing and grind into powder, precision takes by weighing 0.5g, puts in the brown volumetric flask of 25ml 70% methanol constant volume.Ultrasonic Extraction 30min is put coldly, adds 70% methyl alcohol and supplies weight.Solution is crossed 0.45 μ m filter membrane.Other condition is with embodiment 1.Sample introduction 10 μ l carry out stratographic analysis, get DANQI PIAN HPLC-DAD finger-print, see Fig. 6.
Get commercially available Fufang Danshen Pian (White Cloud Mountain, Guangdong pharmaceutical factory, lot number: 03121024; Nanjing Pharmaceutical Co of Tongrentang, lot number: 040602: Hu Qingyu Pharmaceutical Workshop, Zhejiang Pharmaceutical Co, lot number: 050308) 20, grind to form powder, precision takes by weighing 0.5g, puts in the brown volumetric flask of 25ml 70% methanol constant volume.Ultrasonic Extraction 30min is put coldly, adds 70% methyl alcohol and supplies weight.Solution is crossed 0.45 μ m filter membrane.Other condition is with embodiment 1.Sample introduction 10 μ l carry out stratographic analysis, get 3 the Fufang Danshen Pian HPLC-DAD of producer finger-prints, see Fig. 7-9.
Embodiment 4
Get commercially available compound danshen dripping pills (sky, Tianjin Shi Li Pharmaceutical Co, lot number: 20020921,20030604,20040303) 75, accurate claim surely, be ground into powder, remove film-coating, with 70% dissolve with methanol and transfer to constant volume in the brown volumetric flask of 25ml.Ultrasonic Extraction 30min is put coldly, adds 70% methyl alcohol and supplies weight.Solution is crossed 0.45 μ m filter membrane.Other condition is with embodiment 1.Sample introduction 10 μ l carry out stratographic analysis, get the HPLC-DAD finger-print of 3 lot number compound danshen dripping pillses.See Figure 10-12.
With the same method of the foregoing description, be after changing gradient into 55 minutes: 55-65min, 35-65%B, 65-80min, 65-80%B, 80-85min, 80-100%B.Respectively to red seven sides, 03121024) and compound danshen dripping pills (sky, Tianjin Shi Li Pharmaceutical Co, lot number: 20020921) carry out stratographic analysis, must see Figure 13-16 by finger-print DANQI PIAN, Fufang Danshen Pian (White Cloud Mountain, Guangdong pharmaceutical factory, lot number:.
With the method for embodiment 1,2,4, just change 60 minutes into writing time, respectively to DANQI PIAN and compound danshen dripping pills (sky, Tianjin Shi Li Pharmaceutical Co, lot number: 20020921) carry out stratographic analysis.Get finger-print and see Figure 17-18.
To sum up, the HPLC-DAD finger-print of the red sage root that the present invention set up and notoginseng can be used for detecting simultaneously in the red sage root saponin component in diterpene quinones liposoluble constituent such as phenolic acids water soluble ingredient such as tanshin polyphenolic acid B and tanshinone IIA and the pseudo-ginseng, method is reliable, stable, can be used for containing the quality control of the compound preparation of the red sage root and pseudo-ginseng.
Claims (7)
1, the finger print atlas identifying method of the red sage root and notoginseng preparation: comprise the standard of foundation finger-print, with same procedure measure the finger-print of testing sample, with the finger-print and the standard finger-print contrast of product to be tested, its feature adopts following method acquisition finger-print:
Use high performance liquid chromatograph, the DAD detecting device, chromatographic work station, with the red sage root and notoginseng solution, adopt following chromatographic condition:
Chromatographic column: carbon octadecyl silane filler chromatographic column and pre-column;
Column temperature: 25-35 ℃;
Moving phase: A is the phosphoric acid water of 0.1-0.5%; B is an acetonitrile; A+B=100% adopts gradient elution: 0-10min, 7-17%B, 10-12min, 17-20%B, 12-16min, 20-21%B, 16-32min, 21%B, 32-40min, 21-29%B, 40-55min, 29-35%B, 55-65min, 35-70%B, 65-75min, 70-80%B, 75-80min, 80-97%B, 80-82min, 97-100%B, 82-85min, 100%B; Perhaps gradient is after 55 minutes: 55-65min, 35-65%B, 65-80min, 65-80%B, 80-85min, 80-100%B;
Flow velocity: 1ml/min, in the time of 22～28 minutes, flow velocity is 0.8ml/min;
Detect wavelength: 203,281nm.
2, the finger print atlas identifying method of claim 1, wherein column temperature is 30 ℃.
3, the finger print atlas identifying method of claim 1, wherein the concentration of phosphoric acid water is 0.1%.
4, the finger print atlas identifying method of claim 1, wherein the preparation method of standard diagram need testing solution is: get the red sage root and the pseudo-ginseng of pulverizing, add the 85-95% alcohol immersion, the water-bath refluxing extraction is put coldly, filters; Dregs of a decoction boiling is put coldly, filters, and merging filtrate is concentrated near doing, and adds the 50-90% dissolve with methanol, constant volume.
5, the finger print atlas identifying method of claim 4, wherein the preparation method of standard diagram need testing solution is: get the red sage root and the pseudo-ginseng of the same umber of pulverizing, add 6-12 times of parts by weight 90% alcohol immersion, the water-bath refluxing extraction is put coldly, filters; The dregs of a decoction add poach, amount of water be dregs of a decoction weight 10-30 doubly, put coldly, filter, merging filtrate is evaporated near doing in 50 ℃, adds 70% dissolve with methanol, constant volume.
6, the finger print atlas identifying method of claim 1, wherein the preparation method of testing sample is: with testing sample preparation desaccharification clothing or removal film-coating, pulverize, with 70% dissolve with methanol and constant volume, ultrasonic Extraction, put cold, add 70% methyl alcohol and supply weight, filter, promptly.
7, the finger print atlas identifying method of claim 1, liquid chromatograph sample size are 10 μ l.
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| CN108333282A (en) * | 2018-04-24 | 2018-07-27 | 山东农业大学 | A kind of method of a variety of phenolic acid class and tanshinone component in Rapid Simultaneous Determination Fufang Danshen Pian |
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| CN1669573A (en) * | 2004-03-17 | 2005-09-21 | 天津天士力制药股份有限公司 | Chinese medicine preparation for treating cardiovascular and cerebrovascular diseases and preparing process thereof |
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