CN1772041A - Quality detection method for compound prepn of red sage and notoginseng - Google Patents
Quality detection method for compound prepn of red sage and notoginseng Download PDFInfo
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Abstract
The present invention relates to Chinese medicine quality detecting technology, and is especially the quality detection method for compound preparation of red sage and notoginseng. HPLC-DAD process is adopted to measure the contents of protocatechuic aldehyde, salvianolic acid B, cryptotanshinone, neotanshinone IIA, arasaponin R1, ginsenoside Rg1 and ginsenoside Rb1 in compound red sage preparation simultaneously. The process is simple, precise, repeatable and reliable, and may be used in the quality control of compound red sage preparation.
Description
Technical field:
The present invention relates to the Chinese medicine quality detection range, relate in particular to a kind of quality determining method that contains the compound preparation of 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.Modern study shows that the active component of Radix Salviae Miltiorrhizae is mainly fat-soluble and salvianolic acid (as salvianolic acid B etc.) aqueous soluble active constituent of diterpene quinones (as tanshinone etc.), salvianolic acid constituents tool anticoagulant, 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.Arasaponin class (as arasaponin R1, ginsenoside Rg1 and ginsenoside Rb1) composition is the main active of Radix Notoginseng, and the tool antithrombotic forms, effects such as blood vessel dilating and protection cardiac muscle.
The quality standard of relevant compound red sage root preparation is not quite similar, and DANQI PIAN and coronary disease Radix Salviae Miltiorrhizae Tabellae do not have the assay index, and the assay index of FUFANG DANSHEN PIAN is tanshinone and salvianolic acid B, and FUFANG DANSHEN DIWAN is a danshensu.As seen the big and imperfection of the quality standard difference of compound red sage root preparation, FUFANG DANSHEN PIAN quality standard improve but also just fat-soluble the and water soluble ingredient of Radix Salviae Miltiorrhizae are carried out Quality Control respectively.Do not have as yet in the quality standard of compound red sage root preparation the wherein content control of pseudo-ginseng activity composition.The detection method of relevant bibliographical information has: the HPLC method is measured 3 kinds of liposoluble constituent content (Beijing University of Chinese Medicine's journals of Radix Salviae Miltiorrhizae in the compound red sage root formula, 2003 the 26th the 4th phases of volume), the HPLC method is measured the content (Chinese herbal medicine of three kinds of water soluble ingredients of Radix Salviae Miltiorrhizae in the compound Salviae Miltiorrhizae, 2002 the 33rd the 10th phases of volume), HPLC measures the content (new Chinese medicine and clinical pharmacology, 2003 the 14th the 2nd phases of volume) of Saponins Content in Compound Danshen Prescription.All can only the separated measuring Radix Salviae Miltiorrhizae in the prior art or Radix Notoginseng in the content of a certain active component, have very big meaning so set up a kind of method that can control multiclass active constituent content in Radix Salviae Miltiorrhizae and the Radix Notoginseng simultaneously.
Summary of the invention:
The objective of the invention is to overcome the existing quality control defective that contains the compound preparation of Radix Salviae Miltiorrhizae and pseudo-ginseng, set up a kind of quality determining method that can measure the multiclass active component content of Radix Salviae Miltiorrhizae and Radix Notoginseng two flavor medicines in this type of compound preparation simultaneously.
The present invention tests and has adopted the HPLC-DAD method to measure protocatechualdehyde in the compound red sage root preparation simultaneously, salvianolic acid B, cryptotanshinone, tanshinone, arasaponin R1, the ginsenoside Rg1, ginsenoside Rb1's content, this method is simple relatively, the precision that tool is good, repeatability and reliability can be measured the content of the multiclass active component of Radix Salviae Miltiorrhizae and Radix Notoginseng in the compound red sage root preparation simultaneously, can be used for the quality control of compound red sage root preparation.
