CN1899362B - Quality control method for shenqi injection strengthening body resistance - Google Patents
Quality control method for shenqi injection strengthening body resistance Download PDFInfo
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Abstract
The quality control method for body resistance strengthening Shenqi injection includes the following steps: 1. preparing sample solution of body resistance strengthening Shenqi injection; 2. preparing reference substance solution; 3. selecting chromatographic conditions; 4. efficient liquid chromatographic detection to obtain the fingerprint of the sample solution of body resistance strengthening Shenqi injection; and 5. comparing the obtained fingerprint of the sample solution of body resistance strengthening Shenqi injection with standard fingerprint and judging product quality based on whether to have similarity degree higher than 0.9. The quality control method is simple, stable, precise and high in reproductivity.
Description
Technical field
The present invention relates to the method for quality control of ginseng and astragalus injection for strengthening body, particularly relate to the fingerprint control method of ginseng and astragalus injection for strengthening body.
Background technology
Radix Codonopsis (Radix Codonopsis) property of medicine is gentle, and purposes is wide, has various pharmacological activities, not only digestion, cardiovascular system is had effect, and can also regulate function of immune system, and the resistibility of enhancing body, toxicity are very little.The Radix Astragali (Radix Astragalus) is the tonifying Qi main ingredient, can obviously increase the phagocytic function of macrophage, share with Radix Codonopsis, and the effect of macrophage phagocytic objectionable impurities is strengthened.Ginseng and astragalus injection for strengthening body is the pure Chinese medicinal preparation of being made through extraction by Radix Codonopsis, the Radix Astragali, sets upright based on beneficial gas.The nature and flavor of two kinds of medicines of the Radix Codonopsis and the Radix Astragali and returning through consistent, effect is basic identical, and both additions play that the monarch and his subjects help mutually, the synergy of the mutual-assistance, have obviously strengthened clinical efficacy.But, also there is not at present the control method of ginseng and astragalus injection for strengthening body finger-print, be difficult to guarantee the stability and the clinical safety in utilization of product.
Summary of the invention
The method of quality control that the purpose of this invention is to provide a kind of efficient, sensitive ginseng and astragalus injection for strengthening body.
The method of quality control of ginseng and astragalus injection for strengthening body provided by the present invention comprises the steps:
1) test solution of ginseng and astragalus injection for strengthening body sample preparation: will pass through macroporous adsorptive resins after the ginseng and astragalus injection for strengthening body sample concentration, elder generation's water wash-out, use certain density ethanol elution again, collecting ethanol eluate is concentrated into dried, residue adds water or certain density dissolve with ethanol, gets the test solution of ginseng and astragalus injection for strengthening body sample;
2) preparation of reference substance solution: calycosin-7-O-β-D-glucopyranoside reference substance is dissolved in methyl alcohol, as the reference substance solution of phenolic acids finger-print; The Astragaloside IV reference substance is dissolved in methyl alcohol, as the reference substance solution of saponins finger-print.
3) chromatographic condition: chromatographic column is filling agent with the octadecylsilane chemically bonded silica; Second eyeball-water is moving phase, gradient elution; Detect phenolic acids finger-print under 200-215nm and the 250-280nm respectively with UV-detector; Detect the saponins finger-print with evaporative light-scattering detector;
4) high performance liquid chromatography detects: the test solution and the reference substance solution of getting the ginseng and astragalus injection for strengthening body sample, inject high performance liquid chromatograph, carry out high performance liquid chromatography and detect, obtain three of the finger-prints of ginseng and astragalus injection for strengthening body sample: one of two of phenolic acids finger-prints and saponins finger-print;
5) comparison: the finger-print of gained ginseng and astragalus injection for strengthening body sample is compared with the reference fingerprint of ginseng and astragalus injection for strengthening body respectively, and similarity is specification product greater than 0.9 ginseng and astragalus injection for strengthening body sample;
