CN101352478A - Quality control method of ginseng and astragalus injection for strengthening body - Google Patents
Quality control method of ginseng and astragalus injection for strengthening body Download PDFInfo
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Abstract
The invention discloses an improved quality control method of a ginseng and astragalus body resistance strengthening injection, in particular to an improved fingerprint control method of a ginseng and astragalus body resistance strengthening injection. In the method of the invention, the preparation method of the test solution of the ginseng and astragalus body resistance strengthening injection sample is modified into an A method: a ginseng and astragalus body resistance strengthening injection sample is concentrated in accordance with legal rules and passes through a macroporous absorptive resin column, water is firstly used for eluting, then ethanol is adopted for eluting, ethanol eluent is collected and concentrated to be dried, and residue is added with water or ethanol for being dissolved so as to obtain the test solution of the ginseng and astragalus body resistance strengthening injection sample; or into a B method: the ginseng and astragalus body resistance strengthening injection sample is leached by saturated normal butanol, the normal butanol liquid is concentrated to be dried, residue is added with polar solvent for dissolving and diluting and is filtered by a microporous film so as to obtain the test solution of the ginseng and astragalus body resistance strengthening injection sample.
Description
Technical field
The present invention relates to the method for quality control of improved SHENQI FUZHENG ZHUSHEYE, particularly relate to the fingerprint control method of improved SHENQI FUZHENG ZHUSHEYE.
Background technology
SHENQI FUZHENG ZHUSHEYE is the pure Chinese medicinal preparation of being made through extraction by Radix Codonopsis, the Radix Astragali, sets upright based on QI invigorating.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 synergism of the mutual-assistance, have obviously strengthened clinical efficacy.Yet quality control is the sixty-four dollar question that is used to guarantee Chinese medicine injection stability and clinical safety in utilization all the time.
Reported the method for quality control of relevant SHENQI FUZHENG ZHUSHEYE on January 24th, 2007 in disclosed No. 200610098953.1 Chinese patent application,, set up the HPLC finger printing of SHENQI FUZHENG ZHUSHEYE according to the method for putting down in writing in this patent disclosure.Although the method for record was according to having many advantages during this patent application was open, but the improvements of needs are arranged still, for example the preparation method of the test solution of SHENQI FUZHENG ZHUSHEYE sample only limits to a kind of method, and relate to the macroporous adsorbent resin that uses specific a kind of model in the method, its method universal applicability is restricted.Grope through test, adopt another preparation method can obtain same even better effect, increased the universal applicability of method.
Summary of the invention
The invention provides a kind of method of quality control of improved SHENQI FUZHENG ZHUSHEYE.
The method of quality control of SHENQI FUZHENG ZHUSHEYE provided by the present invention comprises the steps:
(1) test solution of preparation SHENQI FUZHENG ZHUSHEYE sample, described test solution comprises phenolic acids finger printing test fluid and saponins finger printing test fluid, the concrete preparation method of described test solution comprises the operating procedure that is selected from following A method or B method:
The A method: macroporous adsorptive resins is passed through in the legal concentrated back of SHENQI FUZHENG ZHUSHEYE sample, first water eluting, the reuse ethanol elution, the collection ethanol elution is concentrated into dried, and residue adds water or dissolve with ethanol, gets the test fluid of SHENQI FUZHENG ZHUSHEYE sample;
Or B method: with the saturated n-butanol extraction of SHENQI FUZHENG ZHUSHEYE sample, n-butyl alcohol liquid is concentrated into dried, residue additive polarity dissolution with solvents dilution filters with microporous membrane, obtains the test solution of SHENQI FUZHENG ZHUSHEYE sample.