Concrete technical scheme of the present invention is as follows:
Contain the quality determining method of the compound preparation of Radix Salviae Miltiorrhizae and pseudo-ginseng, may further comprise the steps: prepare need testing solution and reference substance solution respectively, use high effective liquid chromatography for measuring, it is characterized in that:
Reference substance is: be selected from protocatechualdehyde, Panax Notoginseng saponin R
1, the ginsenoside Rg
1, salvianolic acid B, ginsenoside Rb
1, several in cryptotanshinone or the tanshinone;
Chromatographic condition is: with octadecyl silane is filler; The phosphoric acid water of acetonitrile-0.1% is a mobile phase, and wherein A is 0.1% phosphoric acid water, and B is an acetonitrile, A+B=100%, adopt 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, 35-65%B, 65-80min, 65-80%B; Column temperature: 25-35 ℃; Flow velocity: 1ml/min (when 22～28min, flow velocity is 0.8ml/min); The DAD detector, detecting wavelength is 203,270,281nm.Measure Panax Notoginseng saponin R at the 203nm place
1, the ginsenoside Rg
1With ginsenoside Rb
1, measure protocatechualdehyde at the 281nm place, salvianolic acid B is measured cryptotanshinone and tanshinone at the 270nm place.Phosphoric acid concentration is a percent by volume.
Preferred column temperature is 30 ℃.
Above-mentioned quality determining method, the preparation method of preferred reference substance is:
Precision takes by weighing reference substance a, protocatechualdehyde respectively, b, Panax Notoginseng saponin R
1, c, ginsenoside Rg
1, d, salvianolic acid B, e, ginsenoside Rb
1, f, cryptotanshinone and g, tanshinone are an amount of, put in the brown volumetric flask, add 70% methanol (cryptotanshinone and tanshinone add methanol) dissolving and standardize solution, product stock solution in contrast.The accurate respectively reference substance stock solution of drawing, put and mix and add 70% methanol constant volume in the brown volumetric flask, form and mix reference substance solution, concentration range is respectively: a, 1.32-210.40 μ g/ml, b, 15.34-368.16 μ g/ml, c, 14.76-590.40 μ g/ml, d, 12.70-762.00 μ g/ml, e, 30.06-601.20 μ g/ml, f, 0.33-66.00 μ g/ml, g, 0.32-64.56 μ g/ml.
Quality determining method of the present invention, wherein the preparation method of preferred need testing solution is: get the compound preparation that contains Radix Salviae Miltiorrhizae and pseudo-ginseng, desaccharide clothing or film-coat, grind into powder, precision takes by weighing 0.25g～2.0g and puts in the brown volumetric flask of 25ml, 70% methanol constant volume.Supersound extraction 30min is put coldly, adds 70% methanol and supplies weight.Shake up, filter, get subsequent filtrate, promptly.
The test sample of above-mentioned preparation and the sample size of reference substance are 10 μ l; Writing time 80min.When only measuring protocatechualdehyde, Panax Notoginseng saponin R
1, the ginsenoside Rg
1, salvianolic acid B, ginsenoside Rb
1The time, be that 60～65min gets final product writing time.
Above-mentioned quality determining method, wherein detecting wavelength can only be 203,281nm.
Quality determining method of the present invention, wherein compound preparation is selected from all compound preparations that contain Radix Salviae Miltiorrhizae and Radix Notoginseng, as DANQI PIAN, FUFANG DANSHEN PIAN, FUFANG DANSHEN DIWAN or GUANXIN DANSHEN PIAN etc.
The compound preparation quality determining method that contains Radix Salviae Miltiorrhizae and pseudo-ginseng of the present invention, adopt the DAD detector, measure arasaponin R1, ginsenoside Rg1 and ginsenoside Rb1 at the 203nm place, measure protocatechualdehyde at the 281nm place, salvianolic acid B is measured cryptotanshinone and tanshinone at the 270nm place.
The compound preparation quality determining method that contains Radix Salviae Miltiorrhizae and pseudo-ginseng of the present invention, the assay index suitably reduces, and still embodies essence of the present invention as the content of measuring arasaponin R1, ginsenoside Rg1, ginsenoside Rb1, salvianolic acid B and tanshinone.
The compound preparation quality determining method that contains Radix Salviae Miltiorrhizae and pseudo-ginseng of the present invention, detecting wavelength is 203nm and 281nm, promptly measures arasaponin R1, ginsenoside Rg1 and ginsenoside Rb1 at the 203nm place, measures protocatechualdehyde at the 281nm place, salvianolic acid B, cryptotanshinone and tanshinone.Still can reach purpose of the present invention.