1. the phenolic acids finger-print under the 200-215nm: have 8 chromatographic peaks, with the retention time of the chromatographic peak of calycosin-7-O-β-D-glucopyranoside and peak area is 1 to calculate the relative retention time and the relative peak area at other peaks, No. 1 peak relative retention time is 0.20-0.30, and relative peak area is 1.60-3.50; No. 2 peak relative retention times are 0.25-0.33, and relative peak area is 0.70-1.50; No. 3 peak relative retention times are 0.40-0.50, and relative peak area is 1.20-2.90; S peak relative retention time is 1, and relative peak area is 1; No. 4 peak relative retention times are 0.90-1.20, and relative peak area is 0.22-0.40; No. 5 peak relative retention times are 1.20-1.40, and relative peak area is 0.22-0.40; No. 6 peak relative retention times are 1.38-1.46, and relative peak area is 0.90-1.50; No. 7 peak relative retention times are 1.42-1.53, and relative peak area is 0.23-0.42;
2. the phenolic acids finger-print under the 250-280nm: have 6 chromatographic peaks, with the retention time of the chromatographic peak of calycosin-7-O-β-D-glucopyranoside and peak area is 1 to calculate the relative retention time and the relative peak area at other peaks, No. 1 peak relative retention time is 0.15-0.28, and relative peak area is 0.80-1.80; No. 2 peak relative retention times are 0.25-0.33, and relative peak area is 1.25-2.50; No. 3 peak relative retention times are 0.25-0.33, and relative peak area is 0.80-1.70; S peak relative retention time is 1, and relative peak area is 1; No. 4 peak relative retention times are 0.33-0.40, and relative peak area is 0.50-1.30; No. 5 peak relative retention times are 0.40-0.50, and relative peak area is 1.20-2.50; S peak relative retention time is 1, and relative peak area is 1;
3. saponins finger-print: have 9 chromatographic peaks, with the retention time of the chromatographic peak of Astragaloside IV and peak area is 1 to calculate the relative retention time and the relative peak area at other peaks, No. 1 peak relative retention time is 0.51-0.58, and relative peak area is 0.70-1.20; No. 2 peak relative retention times are 0.74-0.82, and relative peak area is 0.45-1.20; No. 3 peak relative retention times are 0.78-0.85, and relative peak area is 0.15-0.23; No. 4 peak relative retention times are 0.88-0.93, and relative peak area is 0.17-0.25; No. 5 peak relative retention times are 0.90-1.00, and relative peak area is 0.09-0.17; S peak relative retention time is 1, and relative peak area is 1; No. 6 peak relative retention times are 0.95-1.10, and relative peak area is 0.30-0.40; No. 7 peak relative retention times are 0.98-1.10, and relative peak area is 0.60-0.80; No. 8 peak relative retention times are 0.10-1.15, and relative peak area is 0.60-1.0.
Wherein, the test solution preparation process of phenolic acids finger-print is preferably: precision is measured ginseng and astragalus injection for strengthening body sample 25ml, put and be concentrated into about 5ml in the water-bath, slowly (column internal diameter is 1.5cm by the AB-8 macroporous adsorptive resins, column length is 20cm), water 70ml wash-out, discard water elution liquid, continuous with 70% ethanol 80ml wash-out, collect 70% ethanol eluate, put be concentrated in the water-bath dried, residue is dissolved in water and is transferred in the 10ml measuring bottle, and thin up shakes up to scale, filter with 0.45 μ m miillpore filter, promptly.
The test solution preparation process of saponins finger-print is preferably: precision is measured ginseng and astragalus injection for strengthening body sample 200ml, put and be concentrated into about 10ml in the water-bath, slowly by AB-8 macroporous adsorptive resins (column internal diameter is 1.5cm, and column length is 20cm), water 80ml wash-out discards water elution liquid; Continuous with 20% ethanol 80ml wash-out, discard 20% ethanol eluate; Use 80% ethanol 100ml wash-out again, collect 80% ethanol eluate, put and be concentrated into driedly in the water-bath, residue adds 80% dissolve with ethanol and is transferred in the 5ml measuring bottle, is diluted to scale, shakes up, and filters with 0.45 μ m miillpore filter, promptly.
Step 2) preparation process of described reference substance solution is preferably: it is an amount of to get calycosin-7-O-β-D-glucopyranoside reference substance, adds methyl alcohol and makes the solution that contains 0.06mg in every 1ml solution, as the reference substance solution of phenolic acids finger-print; It is an amount of to get the Astragaloside IV reference substance, adds methyl alcohol and makes the solution that contains 0.1mg in every 1ml solution, as the reference substance solution of saponins finger-print.