(2) preparation of reference substance solution:
Calycosin-7-O-β-D-pyranglucoside reference substance is dissolved in methanol, as the reference substance solution of fen acids finger printing; The astragaloside reference substance is dissolved in methanol, as the reference substance solution of saponins finger printing;
(3) chromatographic condition
Chromatographic column is filler with the octadecylsilane chemically bonded silica; Second eyeball one water is mobile phase, gradient elution; Detect phenolic acids finger printing under 200-215nm and the 250-280nm respectively with UV-detector; Detect the saponins finger printing with evaporative light scattering detector;
(4) high performance liquid chromatography detects:
Get the test solution and the reference substance solution of the SHENQI FUZHENG ZHUSHEYE sample that A method or B method make, inject high performance liquid chromatograph, carry out high performance liquid chromatography and detect, obtain three of the finger printing of SHENQI FUZHENG ZHUSHEYE sample: one of two of phenolic acids finger printing and saponins finger printing;
(5) comparison:
The finger printing of gained SHENQI FUZHENG ZHUSHEYE sample is compared with the reference fingerprint of SHENQI FUZHENG ZHUSHEYE respectively, and similarity is qualified products greater than 0.9 SHENQI FUZHENG ZHUSHEYE sample;
1. the phenolic acids finger printing under the 200-215nm: have 8 chromatographic peaks, with the retention time of the chromatographic peak of calycosin-7-O-β-D-pyranglucoside 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 time are 0.25-0.33, and relative peak area is 0.70-1.50; No. 3 peak relative retention time 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 time are 0.90-20, and relative peak area is 0.22-0.40; No. 5 peak relative retention time are 1.20-1.40, and relative peak area is 0.22-0.40; No. 6 peak relative retention time are 1.38-1.46, and relative peak area is 0.90-1.50; No. 7 peak relative retention time are 1.42-1.53, and relative peak area is 0.23-0.42;
2. the phenolic acids finger printing under the 250-280nm: have 6 chromatographic peaks, with the retention time of the chromatographic peak of calycosin-7-O-β-D-pyranglucoside 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 time are 0.25-0.33, and relative peak area is 1.25-2.50; No. 3 peak relative retention time 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 time are 0.33-0.40, and relative peak area is 0.50-1.30; No. 5 peak relative retention time 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 printing: have 9 chromatographic peaks, with the retention time of the chromatographic peak of astragaloside 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 time are 0.74-0.82, and relative peak area is 0.45-1.20; No. 3 peak relative retention time are 0.78-0.85, and relative peak area is 0.15-0.23; No. 4 peak relative retention time are 0.88-0.93, and relative peak area is 0.17-0.25; No. 5 peak relative retention time 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 time are 0.95-1.10, and relative peak area is 0.30-0.40; No. 7 peak relative retention time are 0.98-10, and relative peak area is 0.60-0.80; No. 8 peak relative retention time are 0.10-1.15, and relative peak area is 0.60-1.0.
In the method for the invention, the preparation method of phenolic acids finger printing test solution is preferably: the A method: precision is measured SHENQI FUZHENG ZHUSHEYE sample 25ml, put and be concentrated into 5ml in the water-bath, slowly by AB-8 macroporous adsorptive resins (internal diameter 1.5cm, long 20cm), water 70ml eluting discards eluent, reuse 70% ethanol 80ml eluting, collect eluent, put and be concentrated into driedly in the water-bath, residue adds water makes dissolving, be transferred in the 10ml measuring bottle, thin up shakes up to scale, with microporous filter membrane (water, 0.45 μ m) filter, promptly.
Or B method: precision is measured SHENQI FUZHENG ZHUSHEYE sample 25ml, with water saturated n-butanol extraction four times, and each 20ml, merge n-butyl alcohol liquid, leave standstill, after treating to clarify fully, discard residual water layer, n-butyl alcohol liquid is put and is concentrated into driedly in the water-bath, and residue adds water makes dissolving, be transferred in the 10ml measuring bottle, thin up shakes up to scale, with microporous filter membrane (water, 0.45 μ m) filter, promptly.
A, B method all can, the B method is more excellent.
The preparation method of saponins finger printing test solution is preferably:
The A method: precision is measured SHENQI FUZHENG ZHUSHEYE sample 200ml, puts and is concentrated into about 10ml in the water-bath, slowly by AB-8 macroporous adsorptive resins (internal diameter 1.5cm, long 20cm), water 70ml eluting discards eluent, reuse 70% ethanol 80ml eluting is collected eluent, put be concentrated in the water-bath dried, residue adds methanol makes dissolving, is transferred in the 5ml measuring bottle, adds methanol and is diluted to scale, shake up, filter with microporous filter membrane (organic facies, 0.45 μ m), as need testing solution.