Method of the present invention is as follows with the progressive that existing compound red sage root preparation quality determining method is compared: this method has overcome the defective that existing national standard detection method does not have compound components of panax notoginseng assay index, by adopting the HPLC-DAD method, realized measuring the multiclass active component content time in Radix Salviae Miltiorrhizae and the Radix Notoginseng.The results showed that the multiple component separating degree of being surveyed is good, linear relationship, repeatability, precision, stability, the response rate are all better.This method is accurate, and the advanced person is easy and simple to handle, can more effective, more fully control the quality of product.
The specific embodiment
Embodiment 1
1. instrument and reagent
Agilent 1100 type series of high efficiency chromatograph of liquid comprise G1312A quaternary gradient pump, G1313A automatic sampler, G1316A column oven, G1315A DAD detector; Chemstation 6.01 chromatographic work stations.
Compound red sage root preparation: DANQI PIAN (Radix Salviae Miltiorrhizae: Radix Notoginseng=1: 1): the Hunan Pharmaceutical Co's (lot number: 040803) that stablizes the country; FUFANG DANSHEN PIAN (Radix Salviae Miltiorrhizae: Radix Notoginseng=450: 141): 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); FUFANG DANSHEN DIWAN: sky, Tianjin Shi Li Pharmaceutical Co (lot number: 20020921,20030604,20040303).
Reference substance: protocatechualdehyde, salvianolic acid B, tanshinone, Panax Notoginseng saponin R
1, the ginsenoside Rg
1, ginsenoside Rb
1Available from Nat'l Pharmaceutical ﹠ Biological Products Control Institute; Cryptotanshinone is purchased in Chengdu Cisco China Bioisystech Co., Ltd.Purity all＞98%.
Methanol (chromatographically pure), acetonitrile (chromatographically pure, German Merck company), Milli-Q ultra-pure water.All the other reagent are analytical pure.
2. chromatographic condition
Chromatographic column: C18 chromatographic column (ZORBAX ODS 4.6 * 250mm ID, 5 μ m) and pre-column (4.6 * 12.5mm ID, 5 μ m); 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, 35-65%B, 65-80min, 65-80%B.Column temperature: 30 ℃; Flow velocity: 1ml/min (22-28min, 0.8ml/min); Detect wavelength 203nm, 270nm, 281nm measures arasaponin R1, ginsenoside Rg1 and ginsenoside Rb1 at the 203nm place, measures protocatechualdehyde at the 281nm place, and salvianolic acid B is measured cryptotanshinone and tanshinone at the 270nm place.Writing time 80min.
3. experimental technique and result
3.1 the preparation of need testing solution:
Get 20 of DANQI PIAN (desaccharide clothing) and FUFANG DANSHEN PIAN, weigh, it is heavy to calculate average sheet, and grinds to form powder, and precision takes by weighing 0.5g, puts in the brown volumetric flask of 25ml 70% methanol constant volume.Get 75 of FUFANG DANSHEN DIWAN (about 2g), 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 filters, and gets subsequent filtrate, promptly.
3.2 the preparation of reference substance solution:
Precision takes by weighing reference substance (1) protocatechualdehyde 2.63mg, (2) arasaponin R1 7.67mg, (3) ginsenoside Rg1 12.30mg respectively, (4) salvianolic acid B 2.54mg, (5) ginsenoside Rb1 12.53mg puts in the brown volumetric flask of 5ml, adds 70% methanol, (6) cryptotanshinone 2.75mg, (7) tanshinone 2.69mg puts in the brown volumetric flask of 5ml, adds methanol, dissolving and standardize solution, product stock solution in contrast.
A certain amount of reference substance stock solution of accurate respectively absorption is put brown volumetric flask and is mixed and add 70% methanol constant volume, forms and mixes reference substance solution.Each reference substance concentration is respectively: (1) 105.2 μ g/ml, (2) 184.08 μ g/ml, (3) 381.0 μ g/ml, (4) 295.2 μ g/ml, (5) 100.20 μ g/ml, (6) 33.0 μ g/ml, (7) 21.52 μ g/ml.
3.3 content assaying method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure.The results are shown in Table 1.