The step 3) chromatographic condition is preferably: chromatographic column is filling agent with the octadecylsilane chemically bonded silica, model is Discovery C18,250 * 4.6mm, 5 μ m, theoretical cam curve is not less than 3000, is not less than 4000 by Astragaloside IV in the saponins finger-print by calycosin-7-O-β-D-glucopyranoside in the phenolic acids finger-print.30 ℃ of column temperatures; The phenolic acids finger-print detects with UV-detector, and the detection wavelength is 208nm, 266nm; The saponins finger-print detects with evaporative light-scattering detector, is mobile phase A with the acetonitrile, is Mobile phase B with water, and the regulation in the according to the form below is carried out gradient elution;
Step 4) high performance liquid chromatography testing process is preferably: accurate each 20 μ l of test solution that draw reference substance solution and ginseng and astragalus injection for strengthening body sample, inject high performance liquid chromatograph, and be 70 minutes writing time.
Principle of the present invention is to set up the HPLC finger-print of ginseng and astragalus injection for strengthening body, liposoluble ingredient in the ginseng and astragalus injection for strengthening body and saponin component are detected respectively with many finger-prints, hold ginseng and astragalus injection for strengthening body quality situation from the whole facial feature of each chromatogram, avoided estimating the one-sidedness of ginseng and astragalus injection for strengthening body total quality because of only measuring one, two chemical constitution, having reduced is the possibility of the artificial processing of requisite quality.The present invention has that method is easy, stable, precision is high, favorable reproducibility, be easy to characteristics such as grasp, simultaneously available this method distinguish with ginseng and astragalus injection for strengthening body at the similar traditional Chinese medicine of appearance luster ten, in case palm off, have a extensive future.
Description of drawings
Fig. 1～Fig. 3 is respectively the standard finger-print (being respectively phenolic acids finger-print and the saponins finger-print of 266nm, 208nm) of ginseng and astragalus injection for strengthening body;
Fig. 4 is determining of phenolic acids finger-print (208nm) S peak;
Fig. 5 is determining of phenolic acids finger-print (266nm) S peak;
Fig. 6 is determining of saponins finger-print S peak;
Fig. 7 A-Fig. 7 C is respectively astragalus injection finger-print (being respectively phenolic acids finger-print and the saponins finger-print of 266nm, 208nm);
Fig. 8 A-Fig. 8 C is respectively red sage roo drip liquid finger-print (being respectively phenolic acids finger-print and the saponins finger-print of 266nm, 208nm);
Fig. 9 A-Fig. 9 C is respectively ginseng and astragalus injection for strengthening body finger-print (being respectively phenolic acids finger-print and the saponins finger-print of 266nm, 208nm).
Embodiment
The foundation of the standard finger-print of embodiment 1, ginseng and astragalus injection for strengthening body
1, the preparation of standard testing solution
1. the specimen of phenolic acids finger-print: precision is measured ginseng and astragalus injection for strengthening body sample 25ml, puts and is concentrated into about 5ml in the water-bath, and slowly (column internal diameter is 1.5cm by the AB-8 macroporous adsorptive resins, column length is 20cm), water 70ml wash-out discards water elution liquid, continuous with 70% ethanol 80ml wash-out, collect 70% ethanol eluate, put and be concentrated into driedly in the water-bath, residue is dissolved in water and is transferred in the 10ml measuring bottle, thin up is to scale, shake up, filter with 0.45 μ m miillpore filter, promptly.
2. the specimen of saponins finger-print: precision is measured ginseng and astragalus injection for strengthening body sample 200ml, put and be concentrated into about 10ml in the water-bath, slowly by AB-8 macroporous adsorptive resins (column internal diameter is 1.5cm, and column length is 20cm), water 80ml wash-out discards water elution liquid; Continuous with 20% ethanol 80ml wash-out, discard 20% ethanol eluate; Use 80% ethanol 100ml wash-out again, collect 80% ethanol eluate, put and be concentrated into driedly in the water-bath, residue adds 80% dissolve with ethanol and is transferred in the 5ml measuring bottle, is diluted to scale, shakes up, and filters with 0.45 μ m miillpore filter, promptly.