Or B method: precision is measured SHENQI FUZHENG ZHUSHEYE sample 200ml, puts and is concentrated into about 20ml in the water-bath, with water saturated n-butanol extraction four times, each 25ml merges n-butyl alcohol liquid, uses twice of the saturated water washing of n-butyl alcohol, each 20ml, discard water layer, n-butyl alcohol liquid is put and is concentrated into driedly in the water-bath, and residue adds 80% dissolve with ethanol and is transferred in the 5ml measuring bottle, be diluted to scale, shake up, filter with 0.45 μ m microporous filter membrane, promptly.
A, B method all can, the B method is more excellent.
Step 2) preparation process of described reference substance solution is preferably: it is an amount of to get calycosin-7-O-β-D-pyranglucoside reference substance, adds methanol and makes the solution that contains 0.06mg in every 1ml solution, as the reference substance solution of phenolic acids finger printing; It is an amount of to get the astragaloside reference substance, adds methanol and makes the solution that contains 0.1mg in every 1ml solution, as the reference substance solution of saponins finger printing.
The step 3) chromatographic condition is preferably: chromatographic column is filler 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 in the saponins finger printing by calycosin-7-O-β-D-pyranglucoside in the phenolic acids finger printing.30 ℃ of column temperatures; The phenolic acids finger printing detects with UV-detector, and the detection wavelength is 208nm, 266nm; The saponins finger printing detects with evaporative light scattering detector, is mobile phase A with the second eyeball, is Mobile phase B with water, and the regulation in the according to the form below is carried out gradient elution;
| Time (minute) | Mobile phase A (%) | Mobile phase B (%) |
| 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 |
Step 4) high performance liquid chromatography testing process is preferably: accurate each 20 μ l of test solution that draw reference substance solution and SHENQI FUZHENG ZHUSHEYE sample, inject high performance liquid chromatograph, and be 70 minutes writing time.
Principle of the present invention is on the HPLC of the former SHENQI FUZHENG ZHUSHEYE of having set up finger printing basis, the preparation method of the test solution by improving the SHENQI FUZHENG ZHUSHEYE sample, obtain HPLC finger printing more accurate, reliable SHENQI FUZHENG ZHUSHEYE, thereby control the product quality of SHENQI FUZHENG ZHUSHEYE better, improve the safety of its stability and clinical use.The preparation method practicality of the test solution of the SHENQI FUZHENG ZHUSHEYE sample after the improvement is stronger.
Description of drawings
The standard finger-print of Fig. 1-3 SHENQI FUZHENG ZHUSHEYE (A method) (Fig. 1: phenolic acids reference fingerprint (266nm), Fig. 2: phenolic acids reference fingerprint (208nm), Fig. 3: saponins finger printing (ELSD));
Determining of Fig. 4 phenolic acids finger printing (208nm) S peak;
Determining of Fig. 5 phenolic acids finger printing (266nm) S peak;
Determining of Fig. 6 saponins finger printing S peak;
Fig. 7 A-Fig. 7 C is respectively Radix Astragali injection finger printing (Fig. 7 A: phenolic acids finger printing (208nm), Fig. 7 B: phenolic acids finger printing (266nm), Fig. 7 C: saponins finger printing (ELSD));
Fig. 8 A-Fig. 8 C is respectively Radix Salviae Miltiorrhizae drip liquid finger printing (Fig. 8 A: phenolic acids finger printing (208nm), Fig. 8 B: phenolic acids finger printing (266nm), Fig. 8 C: saponins finger printing (ELSD));
Fig. 9 A-Fig. 9 C is respectively SHENQI FUZHENG ZHUSHEYE finger printing (Fig. 9 A: phenolic acids finger printing (208nm), Fig. 9 B: phenolic acids finger printing (266nm), Fig. 9 C: saponins finger printing (ELSD));
Figure 10 A-Figure 10 C is respectively the comparison that SHENQI FUZHENG ZHUSHEYE A and B method make finger printing, wherein, upward be the A method, be B method (Figure 10 A: phenolic acids finger printing (266nm) down, Figure 10 B: phenolic acids finger printing (208nm), Figure 10 C: saponins finger printing (ELSD)).