Three kinds of compound red sage root preparation assays of table 1 result (detect wavelength 203nm, 270nm, 281nm)
| Medicine | Lot number | Content (mg/g) | ||||||
| Protocatechualdehyde | Arasaponin R1 | The ginsenoside Rg1 | Salvianolic acid B | The ginsenoside Rb1 | Cryptotanshinone | Tanshinone | ||
| DANQI PIAN FUFANG DANSHEN PIAN FUFANG DANSHEN DIWAN | 040803 050308 03121024 040602 20020921 20030604 | 0.44±0.009 0.18±0.001 0.16±0.009 0.42±0.015 1.9±0.02 1.79±0.06 | 3.87±0.08 3.61±0.18 1.74±0.08 5.93±0.07 1.54±0.05 1.59±0.11 | 13.16±0.22 11.20±0.35 5.81±0.29 14.42±0.48 3.63±0.11 2.18±0.07 | 5.81±0.07 21.55±0.65 14.31±0.74 25.35±0.72 0.92+0.04 1.29±0.04 | 12.71±0.52 8.64±0.26 4.89±0.22 16.14±0.26 2.89±0.27 1.98±0.07 | ND 1.25±0.02 1.13±0.04 1.36±0.04 0.0185±0.0010 0.0149±0.0008 | ND 1.58±0.03 1.07±0.05 2.24±0.13 0.0208±0.0009 0.0196±0.0011 |
| 20040303 | 1.99±0.04 | 1.51±0.03 | 3.19±0.05 | 1.67±0.03 | 2.88±0.06 | 0.0315±0.0017 | 0.0371±0.0016 | |
| Content (mg/tablet, pill) | ||||||||
| Protocatechualdehyde | Panax Notoginseng saponin R 1 | The ginsenoside Rg 1 | Salvianolic acid B | Ginsenoside Rb 1 | Cryptotanshinone | Tanshinone | ||
| DANQI PIAN FUFANG DANSHEN PIAN FUFANG DANSHEN DIWAN | 40803 050308 3121024 040602 20020921 20030604 20040303 | 0.14±0.003 0.06±0.004 0.05±0.0028 0.10±0.0035 0.05±0.0005 0.05±0.0016 0.05±0.0008 | 1.21±0.02 1.24±0.06 0.53±0.02 1.47±0.02 0.04±0.001 0.04±0.003 0.04±0.001 | 4.13±0.07 3.85±0.12 1.78±0.09 3.59±0.13 0.09±0.003 0.06±0.002 0.08±0001 | 1.82±0.02 7.4±0.22 4.37±0.23 6.30±0.16 0.02±0.001 0.03±0.001 0.04±0.001 | 3.99±0.16 2.97±0.09 1.49±0.07 4.01±0.05 0.07±0.007 0.05±0.002 0.08±0.001 | ND 0.43±0.01 0.35±0.01 0.34±0.01 0.0005±0.00002 0.0004±0.00002 0.0008±0.00004 | ND 0.54±0.01 0.33±0.02 0.56±0.03 0.0005±0.00002 0.0005±0.00003 0.0010±0.00004 |
ND: do not detect
Embodiment 2
Detecting wavelength is 203nm and 281nm, measures arasaponin R1, ginsenoside Rg1 and ginsenoside Rb1 at the 203nm place, measures protocatechualdehyde, salvianolic acid B, cryptotanshinone and tanshinone at the 281nm place.Writing time 80min.Other is with embodiment 1.Experimental result such as table 2:
Three kinds of compound red sage root preparation assays of table 2 result (detects wavelength 203nm, 281nm)
| Medicine | Lot number | Content (mg/g) | ||||||
| Protocatechualdehyde | Panax Notoginseng saponin R 1 | The ginsenoside Rg 1 | Salvianolic acid B | Ginsenoside Rb 1 | Cryptotanshinone | Radix Salviae Miltiorrhizae IIA | ||