2, the preparation of reference substance solution
It is an amount of to get calycosin-7-O-β-D-glucopyranoside reference substance, adds methyl alcohol and makes the solution that contains 0.06mg in every 1ml solution, as the reference substance solution of phenolic acids finger-print; It is an amount of to get the Astragaloside IV reference substance, adds methyl alcohol and makes the solution that contains 0.1mg in every 1ml solution, as the reference substance solution of saponins finger-print;
3, chromatographic condition
Chromatographic column is filling agent with the octadecylsilane chemically bonded silica, and model is Discovery C18,250 * 4.6mm, and 5 μ m are mobile phase A with the acetonitrile, are Mobile phase B with water, carry out gradient elution by the gradient of table 1; 30 ℃ of column temperatures; The phenolic acids finger-print detects with UV-detector, and the detection wavelength is 208nm, 266nm; The saponins finger-print detects with evaporative light-scattering detector.Theoretical cam curve is not less than 3000, is not less than 4000 by Astragaloside IV in the saponins finger-print by calycosin-7-O-β-D-glucopyranoside in the phenolic acids finger-print.
Table 1 gradient table
4, measure
Accurate standard testing solution and each 20 μ l of reference substance solution of drawing inject liquid chromatograph respectively, write down 70 minutes chromatogram,, and calculate similarity that is.
5, determine total peak
1. the total peak of phenolic acids finger-print (208nm) is definite: set up phenolic acids finger-print (208nm), it is auxiliary detection to phenolic acids finger-print (266nm), can detect detect at 266nm wavelength place less than composition, mainly concentrate in 35～50min, so with in this section more stable 4,5,6,7 chromatographic peaks are all listed in the total peak, alternative is selected the bigger chromatographic peak of peak area and is also classified total peak as. the chromatogram of contrast calycosin-7-O-β-D-glucopyranoside reference substance solution, select the S peak, see Fig. 4.
Select 20 batches of ginseng and astragalus injection for strengthening body (Livzon Group Limin Pharmaceutical Factory provides) to simulate with reference to spectrogram.
In similarity software, after total peak mated, it was as follows to calculate similarity result:
| Lot number | 060101 | 060102 | 060103 | 060104 | 060105 | 060106 | 060107 | 060108 | 060109 | 060110 |
| Similarity | 0.986 | 0.986 | 0.980 | 0.989 | 0.985 | 0.963 | 0.994 | 0.990 | 0.991 | 0.966 |
| Lot number | 06011 | 060112 | 060213 | 060214 | 060215 | 060216 | 060217 | 060218 | 060219 | 060220 |
| Similarity | 0.966 | 0.995 | 0.987 | 0.991 | 0.988 | 0.990 | 0.993 | 0.995 | 0.993 | 0.993 |
In sum, the phenolic acids finger-print (208nm) of ginseng and astragalus injection for strengthening body as shown in Figure 2.
2. the total peak of phenolic acids finger-print (266nm) is definite: selected total peak-to-peak area is bigger, comparatively stable, and all the other peak-to-peak areas are little, are subjected to baseline interference big, and reappearance is not good, so it is not proofreaied and correct when similarity is calculated, does not classify total peak as.The chromatogram of contrast calycosin-7-O-β-D-glucopyranoside reference substance solution is selected the S peak, sees Fig. 5.
In similarity software, after total peak mated, it was as follows to calculate similarity result:
| Lot number | 060101 | 060102 | 060103 | 060104 | 060105 | 060106 | 060107 | 060108 | 060109 | 060110 |
| Similarity | 0.990 | 0.980 | 0.989 | 0.993 | 0.993 | 0.987 | 0.993 | 0.999 | 0.999 | 0.999 |
| Lot number | 06011 | 060112 | 060213 | 060214 | 060215 | 060216 | 060217 | 060218 | 060219 | 060220 |
| Similarity | 0.982 | 0.995 | 0.992 | 0.996 | 0.994 | 0.998 | 0.998 | 0.991 | 0.990 | 0.994 |
In sum, the phenolic acids finger-print (266nm) of ginseng and astragalus injection for strengthening body as shown in Figure 1.
3. the total peak of saponins finger-print is definite: on collection of illustrative plates, the chromatographic peak in 35～45min is many and unstable, and the chromatographic peak in 45～70min is the saponins composition, so the chromatographic peak in main this section of selection is total peak.The chromatogram of contrast Astragaloside IV reference substance solution is selected the S peak, sees Fig. 6.