The specific embodiment
The foundation of the standard finger-print of embodiment 1, SHENQI FUZHENG ZHUSHEYE (A method)
1, the preparation of standard testing solution
1. phenolic acids finger printing: precision is measured SHENQI FUZHENG ZHUSHEYE 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 eluting discards water elution liquid, continuous with 70% ethanol 80ml eluting, collect 70% ethanol elution, 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 microporous filter membrane, promptly.
2. saponins finger printing: precision is measured SHENQI FUZHENG ZHUSHEYE sample 200ml, puts and is concentrated into about 10ml in the water-bath, and slowly by AB-8 macroporous adsorptive resins (column internal diameter is 1.5cm, and column length is 20cm), water 80ml eluting discards water elution liquid; Continuous with 20% ethanol 80ml eluting, discard 20% ethanol elution; Reuse 80% ethanol 100ml eluting is collected 80% ethanol elution, puts to be concentrated into driedly in the water-bath, and 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 microporous filter membrane, promptly.
2, the preparation of reference substance solution
It is an amount of to get calycosin-7-O-β-D-pyranglucoside reference substance, adds methanol and makes the solution that contains 0.06mg in every 1ml solution, as the reference substance solution of phenolic acids finger printing; It is an amount of to get the astragaloside reference substance, adds methanol and makes the solution that contains 0.1mg in every 1ml solution, as the reference substance solution of saponins finger printing;
3, chromatographic condition
Chromatographic column is filler 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, the regulation in the according to the form below is carried out gradient elution; 30 ℃ of column temperatures; The phenolic acids finger printing detects with UV-detector, and the detection wavelength is 208nm, 266nm; The saponins finger printing detects with evaporative light scattering detector.Theoretical cam curve is not less than 3000, is not less than 4000 by astragaloside in the saponins finger printing by calycosin-7-O-β-D-pyranglucoside in the phenolic acids finger printing.
4, measure
Accurate standard testing solution and each 20 μ l of reference substance solution of drawing inject chromatograph of liquid respectively, write down 70 minutes chromatogram,, and calculate similarity that is.
5, determine total peak
1. the total peak of phenolic acids finger printing (208nm) is definite: set up phenolic acids finger printing (208nm), it is auxiliary detection to phenolic acids finger printing (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, and alternative is selected the bigger chromatographic peak of peak area and also classified total peak as.The chromatogram of contrast calycosin-7-O-β-D-pyranglucoside reference substance solution is selected the S peak, sees accompanying drawing 4.
Select 20 batches of SHENQI FUZHENG ZHUSHEYE (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 | 0601 01 | 0601 02 | 0601 03 | 0601 04 | 0601 05 | 0601 06 | 0601 07 | 0601 08 | 0601 09 | 0601 10 |
| Similarity | 0.98 6 | 0.98 6 | 0.98 0 | 0.98 9 | 0.98 5 | 0.96 3 | 0.99 4 | 0.99 0 | 0.99 1 | 0.96 6 |
| Lot number | 0601 1 | 0601 12 | 0602 13 | 0602 14 | 0602 15 | 0602 16 | 0602 17 | 0602 18 | 0602 19 | 0602 20 |
| Similarity | 0.96 6 | 0.99 5 | 0.98 7 | 0.99 1 | 0.98 8 | 0.99 0 | 0.99 3 | 0.99 5 | 0.99 3 | 0.99 3 |
In sum, the phenolic acids finger printing (208nm) of SHENQI FUZHENG ZHUSHEYE as shown in Figure 1.
2. the total peak of phenolic acids finger printing (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 repeatability 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-pyranglucoside reference substance solution is selected the S peak, sees accompanying drawing 5.
In similarity software, after total peak mated, it was as follows to calculate similarity result:
| Lot number | 0601 01 | 0601 02 | 0601 03 | 0601 04 | 0601 05 | 0601 06 | 0601 07 | 0601 08 | 0601 09 | 0601 10 |
| Similarity | 0.99 0 | 0.98 0 | 0.98 9 | 0.99 3 | 0.99 3 | 0.98 7 | 0.99 3 | 0.99 9 | 0.99 9 | 0.99 9 |
| Lot number | 0601 1 | 0601 12 | 0602 13 | 0602 14 | 0602 15 | 0602 16 | 0602 17 | 0602 18 | 0602 19 | 0602 20 |
| Similarity | 0.98 2 | 0.99 5 | 0.99 2 | 0.99 6 | 0.99 4 | 0.99 8 | 0.99 8 | 0.99 1 | 0.99 0 | 0.99 4 |
In sum, the phenolic acids finger printing (266nm) of SHENQI FUZHENG ZHUSHEYE as shown in Figure 2.