| DANQI PIAN FUFANG DANSHEN PIAN FUFANG DANSHEN DIWAN | 40803 50308 3121024 40602 20020921 20030604 20040303 | 0.44±0.009 0.18±0.001 0.16±0.009 0.42±0.015 1.9±0.02 1.79±0.06 1.99±0.04 | 3.87±0.08 3.61±0.18 1.74±0.08 5.93±0.07 1.54±0.05 1.59±0.11 1.51±0.03 | 13.16±0.22 11.20±0.35 5.81±0.29 14.42±0.48 3.63±0.11 2.18±0.07 3.19±0.05 | 5.81±0.07 21.55±0.65 14.31±0.74 25.35±0.72 0.92±0.04 1.29±0.04 1.67±0.03 | 12.71±0.52 8.64±0.26 4.89±0.22 16.14±0.26 2.89±0.27 1.98±0.07 2.88±0.06 | ND 1.33±0.10 1.19±0.04 1.44±0.03 0.0218±0.0009 0.0213±0.0009 0.0381±0.0008 | ND 1.58±0.03 1.09±0.04 2.15±0.12 0.0228±0.0003 0.0223±0.0003 0.0394±0.0005 |
| Content (mg/tablet, pill) | ||||||||
| Protocatechualdehyde | Panax Notoginseng saponin R 1 | The ginsenoside Rg 1 | Salvianolic acid B | Ginsenoside Rb 1 | Cryptotanshinone | Radix Salviae Miltiorrhizae IIA | ||
| The DANQI PIAN FUFANG DANSHEN PIAN | 40803 50308 3121024 | 0.14±0.003 0.06±0.004 0.05±0.0028 | 1.21±0.02 1.24±0.06 0.53±0.02 | 4.13±0.07 3.85±0.12 1.78±0.09 | 1.82±0.02 7.4±0.22 4.37±0.23 | 3.99±0.16 2.97±0.09 1.49±0.07 | ND 0.46±0.04 0.37±0.01 | ND 0.54±0.01 0.33±0.01 |
| FUFANG DANSHEN DIWAN | 40602 20020921 20030604 20040303 | 0.10±0.0035 0.05±0.0005 0.05±0.0016 0.05±0.0008 | 1.47±0.02 0.04±0.001 0.04±0.003 0.04±0.001 | 3.59±0.13 0.09±0.003 0.06±0.002 0.08±0.001 | 6.30±0.16 0.02±0.001 0.03±0.001 0.04±0.001 | 4.01±0.05 0.07±0.007 0.05±0.002 0.08±0.001 | 0.36±0.01 0.0005±0.00002 0.0005±0.00002 0.0010±0.00002 | 0.53±0.03 0.0006±0.00001 0.0006±0.00001 0.0010±0.00001 |
ND: do not detect
Experimental example 3
Methodological study:
1. linear relationship
Precision takes by weighing reference substance (1) protocatechualdehyde 2.63mg, (2) Panax Notoginseng saponin R respectively
17.67mg, (3) ginsenoside Rg
112.30mg, (4) salvianolic acid B 2.54mg, (5) ginsenoside Rb
112.53mg (6) cryptotanshinone 2.75mg and (7) tanshinone 2.69mg put in the brown volumetric flask of 5ml, add 70% methanol (cryptotanshinone and tanshinone add methanol) dissolving and standardize solution, product stock solution in contrast.A certain amount of reference substance stock solution of accurate respectively absorption is put brown volumetric flask and is mixed and add 70% methanol constant volume, forms the mixing reference substance solution of 10 concentration, and concentration is respectively: (1) 1.32,2.63,5.26,7.89,13.15,26.30,52.60,105.20,157.80,210.40 μ g/ml, (2) 15.34,30.68,38.35,46.02,61.36,122.72,184.08,245.44,306.80,368.16 μ g/ml, (3) 29.52,44.28,59.04,73.80,98.40,196.80,295.20,393.60,492.00,590.40 μ g/ml, (4) 12.70,25.40,38.10,63.50,127.00,254.00,381.00,508.00,635.00,762.00 μ g/ml, (5) 30.06,45.09,60.12,75.15,100.20,200.40,300.60,400.80,501.00,601.20 μ g/ml, (6) 0.33,0.66,1.32,2.64,5.28,8.25,11.00,16.50,33.00,66.00 μ g/ml, (7) 0.32,0.65,1.35,2.69,5.38,10.76,16.14,21.52,32.28,64.56 μ g/ml.
Under " embodiment 1 " chromatographic condition, each concentration reference substance solution is sample introduction 10 μ l respectively.With peak area (y) to concentration (x, mgL
-1) carry out linear regression, regression equation, see Table 3 and table 4.
