CN1806819A - 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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- CN1806819A CN1806819A CN 200510095180 CN200510095180A CN1806819A CN 1806819 A CN1806819 A CN 1806819A CN 200510095180 CN200510095180 CN 200510095180 CN 200510095180 A CN200510095180 A CN 200510095180A CN 1806819 A CN1806819 A CN 1806819A
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Abstract
The invention relates to a HPLC-DAD fingerprint pattern identification method for the compound of salvia miltiorrhizae and pseudo-ginseng, which can be applied as one of the quality control indexes for compound preparations containing salvia miltiorrhizae and pseudo-ginseng medicinal materials such as Danqi tablet, compound salvia miltiorrhizae tablet and compound salvia miltiorrhizae drop pill.
Description
Technical field:
The present invention relates to the field of quality control of natural drug, be specially the finger printing field, be specifically related to the HPLC-DAD finger print atlas identifying method of Radix Salviae Miltiorrhizae and notoginseng.It can be used as one of index of the compound preparation quality control that contains Radix Salviae Miltiorrhizae and pseudo-ginseng.
Background technology:
The preparation that contains Radix Salviae Miltiorrhizae and Radix Notoginseng also is called as compound red sage root preparation usually, is widely used in the treatment cardiovascular disease clinically.Common have FUFANG DANSHEN PIAN, FUFANG DANSHEN DIWAN, DANQI PIAN, a GUANXIN DANSHEN PIAN etc.
Radix Salviae Miltiorrhizae and Radix Notoginseng are the main medicines of forming of two of compound red sage root preparation, and wherein Radix Salviae Miltiorrhizae is the dry root of labiate Radix Salviae Miltiorrhizae Salvia miltiorrhiza Bge., the tool stasis-dispelling and pain-killing, promoting blood circulation to restore menstrual flow, the effect of the relieving restlessness that clears away heart-fire is used for menoxenia, amenorrhea dysmenorrhea lumps in the chest and abdomen, breast ventral spine pain, pyretic arthralgia pain, skin infection swells and ache, dysphoria and insomnia, hepatosplenomegaly, angina pectoris; Radix Notoginseng is the dry root of panax araliaceae plant Panax notoginseng (Burk.) F.H.Chen, the hemostasis of tool dissipating blood stasis, the effect of subduing swelling and relieving pain.Be used for spitting of blood, spit blood epistaxis, traumatic hemorrhage, diseases such as tumbling and swelling.
Modern study shows that the active component of Radix Salviae Miltiorrhizae is mainly the fat-soluble and salvianolic acid aqueous soluble active constituent of diterpene quinones, salvianolic acid constituents tool anticoagulant, and antithrombotic forms, effects such as antioxidation and protection heart microvascular endothelial cell; Liposoluble constituents such as TANSHINONES energy coronary artery dilator improves coronary blood flow, protection cardiac muscle and broad-spectrum antibacterial effect.The arasaponin constituents is the main active of Radix Notoginseng, and the tool antithrombotic forms, effects such as blood vessel dilating and protection cardiac muscle.
At present about Radix Salviae Miltiorrhizae and notoginseng preparation finger study of identification method report, mostly be the evaluation of Radix Salviae Miltiorrhizae or Radix Notoginseng single medical material greatly, as red rooted salvia ethanol extraction efficient liquid-phase chromatograph finger print atlas research (Chinese Pharmaceutical Journal the 39th the 8th phase of volume of August in 2004), Radix Notoginseng finger printing research (Strait Pharmaceutical Journal Vol14 No52002).Prior art fails to identify multiclass active component in Radix Salviae Miltiorrhizae and the Radix Notoginseng two flavor medicines simultaneously with finger printing.
Summary of the invention:
The objective of the invention is to set up a kind of finger printing of multiclass active component in the Radix Salviae Miltiorrhizae and Radix Notoginseng two flavor medicines of can identifying simultaneously in Radix Salviae Miltiorrhizae and the notoginseng.
Another object of the present invention is to finger printing of the present invention is used to contain the quality control of the compound preparation of Radix Salviae Miltiorrhizae 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 methoies, chromatographic condition is selected and the chromatographic condition methodological study, has determined pellet seven side HPLC-DAD finger printing.This finger printing detects and analyzes when can satisfy the multiclass active component of Radix Salviae Miltiorrhizae and Radix Notoginseng among red seven sides.We further are used to this finger printing to contain the compound preparation quality control of Radix Salviae Miltiorrhizae and pseudo-ginseng again.