3. the total peak of saponins finger printing 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 reference substance solution is selected the S peak, sees accompanying drawing 6.
In similarity software, after total peak mated, it was as follows to calculate similarity result:
| Lot number | 0601 01 | 0601 02 | 0601 03 | 0601 04 | 0601 05 | 0601 06 | 0601 07 | 0601 08 | 0601 09 | 0601 10 |
| Similarity | 0.99 7 | 0.99 9 | 0.98 5 | 0.99 6 | 0.99 3 | 0.99 0 | 0.98 0 | 0.99 2 | 0.99 7 | 0.98 9 |
| Lot number | 0601 1 | 0601 12 | 0602 13 | 0602 14 | 0602 15 | 0602 16 | 0602 17 | 0602 18 | 0602 19 | 0602 20 |
| Similarity | 0.99 8 | 0.99 1 | 0.98 8 | 0.99 4 | 0.99 4 | 0.98 9 | 0.98 6 | 0.98 0 | 0.99 7 | 0.99 3 |
In sum, the saponins finger printing of SHENQI FUZHENG ZHUSHEYE as shown in Figure 3.
6, the repeatability of finger printing and stability experiment
1. phenolic acids finger printing (208nm):
Get SHENQI FUZHENG ZHUSHEYE 050815, press A method treatment samples test fluid, carried out stability, precision, reproducible methodology test.To its similarity result of calculation such as following table 1, table 2, table 3.
Table 1 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 2 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 3 repeatability 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 (A method) stability, precision, repeatability are good.
2. phenolic acids finger printing (266nm):
Get SHENQI FUZHENG ZHUSHEYE 050815, press A method treatment samples test fluid, carried out stability, precision, reproducible methodology test.To its similarity result of calculation such as following table 4, table 5, table 6.
Table 4 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 5 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 6 repeatability 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 (A method) stability, precision, repeatability are good.
3. saponins finger printing:
Get SHENQI FUZHENG ZHUSHEYE 050815, press A method treatment samples test fluid, carried out stability, precision, reproducible methodology test.To its similarity result of calculation such as following table 7, table 8, table 9.
Table 7 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 8 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 9 repeatability 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 (A method) stability, precision, repeatability are good.
The foundation of the standard finger-print of embodiment 2. SHENQI FUZHENG ZHUSHEYE (B method)
1, the preparation of standard testing solution
(1) specimen of phenolic acids finger printing: precision is measured SHENQI FUZHENG ZHUSHEYE sample 25ml, with water saturated n-butanol extraction four times, and each 20ml, merge n-butyl alcohol liquid, leave standstill, after treating to clarify fully, discard residual water layer, n-butyl alcohol liquid is put and is concentrated into driedly in the water-bath, and residue adds water makes dissolving, be transferred in the 10ml measuring bottle, thin up shakes up to scale, with microporous filter membrane (water, 0.45 μ m) filter, promptly.
(2) specimen of saponins finger printing: precision is measured SHENQI FUZHENG ZHUSHEYE sample 200ml, puts and is concentrated into about 20ml in the water-bath, with water saturated n-butanol extraction four times, each 25ml merges n-butyl alcohol liquid, uses twice of the saturated water washing of n-butyl alcohol, each 20ml, discard water layer, n-butyl alcohol liquid is put and is concentrated into driedly in the water-bath, and residue adds 80% dissolve with ethanol and is transferred in the 5ml measuring bottle, be diluted to scale, shake up, filter with 0.45 μ m microporous filter membrane, promptly.