In similarity software, after total peak mated, it was as follows to calculate similarity result:
| Lot number | 060101 | 060102 | 060103 | 060104 | 060105 | 060106 | 060107 | 060108 | 060109 | 060110 |
| Similarity | 0.997 | 0.999 | 0.985 | 0.996 | 0.993 | 0.990 | 0.980 | 0.992 | 0.997 | 0.989 |
| Lot number | 06011 | 060112 | 060213 | 060214 | 060215 | 060216 | 060217 | 060218 | 060219 | 060220 |
| Lot number | 060101 | 060102 | 060103 | 060104 | 060105 | 060106 | 060107 | 060108 | 060109 | 060110 |
| Similarity | 0.998 | 0.991 | 0.988 | 0.994 | 0.994 | 0.989 | 0.986 | 0.980 | 0.997 | 0.993 |
In sum, the saponins finger-print of ginseng and astragalus injection for strengthening body as shown in Figure 3.
6, the reappearance of finger-print and stability experiment
1. phenolic acids finger-print (208nm):
Get ginseng and astragalus injection liquid 050815, carried out stability, precision, reproducible methodology test.To its similarity result of calculation such as following table 2, table 3, table 4.
Table 2 stability test similarity result of calculation table
| 0hr | 3hr | 6hr | 12hr | 18hr | RSD | |
| Similarity | 0.995 | 0.990 | 0.987 | 0.990 | 0.985 | 0.38％ |
Table 3 precision test similarity result of calculation table
| 1 | 2 | 3 | 4 | 5 | 6 | RSD | |
| Similarity | 0.986 | 0.991 | 0.982 | 0.984 | 0.993 | 0.976 | 0.47％ |
Table 4 reappearance test similarity result of calculation table
| 1 | 2 | 3 | 4 | 5 | 6 | RSD | |
| Similarity | 0.988 | 0.990 | 0.990 | 0.994 | 0.984 | 0.986 | 0.37％ |
The result shows: this method stability, precision, reappearance are good.
2. phenolic acids finger-print (266nm):
Get ginseng and astragalus injection liquid 050815, carried out stability, precision, reproducible methodology test.To its similarity result of calculation such as following table 5, table 6, table 7.
Table 5 stability test similarity result of calculation table
| 0hr | 3hr | 6hr | 12hr | 18hr | RSD | |
| Similarity | 0.986 | 0.984 | 0.971 | 0.985 | 0.975 | 0.69％ |
Table 6 precision test similarity result of calculation table
| 1 | 2 | 3 | 4 | 5 | 6 | RSD | |
| Similarity | 0.972 | 0.968 | 0.987 | 0.990 | 0.988 | 0.966 | 1.04％ |
Table 7 reappearance test similarity result of calculation table
| 1 | 2 | 3 | 4 | 5 | 6 | RSD | |
| Similarity | 0.991 | 0.983 | 0.989 | 0.986 | 0.991 | 0.972 | 0.35％ |
The result shows: this method stability, precision, reappearance are good.
3. saponins finger-print:
Get ginseng and astragalus injection liquid 050815, carried out stability, precision, reproducible methodology test.To its similarity result of calculation such as following table 8, table 9, table 10.
Table 8 stability test similarity result of calculation table
| 0hr | 3hr | 6hr | 12hr | 18hr | RSD | |
| Similarity | 0.992 | 0.994 | 0.994 | 0.996 | 0.993 | 0.15％ |
Table 9 precision test similarity result of calculation table
| 1 | 2 | 3 | 4 | 5 | 6 | RSD | |
| Similarity | 0.990 | 0.999 | 0.994 | 0.994 | 0.995 | 0.993 | 0.32％ |
Table 10 reappearance test similarity result of calculation table
| 1 | 2 | 3 | 4 | 5 | 6 | RSD | |
| Similarity | 0.991 | 0.992 | 0.994 | 0.991 | 0.997 | 0.990 | 0.26％ |
The result shows: this method stability, precision, reappearance are good.
Embodiment 2, this method are applied to the quality control of ginseng and astragalus injection for strengthening body
Choose commercially available astragalus injection, red sage roo drip liquid, ginseng and astragalus injection for strengthening body, measure its finger-print according to the method for embodiment 1, compare with standard finger-print, similarity greater than 0.9 be ginseng and astragalus injection for strengthening body, remaining all is lower than 0.9, can be used for differentiating the true and false of ginseng and astragalus injection for strengthening body.
Astragalus injection:
As Fig. 7 A-Fig. 7 C, its similarity is respectively 0.409,0.315,0.611 respectively for the phenolic acids finger-print of 208nm, 266 nanometers and saponins finger-print.
Red sage roo drip liquid:
The phenolic acids finger-print of 208nm, 266 nanometers and saponins finger-print be respectively as Fig. 8 A-Fig. 8 C, and its similarity is respectively 0.292,0.257,0.000.