Concrete scheme of the present invention is as follows:
Use high performance liquid chromatograph, the DAD detector, chromatographic work station, with Radix Salviae Miltiorrhizae and notoginseng solution, adopt following chromatographic condition:
Chromatographic column: carbon octadecyl silane filler chromatographic column and pre-column;
Column temperature: 25-35 ℃;
Mobile 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 Radix Salviae Miltiorrhizae and the Radix Notoginseng of pulverizing, add the 85-95% soak with ethanol, the water-bath reflux, extract, is put coldly, filters; Medicinal residues decoct with water, and put coldly, filter, and merging filtrate is concentrated near doing, and adds the 50-90% dissolve with methanol, standardize solution.
Preferred manufacturing procedure is: get the Radix Salviae Miltiorrhizae and the Radix Notoginseng of the same umber of pulverizing, add 90% soak with ethanol of 6-12 times of parts by weight, the water-bath reflux, extract, is put coldly, filters; Medicinal residues add decocting in water, amount of water be medical material weight 10-30 doubly, put coldly, filter, merging filtrate is evaporated near doing in 50 ℃, adds 70% dissolve with methanol, standardize solution.
The preferred 10 μ l of above-mentioned chromatograph of liquid 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 FUFANG DANSHEN DIWAN.
Be part test of the present invention below:
1. the preparation of need testing solution: the Radix Salviae Miltiorrhizae and the Radix Notoginseng of getting pulverizing are an amount of, add 90% ethanol, soak, and water-bath reflux, extract, 2h is put coldly, filters; Medicinal residues 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 chromatography.
2.HPLC chromatographiccondition:
Chromatographic column: carbon octadecyl silane filler chromatographic column (4.6 * 250mm ID, 5 μ m) and pre-column (4.6 * 12.5mm ID, 5 μ m); Column temperature: 30 ℃; Mobile 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 absworption 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 main component of Radix Notoginseng is the arasaponin class in red seven side's extracting solution; The main component of Radix Salviae Miltiorrhizae is salvianolic acid water solublity and Radix Salviae Miltiorrhizae quinones liposoluble constituent.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 arasaponin constituents only goes out the peak at the low wavelength place of 203nm; The Radix Salviae Miltiorrhizae chemical constituent 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 ingredient comprehensively, reduces the interference of impurity such as saccharide, tannin simultaneously.
Test liquid 1: get the Radix Salviae Miltiorrhizae 0.6g of pulverizing, Radix Notoginseng 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 standardize solution.
Test liquid 2: the Radix Salviae Miltiorrhizae 0.6g that gets pulverizing, Radix Notoginseng 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 precipitate with ethanol, refrigerator left standstill liquid, filter, filtrate is evaporated near dried in 50 ℃, add 70% dissolve with methanol and be transferred to 50ml volumetric flask standardize solution.
Test liquid 3: get the Radix Salviae Miltiorrhizae 0.6g of pulverizing, Radix Notoginseng 0.6g adds 90% ethanol 10ml and soaks 1h, and water-bath reflux, extract, 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 standardize solution.
Test liquid 4: the Radix Salviae Miltiorrhizae 0.6g that gets pulverizing, Radix Notoginseng 0.6g, add 70% ethanol 10ml and soak 1h, water-bath reflux, extract, 2h is put coldly, filters, medicinal residues continue with 70% ethanol extraction 1 time, merging filtrate, filtrate is evaporated near dried in 50 ℃, add 70% dissolve with methanol and be transferred to 50ml volumetric flask standardize solution.
Test liquid 5: get the Radix Salviae Miltiorrhizae 0.6g of pulverizing, Radix Notoginseng 0.6g adds 90% ethanol 10ml and soaks 1h, and water-bath reflux, extract, 2h is put coldly, filters; Medicinal residues 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 standardize solution.
Test liquid 6: get the Radix Salviae Miltiorrhizae 0.6g of pulverizing, Radix Notoginseng 0.6g adds 90% ethanol 10ml and soaks 1h, and water-bath reflux, extract, 2h is put coldly, filters; Medicinal residues add water 30ml and decoct 2h, put coldly, filter, and filtrate is evaporated to 2ml in 50 ℃, add 3 times of amount 95% ethanol precipitate with ethanol, refrigerator left standstill liquid, filtered, filtrate merges with 90% ethanol extraction filtrate, is evaporated to closely in 50 ℃ and does, and adds 70% dissolve with methanol and is transferred to 50ml volumetric flask standardize solution.
Test liquid 7: get the Radix Salviae Miltiorrhizae 0.6g of pulverizing, Radix Notoginseng 0.6g adds 90% ethanol 10ml and soaks 1h, and water-bath reflux, extract, 2h is put coldly, filters; Medicinal residues 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 standardize solution.
Test liquid 8: get the Radix Salviae Miltiorrhizae 0.6g of pulverizing, Radix Notoginseng 0.6g adds 90% ethanol 10ml and soaks 1h, and water-bath reflux, extract, 2h is put coldly, filters; Medicinal residues 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 standardize solution.