2, the preparation of reference substance solution
It is an amount of to get calycosin-7-O-β-D-pyranglucoside reference substance, adds methanol and makes the solution that contains 0.06mg in every 1ml solution, as the reference substance solution of phenolic acids finger printing; It is an amount of to get the astragaloside reference substance, adds methanol and makes the solution that contains 0.1mg in every 1ml solution, as the reference substance solution of saponins finger printing;
3, chromatographic condition
Chromatographic column is filler with the octadecylsilane chemically bonded silica, and model is Discovery C18,250 * 4.6mm, and 5 μ m are mobile phase A with the second eyeball, are Mobile phase B with water, the gradient of according to the form below is carried out gradient elution; 30 ℃ of column temperatures; The phenolic acids finger printing detects with UV-detector, and the detection wavelength is 208nm, 266nm; The saponins finger printing detects with evaporative light scattering detector.Theoretical cam curve is not less than 3000, is not less than 4000 by astragaloside in the saponins finger printing by calycosin-7-O-β-D-pyranglucoside in the phenolic acids finger printing.
| Time (minute) | Mobile phase A (%) | Mobile phase B (%) |
| 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, measure
Accurate standard testing solution and each 20 μ l of reference substance solution of drawing inject chromatograph of liquid respectively, write down 70 minutes chromatogram,, and calculate similarity that is.
5, determine total peak
1. the total peak of phenolic acids finger printing (208nm) is definite: set up phenolic acids finger printing (208nm), it is auxiliary detection to phenolic acids finger printing (266nm), can detect detect at 266nm wavelength place less than composition, mainly concentrate in 35～50 minutes, so 4,5,6,7 more stable in this section chromatographic peaks are all listed in the total peak, and 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-pyranglucoside reference substance solution is selected the S peak, sees Fig. 4.
Select 20 batches of SHENQI FUZHENG ZHUSHEYE (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 | 051041 | 051042 | 051043 | 051046 | 051047 | 051048 | 051049 | 060464 | 060466 | 060467 |
| Similarity | 0.967 | 0.978 | 0.974 | 0.983 | 0.974 | 0.981 | 0.977 | 0.985 | 0.980 | 0.983 |
| Lot number | 060468 | 060470 | 060471 | 060472 | 061009 | 061010 | 061013 | 061016 | 0701002 | 0701008 |
| Similarity | 0.982 | 0.984 | 0.986 | 0.981 | 0.980 | 0.977 | 0.979 | 0.983 | 0.979 | 0.959 |
2. the total peak of phenolic acids finger printing (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 repeatability 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-pyranglucoside 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 | 051041 | 051042 | 051043 | 051046 | 051047 | 051048 | 051049 | 060464 | 060466 | 060467 |
| Similarity | 0.974 | 0.976 | 0.979 | 0.985 | 0.977 | 0.986 | 0.981 | 0.986 | 0.985 | 0.986 |
| Lot number | 060468 | 060470 | 060471 | 060472 | 061009 | 061010 | 061013 | 061016 | 0701002 | 0701008 |
| Similarity | 0.980 | 0.986 | 0.987 | 0.984 | 0.979 | 0.980 | 0.984 | 0.986 | 0.981 | 0.957 |
3. the total peak of saponins finger printing 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 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 | 051041 | 051042 | 051043 | 051046 | 051047 | 051048 | 051049 | 060464 | 060466 | 060467 |
| Similarity | 0.977 | 0.973 | 0.976 | 0.983 | 0.982 | 0.982 | 0.984 | 0.991 | 0.981 | 0.980 |
| Lot number | 060468 | 060470 | 060471 | 060472 | 061009 | 061010 | 061013 | 061016 | 0701002 | 0701008 |
| Similarity | 0.976 | 0.983 | 0.986 | 0.987 | 0.974 | 0.975 | 0.979 | 0.983 | 0.984 | 0.961 |
6, the repeatability of finger printing and stability experiment
1. phenolic acids finger printing (208nm):
Get 0701002 batch of SHENQI FUZHENG ZHUSHEYE, carried out stability, precision, reproducible methodology test.To its similarity result of calculation such as following table 10, table 11, table 12.
Table 10 stability test similarity result of calculation table
| 0hr | 3hr | 6hr | 12hr | 18hr | RSD | |
| Similarity | 0.985 | 0.984 | 0.987 | 0.985 | 0.986 | 0.12％ |
Table 11 precision test similarity result of calculation table
| 1 | 2 | 3 | 4 | 5 | 6 | RSD | |
| Similarity | 0.985 | 0.984 | 0.986 | 0.983 | 0.984 | 0.983 | 0.12％ |
Table 12 repeatability test similarity result of calculation table
| 1 | 2 | 3 | 4 | 5 | 6 | RSD | |
| Similarity | 0.964 | 0.981 | 0.986 | 0.973 | 0.961 | 0.966 | 1.09％ |
The result shows: this method stability, precision, repeatability are good.