Ginseng and astragalus injection for strengthening body:
As Fig. 9 A-Fig. 9 C, its similarity is respectively 0.983,0.985,0.981 respectively for the phenolic acids finger-print of 208nm, 266 nanometers and saponins finger-print.
Many batches of commercially available ginseng and astragalus injection for strengthening body are measured its finger-print according to the method for embodiment 1, compare with standard finger-print, similarity confirms not find the product of inferior quality all greater than 0.9.
Claims (4)
1. the discrimination method of a ginseng and astragalus injection for strengthening body comprises the steps:
1) test solution of ginseng and astragalus injection for strengthening body sample preparation:
The test solution preparation process of phenolic acids finger-print is: precision is measured ginseng and astragalus injection for strengthening body sample 25ml, puts and is concentrated into 5ml in the water-bath, and slowly by the AB-8 macroporous adsorptive resins, column internal diameter is 1.5cm, and column length is 20cm; The water 70ml of elder generation wash-out discards water elution liquid, and is continuous with 70% ethanol 80ml wash-out, collects 70% ethanol eluate, put and be concentrated into driedly in the water-bath, residue is dissolved in water and is transferred in the 10ml measuring bottle, and thin up shakes up to scale, filter with 0.45 μ m miillpore filter, that is, and
The test solution preparation process of saponins finger-print is: precision is measured ginseng and astragalus injection for strengthening body sample 200ml, puts and is concentrated into 10ml in the water-bath, and slowly by the AB-8 macroporous adsorptive resins, column internal diameter is 1.5cm, and column length is 20cm; The water 80ml of elder generation wash-out discards water elution liquid; Continuous with 20% ethanol 80ml wash-out, discard 20% ethanol eluate; Use 80% ethanol 100ml wash-out again, collect 80% ethanol eluate, put and be concentrated into driedly in the water-bath, residue adds 80% dissolve with ethanol and is transferred in the 5ml measuring bottle, is diluted to scale, shakes up, and filters with 0.45 μ m miillpore filter, promptly;
2) preparation of reference substance solution: calycosin-7-O-β-D-glucopyranoside reference substance is dissolved in methyl alcohol, as the reference substance solution of phenolic acids finger-print; The Astragaloside IV reference substance is dissolved in methyl alcohol, as the reference substance solution of saponins finger-print;
3) chromatographic condition: chromatographic column is filling agent with the octadecylsilane chemically bonded silica; With the acetonitrile-water is moving phase, gradient elution; Detect phenolic acids finger-print under 200-215nm and the 250-280nm respectively with UV-detector; Detect the saponins finger-print with evaporative light-scattering detector, wherein the gradient of gradient elution is as follows:
Time (minute) acetonitrile (%) water (%)
0～8 2→5 98→95
8～18 5→12 95→88
18～40 12→25 88→75
40～50 25→32.5 75→67.5
50～65 32.5→55 67.5→45
65～70 55→95 45→5
70～75 95 5
75～78 95→2 5→98
78～83 2 98
4) high performance liquid chromatography detects: get the test solution and the reference substance solution of ginseng and astragalus injection for strengthening body sample, inject high performance liquid chromatograph, carry out high performance liquid chromatography and detect, obtain the finger-print of ginseng and astragalus injection for strengthening body sample;
5) comparison: the finger-print of gained ginseng and astragalus injection for strengthening body sample and the reference fingerprint of ginseng and astragalus injection for strengthening body are compared, and similarity is specification product greater than 0.9 ginseng and astragalus injection for strengthening body sample;
1. the phenolic acids finger-print under the 200-215nm: have 8 chromatographic peaks, with the retention time of the chromatographic peak of calycosin-7-O-β-D-glucopyranoside and peak area is 1 to calculate the relative retention time and the relative peak area at other peaks, No. 1 peak relative retention time is 0.20-0.30, and relative peak area is 1.60-3.50; No. 2 peak relative retention times are 0.25-0.33, and relative peak area is 0.70-1.50; No. 3 peak relative retention times are 0.40-0.50, and relative peak area is 1.20-2.90; S peak relative retention time is 1, and relative peak area is 1; No. 4 peak relative retention times are 0.90-1.20, and relative peak area is 0.22-0.40; No. 5 peak relative retention times are 1.20-1.40, and relative peak area is 0.22-0.40; No. 6 peak relative retention times are 1.38-1.46, and relative peak area is 0.90-1.50; No. 7 peak relative retention times are 1.42-1.53, and relative peak area is 0.23-0.42;