Test liquid 9: get the Radix Salviae Miltiorrhizae 0.6g of pulverizing, Radix Notoginseng 0.6g adds 90% ethanol 10ml and soaks 1h, and water-bath reflux, extract, 2h is put coldly, filters; Medicinal residues 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 standardize solution.
Red each need testing solution of seven sides of preparation, chromatograph of liquid auto injection 10 μ l carry out chromatography.The result shows: simple water is carried, and 70% ethanol and 90% ethanol extraction all can not well be taken into account red seven side's water solublity and liposoluble constituents; 90% ethanol combines with water extraction and combines effectively than 90% ethanol with 50% ethanol extraction, but water puies forward part and through precipitate with ethanol protocatechualdehyde is slightly lost, so can be without precipitate with ethanol; Sample with 70% dissolve with methanol than taking into account water solublity 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 printing 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 Radix Salviae Miltiorrhizae and pseudo-ginseng coarse powder (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 printing (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 methoies are reliable and stable, has good repeatability.
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, salvianolic acid B, cryptotanshinone, tanshinone, arasaponin R1, 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 methoies, 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 Radix Salviae Miltiorrhizae and Radix Notoginseng among red seven sides.
We are further used for this finger printing condition to contain the quality control of the compound preparation of Radix Salviae Miltiorrhizae 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 (desaccharide clothing), FUFANG DANSHEN PIAN and FUFANG DANSHEN DIWAN (removal film-coat), and pulverize is with 70% dissolve with methanol and transfer to standardize solution in the volumetric flask.Supersound extraction is put coldly, adds 70% methanol and supplies weight.Solution is crossed 0.45 μ m filter membrane, promptly.
2. with finger printing condition of the present invention the test liquid of compound red sage root preparation is carried out the HPLC-DAD chromatography, promptly get the compound red sage root preparation finger printing.
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 printing among the embodiment 1
Fig. 6 is the finger printing of commercially available DANQI PIAN among the embodiment 2
Fig. 7 is that commercially available lot number is the finger printing of 040602 FUFANG DANSHEN PIAN among the embodiment 3
Fig. 8 is that commercially available lot number is the finger printing of 050308 FUFANG DANSHEN PIAN among the embodiment 3
Fig. 9 is that commercially available lot number is the finger printing of 03121024 FUFANG DANSHEN PIAN among the embodiment 3
Figure 10 is that lot number is the finger printing of 20020921 FUFANG DANSHEN DIWAN among the embodiment 4
Figure 11 is that lot number is the finger printing of 20030604 FUFANG DANSHEN DIWAN among the embodiment 4
Figure 12 is that lot number is the finger printing of 20040303 FUFANG DANSHEN DIWAN among the embodiment 4
Figure 13 is the finger printing of red seven sides among the embodiment 5.
Figure 14 is the finger printing of DANQI PIAN among the embodiment 5.
Figure 15 is the finger printing of FUFANG DANSHEN PIAN among the embodiment 5.
Figure 16 is the finger printing of FUFANG DANSHEN DIWAN among the embodiment 5.
Figure 17 is the finger printing of DANQI PIAN among the embodiment 6.
Figure 18 is the finger printing of FUFANG DANSHEN DIWAN among the embodiment 6.
Each numeral is in the above accompanying drawing: 1. protocatechualdehyde 2. arasaponin R1s 3. ginsenoside Rg1s 4. salvianolic acid Bs 5. ginsenoside Rb1s 6. cryptotanshinones 7. tanshinones
The specific embodiment:
1 experiment material
1.1 instrument and equipment:
Agilent 1100 type series of high efficiency chromatograph of liquid comprise G1312A quaternary gradient pump, G1313A automatic sampler, G1316A column oven, G1315A DAD detector, HP Chemstation chromatographic work station (U.S. Hui Pu company); Rotating thin film evaporimeter (Switzerland B ü chi company).
1.2 reagent and reagent:
Medical material: Radix Salviae Miltiorrhizae (sky, Shaanxi scholar's power plant pharmaceutcal corporation, Ltd, Shanglou, Shaanxi) is accredited as the dry root of labiate Radix Salviae Miltiorrhizae Salvia miltiorrhiza Bge. through professor Li Ping; Radix Notoginseng (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 ℃; Mobile 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 Radix Salviae Miltiorrhizae 1.2g of pulverizing, Radix Notoginseng 1.2g adds 90% ethanol 25ml, soaks 1h, and water-bath reflux, extract, 2h is put coldly, filters; Medicinal residues 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 chromatography with the need testing solution sample introduction, promptly get red seven side's finger printing, and be 85min writing time.See Fig. 5.