2. phenolic acids finger printing (266nm):
Get 0701002 batch of SHENQI FUZHENG ZHUSHEYE, carried out stability, precision, reproducible methodology test.To its similarity result of calculation such as following table 13, table 14, table 15.
Table 13 stability test similarity result of calculation table
| 0hr | 3hr | 6hr | 12hr | 18hr | RSD | |
| Similarity | 0.984 | 0.984 | 0.984 | 0.986 | 0.985 | 0.09％ |
Table 14 precision test similarity result of calculation table
| 1 | 2 | 3 | 4 | 5 | 6 | RSD | |
| Similarity | 0.984 | 0.984 | 0.984 | 0.984 | 0.984 | 0.984 | 0％ |
Table 15 repeatability test similarity result of calculation table
| 1 | 2 | 3 | 4 | 5 | 6 | RSD | |
| Similarity | 0.961 | 0.984 | 0.984 | 0.969 | 0.958 | 0.963 | 1.19％ |
The result shows: adopt the B method, method stability, precision, repeatability are good.
3. saponins finger printing:
Get 0701002 batch of SHENQI FUZHENG ZHUSHEYE, carried out stability, precision, reproducible methodology test.To its a similarity result of calculation such as a following table 16, table 17, table 18.
Table 16 stability test similarity result of calculation table
| 0hr | 3hr | 6hr | 12hr | 18hr | RSD | |
| Similarity | 0.986 | 0.985 | 0.983 | 0.986 | 0.987 | 0.15％ |
Table 17 precision test similarity result of calculation table
| 1 | 2 | 3 | 4 | 5 | 6 | RSD |
| Similarity | 0.985 | 0.985 | 0.986 | 0.985 | 0.985 | 0.985 | 0％ |
Table 18 repeatability test similarity result of calculation table
| 1 | 2 | 3 | 4 | 5 | 6 | RSD | |
| Similarity | 0.977 | 0.983 | 0.987 | 0.971 | 0.961 | 0.964 | 1.05％ |
The result shows: adopt the B method, method stability, precision, repeatability are good.
Choose commercially available Radix Astragali injection, Radix Salviae Miltiorrhizae drip liquid, SHENQI FUZHENG ZHUSHEYE, A method according to embodiment 1 is measured its finger printing, compare with standard finger-print, similarity greater than 0.9 be SHENQI FUZHENG ZHUSHEYE, remaining all is lower than 0.9, can be used for differentiating the true and false of SHENQI FUZHENG ZHUSHEYE.
Radix Astragali injection:
As Fig. 7 A one Fig. 7 C, its similarity is respectively 0.409,0.315,0.611 respectively for the phenolic acids finger printing of 208nm, 266nm and saponins finger printing.
Radix Salviae Miltiorrhizae drip liquid:
As Fig. 8 A one Fig. 8 C, its similarity is respectively 0.292,0.257,0.000 respectively for the phenolic acids finger printing of 208nm, 266nm and saponins finger printing.
SHENQI FUZHENG ZHUSHEYE:
As Fig. 9 A one Fig. 9 C, its similarity is respectively 0.983,0.985,0.981 respectively for the phenolic acids finger printing of 208nm, 266nm and saponins finger printing.
Many batches of commercially available SHENQI FUZHENG ZHUSHEYE are measured its finger printing 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.
Get 060470 batch of SHENQI FUZHENG ZHUSHEYE, make test fluid by A method and B method respectively, detect by above-mentioned testing conditions, obtain the 208nml collection of illustrative plates respectively, 266nm collection of illustrative plates and ELSD collection of illustrative plates are seen attached Figure 10 A-10C.Carry out the contrast of A method and B method collection of illustrative plates similarity respectively, the result is respectively: 0.988 (208nml collection of illustrative plates), 0.991 (266nm collection of illustrative plates) and 0.986 (ELSD collection of illustrative plates).The result shows that the collection of illustrative plates that A method and B method make is basic identical, but the discovery that studies for a long period of time, the A method is subjected to the different influence of different batches resin absorption performance to cause testing result to differ greatly sometimes, and the B method is more stable, so preferred B method.