2. the phenolic acids finger-print under the 250-280nm: have 6 chromatographic peaks, with the retention time of the chromatographic peak of calycosin-7-O-β-D-glucopyranoside and peak area is 1 to calculate the relative retention time and the relative peak area at other peaks, No. 1 peak relative retention time is 0.15-0.28, and relative peak area is 0.80-1.80; No. 2 peak relative retention times are 0.25-0.33, and relative peak area is 1.25-2.50; No. 3 peak relative retention times are 0.25-0.33, and relative peak area is 0.80-1.70; S peak relative retention time is 1, and relative peak area is 1; No. 4 peak relative retention times are 0.33-0.40, and relative peak area is 0.50-1.30; No. 5 peak relative retention times are 0.40-0.50, and relative peak area is 1.20-2.50; S peak relative retention time is 1, and relative peak area is 1;
3. saponins finger-print: have 9 chromatographic peaks, with the retention time of the chromatographic peak of Astragaloside IV and peak area is 1 to calculate the relative retention time and the relative peak area at other peaks, No. 1 peak relative retention time is 0.51-0.58, and relative peak area is 0.70-1.20; No. 2 peak relative retention times are 0.74-0.82, and relative peak area is 0.45-1.20; No. 3 peak relative retention times are 0.78-0.85, and relative peak area is 0.15-0.23; No. 4 peak relative retention times are 0.88-0.93, and relative peak area is 0.17-0.25; No. 5 peak relative retention times are 0.90-1.00, and relative peak area is 0.09-0.17; S peak relative retention time is 1, and relative peak area is 1; No. 6 peak relative retention times are 0.95-1.10, and relative peak area is 0.30-0.40; No. 7 peak relative retention times are 0.98-1.10, and relative peak area is 0.60-0.80; No. 8 peak relative retention times are 0.10-1.15, and relative peak area is 0.60-1.0.
2. method according to claim 1, it is characterized in that: the preparation process of reference substance solution is: it is an amount of to get calycosin-7-O-β-D-glucopyranoside reference substance, add methyl alcohol and make the solution that contains 0.06mg in every 1ml solution, as the reference substance solution of phenolic acids finger-print; It is an amount of to get the Astragaloside IV reference substance, adds methyl alcohol and makes the solution that contains 0.1mg in every 1ml solution, as the reference substance solution of saponins finger-print.
3. method according to claim 1 is characterized in that: the step 3) chromatographic condition is:
Chromatographic column is filling agent with the octadecylsilane chemically bonded silica, model is Discovery C18,250 * 4.6mm, 5 μ m, theoretical cam curve is not less than 3000, is not less than 4000 by Astragaloside IV in the saponins finger-print by calycosin-7-O-β-D-glucopyranoside in the phenolic acids finger-print; 30 ℃ of column temperatures; The phenolic acids finger-print detects with UV-detector, and the detection wavelength is 208nm, 266nm; The saponins finger-print detects with evaporative light-scattering detector.
4. method according to claim 1, it is characterized in that: step 4) high performance liquid chromatography testing process is: accurate each 20 μ of test solution that draw reference substance solution and ginseng and astragalus injection for strengthening body sample, inject high performance liquid chromatograph, be 70 minutes writing time.
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Non-Patent Citations (6)
| Title |
|---|
| 李锐等.膜荚黄芪与蒙古黄芪化学成分的高效液相色谱-质谱研究.分析化学33 12.2005,33(12),1676-1680. |
| 李锐等.膜荚黄芪与蒙古黄芪化学成分的高效液相色谱-质谱研究.分析化学33 12.2005,33(12),1676-1680. * |
| 胡芳弟等.黄芪的高效液相色谱指纹图谱及主成分含量测定.中药材27 11.2004,27(11),831-834. |
| 胡芳弟等.黄芪的高效液相色谱指纹图谱及主成分含量测定.中药材27 11.2004,27(11),831-834. * |
| 谢海燕等.HPLC-ELSD测定参芪扶正注射液中黄芪甲苷含量.中药研究与信息7 10.2005,7(10),7-9. |
| 谢海燕等.HPLC-ELSD测定参芪扶正注射液中黄芪甲苷含量.中药研究与信息7 10.2005,7(10),7-9. * |
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