Get commercially available DANQI PIAN (the Hunan Pharmaceutical Co that stablizes the country, lot number: 040803) 20, desaccharide clothing and grind into powder, precision takes by weighing 0.5g, puts in the brown volumetric flask of 25ml 70% methanol constant volume.Supersound extraction 30min is put coldly, adds 70% methanol 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 chromatography, get DANQI PIAN HPLC-DAD finger printing, 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.Supersound extraction 30min is put coldly, adds 70% methanol 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 chromatography, get 3 the FUFANG DANSHEN PIAN HPLC-DAD of producer finger printing, see Fig. 7-9.
Get commercially available FUFANG DANSHEN DIWAN (sky, Tianjin Shi Li Pharmaceutical Co, lot number: 20020921,20030604,20040303) 75, accurate claim surely, be ground into powder, remove film-coat, with 70% dissolve with methanol and transfer to standardize solution in the brown volumetric flask of 25ml.Supersound extraction 30min is put coldly, adds 70% methanol 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 chromatography, get the HPLC-DAD finger printing of 3 lot number FUFANG DANSHEN DIWAN.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 FUFANG DANSHEN DIWAN (sky, Tianjin Shi Li Pharmaceutical Co, lot number: 20020921) carry out chromatography, must see Figure 13-16 by finger printing DANQI PIAN, FUFANG DANSHEN PIAN (White Cloud Mountain, Guangdong pharmaceutical factory, lot number:.
Embodiment 6
With the method for embodiment 1,2,4, just change 60 minutes into writing time, respectively to DANQI PIAN and FUFANG DANSHEN DIWAN (sky, Tianjin Shi Li Pharmaceutical Co, lot number: 20020921) carry out chromatography.Get finger printing and see Figure 17-18.
To sum up, the HPLC-DAD finger printing of Radix Salviae Miltiorrhizae that the present invention set up and notoginseng can be used for detecting simultaneously in the Radix Salviae Miltiorrhizae saponin component in diterpene quinones liposoluble constituent such as phenolic acids water soluble ingredient such as salvianolic acid B and tanshinone and the Radix Notoginseng, method is reliable, stable, can be used for containing the quality control of the compound preparation of Radix Salviae Miltiorrhizae and Radix Notoginseng.
Claims (7)
1, the finger print atlas identifying method of Radix Salviae Miltiorrhizae and notoginseng preparation: comprise the standard of foundation finger printing, with same procedure measure the finger printing of testing sample, with the finger printing and the standard finger-print contrast of product to be tested, its feature adopts following method acquisition finger printing:
Use high performance liquid chromatograph, the DAD detector, chromatographic work station, with Radix Salviae Miltiorrhizae and notoginseng solution, adopt following chromatographic condition:
Chromatographic column: carbon octadecyl silane filler chromatographic column and pre-column;
Column temperature: 25-35 ℃;
Mobile 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 Radix Salviae Miltiorrhizae and the Radix Notoginseng of pulverizing, add the 85-95% soak with ethanol, the water-bath reflux, extract, is put coldly, filters; Medicinal residues decoct with water, and put coldly, filter, and merging filtrate is concentrated near doing, and adds the 50-90% dissolve with methanol, standardize solution.
5, the finger print atlas identifying method of claim 4, the wherein preparation method of sample: get the Radix Salviae Miltiorrhizae and the Radix Notoginseng of the same umber of pulverizing, add 6-12 times of parts by weight 90% soak with ethanol, the water-bath reflux, extract, is put coldly, filters; Medicinal residues add decocting in water, amount of water be medicinal residues weight 10-30 doubly, put coldly, filter, merging filtrate is evaporated near doing in 50 ℃, adds 70% dissolve with methanol, standardize solution.
6, the finger print atlas identifying method of claim 1, wherein the preparation method of testing sample is: with testing sample preparation desaccharide clothing or removal film-coat, pulverize, with 70% dissolve with methanol and standardize solution, supersound extraction, put cold, add 70% methanol and supply weight, filter, promptly.
7, the finger print atlas identifying method of claim 1, chromatograph of liquid sample size are 10 μ l.
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| CNB2005100951807A CN100360931C (en) | 2005-11-02 | 2005-11-02 | Quality control method for red sage root and notoginseng preparation |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101912440A (en) * | 2010-08-06 | 2010-12-15 | 广州白云山和记黄埔中药有限公司 | Quality control method of complex salvia tablet and application thereof |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100450501C (en) * | 2004-03-17 | 2009-01-14 | 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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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101912440A (en) * | 2010-08-06 | 2010-12-15 | 广州白云山和记黄埔中药有限公司 | Quality control method of complex salvia tablet and application thereof |
| CN101912440B (en) * | 2010-08-06 | 2012-12-12 | 广州白云山和记黄埔中药有限公司 | Quality control method of complex salvia tablet and application thereof |
| 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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