Table 3 linear relationship experimental result (203,270,281nm) (n=10)
| Reference substance | Detect wavelength | Regression equation | Correlation coefficient | The range of linearity (mgL -1) |
| The protocatechualdehyde Panax Notoginseng saponin R 1The ginsenoside Rg 1Salvianolic acid B | 281nm 203nm 203nm 281nm | y＝43.5608x-12.3336 y＝3.1599x-3.8663 y＝3.7344x-8.3900 y＝5.1923x-8.1529 | 0.9999 0.9996 0.9997 0.9998 | 1.32-210.40 15.34-368.16 14.76-590.40 12.70-762.00 |
| Ginsenoside Rb 1The cryptotanshinone tanshinone | 203nm 270nm 270nm | y＝2.6497x-5.0981 y＝41.3225x-18.6750 y＝47.2084x-31.9843 | 0.9995 0.9992 0.9993 | 30.06-601.20 0.33-66.00 0.32-64.56 |
Y: peak area x: concentration (mgL
-1).
Table 4 linear relationship experimental result (203,281nm) (n=10)
| Reference substance | Detect wavelength | Regression equation | Correlation coefficient | The range of linearity (mgL -1) |
| The protocatechualdehyde Panax Notoginseng saponin R 1The ginsenoside Rg 1Salvianolic acid B ginsenoside Rb 1The cryptotanshinone tanshinone | 281nm 203nm 203nm 281nm 203nm 281nm 281nm | y＝43.5608x-12.3336 y＝3.1599x-3.8663 y＝3.7344x-8.3900 y＝5.1923x-8.1529 y＝2.6497x-5.0981 y＝16.4827x-11.6455 y＝30.4299x-26.0577 | 0.9999 0.9996 0.9997 0.9998 0.9995 0.9993 0.9993 | 1.32-210.40 15.34-368.16 14.76-590.40 12.70-762.00 30.06-601.20 0.66-66.00 0.64-64.56 |
2. precision experiment
Get " linear relationship " item 1/2 Concentraton gradient point down, continuous sample introduction 6 times, with calculated by peak area, 7 chemical compound withinday precisions are respectively 1.25%, 1.05%, 0.71%, 1.12%, 0.61%, 0.46%, 0.61%.Successive analysis 4 days, 7 chemical compound day to day precision are respectively 1.13%, 1.78%, and 0.85%, 1.76%, 1.29%, 0.91%, 2.16%.
3. repeated experiment
Get DANQI PIAN, FUFANG DANSHEN PIAN (050308) and FUFANG DANSHEN DIWAN (20040303), 6 parts in each sample prepares need testing solution and analysis according to embodiment 1 method, and the RSD of 7 chemical compound chromatographic peak areas is respectively as a result: (1) 2.61%, 2.17%, 1.49%; (2) 2.99%, 4.32%, 2.92%; (3) 1.28%, 2.32%, 1.62%; (4) 1.58%, 2.31%, 2.67%; (5) 3.19%, 2.70%, 2.04%; (6) 9.73%, 1.59%, 6.52%; (7) 9.59%, 1.84%, 6.18%.
4. stability experiment
Get " replica test " item DANQI PIAN, FUFANG DANSHEN PIAN and each portion of FUFANG DANSHEN DIWAN need testing solution down, respectively at 0,2, measured in 4,6,8,12 hours, the RSD of 7 chemical compound chromatographic peak areas is respectively: (1) 2.15%, 1.72%, 1.25%; (2) 2.27%, 4.16%, 2.09%; (3) 1.32%, 2.03%, 1.37%; (4) 1.23%, 2.72%, 2.17%; (5) 2.79%, 2.21%, 1.67%; (6) 9.09%, 1.45%, 5.78%; (7) 8.90%, 1.55%, 5.28%.
5. average recovery test
Precision take by weighing known content DANQI PIAN (0.25g), FUFANG DANSHEN PIAN (0.25g, lot number: 050308) and FUFANG DANSHEN DIWAN (40 balls, lot number: 20040303), totally 5 parts, add 7 reference substances respectively: (1) 0.1000,0.0500,2.0000mg; (2) 0.9375,0.9375,1.5625mg; (3) 3.0180,2.8168,3.2192mg; (4) 1.4157,5.2272,1.6335mg; (5) 3.1578,2.1606,2.8254mg; (6) 0.0372,0.3720,0.0372mg; (7) 0.0385,0.3850,0.0385mg.Prepare need testing solution and analysis according to embodiment 1 method, the average recovery rate that gets 7 chemical compounds is respectively: (1) 98.5%, 99.8%, 96.7%; (2) 102.1%, 97.4%, 95.2%; (3) 102.6%, 102.1%, 100.4%; (4) 96.9%, 101.0%, 97.2%; (5) 99.0%, 98.1%, 99.3%; (6) 103.3%, 97.1%, 97.2%; (7) 104.9%, 94.4%, 95.8%.RSD is respectively: (1) 3.89%, 3.89%, 1.50%; (2) 4.60%, 4.60%, 3.57%; (3) 3.52%, 3.52%, 4.07%; (4) 4.07%, 4.07%, 2.05%; (5) 4.43%, 4.43%, 2.22%; (6) 2.97%, 2.97%, 4.59%; (7) 4.45%, 4.45%, 4.19%.
To sum up, the HPLC-DAD method that the present invention set up is measured protocatechualdehyde in the compound red sage root preparation simultaneously, salvianolic acid B, cryptotanshinone, tanshinone, arasaponin R1, the ginsenoside Rg1, ginsenoside Rb1's content, the precision that tool is good, repeatability, reliability, method is advanced simple, can measure the content of multiclass active component in the compound red sage root preparation simultaneously, can more effective, more fully control the quality of the compound preparation that contains Radix Salviae Miltiorrhizae and Radix Notoginseng.
Claims (8)
1, a kind of quality determining method that contains the compound preparation of Radix Salviae Miltiorrhizae and pseudo-ginseng may further comprise the steps: prepare need testing solution and reference substance solution respectively, use high effective liquid chromatography for measuring, it is characterized in that:
Reference substance is: be selected from protocatechualdehyde, Panax Notoginseng saponin R
1, the ginsenoside Rg
1, salvianolic acid B, ginsenoside Rb
1, several in cryptotanshinone or the tanshinone;
Chromatographic condition is: with octadecyl silane is filler; The phosphoric acid water of acetonitrile-0.1% is a mobile phase, and wherein A is 0.1% phosphoric acid water, and B is an acetonitrile, A+B=100%, adopt 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, 35-65%B, 65-80min, 65-80%B; Column temperature: 25-35 ℃; Flow velocity: 1ml/min, when 22～28min, flow velocity changes 0.8ml/min into; The DAD detector, detecting wavelength is 203,270,281nm.
2, the quality determining method of claim 1, wherein reference substance is: protocatechualdehyde, Panax Notoginseng saponin R
1, the ginsenoside Rg
1, salvianolic acid B, ginsenoside Rb
1, cryptotanshinone or tanshinone.
3, the quality determining method of claim 1, wherein column temperature is 30 ℃.
4, the quality determining method of claim 1, wherein the preparation method of reference substance is:
Precision takes by weighing reference substance a, protocatechualdehyde respectively, b, Panax Notoginseng saponin R
1, c, ginsenoside Rg
1, d, salvianolic acid B, e, ginsenoside Rb
1, adding 70% methanol constant volume, f, cryptotanshinone and g, tanshinone add methanol constant volume, in contrast the product stock solution; The accurate respectively reference substance stock solution of drawing, put and mix and add 70% methanol constant volume in the volumetric flask, form and mix reference substance solution, concentration range is respectively: a, 1.32-210.40 μ g/ml, b, 15.34-368.16 μ g/ml, c, 14.76-590.40 μ g/ml, d, 12.70-762.00 μ g/ml, e, 30.06-601.20 μ g/ml, f, 0.33-66.00 μ g/ml, g, 0.32-64.56 μ g/ml.
5, the quality determining method of claim 1, wherein the preparation method of need testing solution is: get the compound preparation that contains Radix Salviae Miltiorrhizae and pseudo-ginseng, desaccharide clothing or film-coat, grind into powder, precision takes by weighing 0.25g～2.0g and puts in the brown volumetric flask of 25ml, 70% methanol constant volume, supersound extraction 30min, put cold, add 70% methanol and supply weight, shake up, filter, get subsequent filtrate, promptly.
6, the quality determining method of claim 1, the sample size of high performance liquid chromatography are 10 μ l; Writing time 80min.
7, the quality determining method of claim 1, wherein detecting wavelength is 203,281nm.
8, the quality determining method of claim 1, wherein compound preparation is selected from DANQI PIAN, FUFANG DANSHEN PIAN, FUFANG DANSHEN DIWAN or GUANXIN DANSHEN PIAN.
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