Claims (8)
1, a kind of method of quality control of SHENQI FUZHENG ZHUSHEYE comprises the steps:
(1) test solution of preparation SHENQI FUZHENG ZHUSHEYE sample, described test solution comprises phenolic acids finger printing test fluid and saponins finger printing test fluid, the concrete preparation method of described test solution comprises the operating procedure that is selected from following A method or B method:
The A method: macroporous adsorptive resins is passed through in the legal concentrated back of SHENQI FUZHENG ZHUSHEYE sample, first water eluting, the reuse ethanol elution, the collection ethanol elution is concentrated into dried, and residue adds water or dissolve with ethanol, gets the test fluid of SHENQI FUZHENG ZHUSHEYE sample;
Or B method: with the saturated n-butanol extraction of SHENQI FUZHENG ZHUSHEYE sample, n-butyl alcohol liquid is concentrated into dried, residue additive polarity dissolution with solvents dilution filters with microporous membrane, obtains the test solution of SHENQI FUZHENG ZHUSHEYE sample;
(2) preparation of reference substance solution:
Calycosin-7-O-β-D-pyranglucoside reference substance is dissolved in methanol, as the reference substance solution of phenolic acids finger printing; The astragaloside reference substance is dissolved in methanol, as the reference substance solution of saponins finger printing;
(3) chromatographic condition
Chromatographic column is filler with the octadecylsilane chemically bonded silica; Second eyeball one water is mobile phase, gradient elution; Detect phenolic acids finger printing under 200-215nm and the 250-280nm respectively with UV-detector; Detect the saponins finger printing with evaporative light scattering detector;
(4) high performance liquid chromatography detects:
Get the test solution and the reference substance solution of the SHENQI FUZHENG ZHUSHEYE sample that A method or B method make, inject high performance liquid chromatograph, carry out high performance liquid chromatography and detect, obtain three of the finger printing of SHENQI FUZHENG ZHUSHEYE sample: one of two of phenolic acids finger printing and saponins finger printing;
(5) comparison:
The finger printing of gained SHENQI FUZHENG ZHUSHEYE sample is compared with the reference fingerprint of SHENQI FUZHENG ZHUSHEYE respectively, and similarity is qualified products greater than 0.9 SHENQI FUZHENG ZHUSHEYE sample;
1. the phenolic acids finger printing under the 200-215nm: have 8 chromatographic peaks, with the retention time of the chromatographic peak of calycosin-7-O-β-D-pyranglucoside 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 time are 0.25-0.33, and relative peak area is 0.70-1.50; No. 3 peak relative retention time 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 time are 0.90-20, and relative peak area is 0.22-0.40; No. 5 peak relative retention time are 1.20-1.40, and relative peak area is 0.22-0.40; No. 6 peak relative retention time are 1.38-1.46, and relative peak area is 0.90-1.50; No. 7 peak relative retention time are 1.42-1.53, and relative peak area is 0.23-0.42;
2. the phenolic acids finger printing under the 250-280nm: have 6 chromatographic peaks, with the retention time of the chromatographic peak of calycosin-7-O-β-D-pyranglucoside 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 time are 0.25-0.33, and relative peak area is 1.25-2.50; No. 3 peak relative retention time 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 time are 0.33-0.40, and relative peak area is 0.50-1.30; No. 5 peak relative retention time 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 printing: have 9 chromatographic peaks, with the retention time of the chromatographic peak of astragaloside 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 time are 0.74-0.82, and relative peak area is 0.45-1.20; No. 3 peak relative retention time are 0.78-0.85, and relative peak area is 0.15-0.23; No. 4 peak relative retention time are 0.88-0.93, and relative peak area is 0.17-0.25; No. 5 peak relative retention time 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 time are 0.95-1.10, and relative peak area is 0.30-0.40; No. 7 peak relative retention time are 0.98-10, and relative peak area is 0.60-0.80; No. 8 peak relative retention time 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 method of phenolic acids finger printing test solution is: the A method: precision is measured SHENQI FUZHENG ZHUSHEYE sample 25ml, put and be concentrated into 5ml in the water-bath, slowly by AB-8 macroporous adsorptive resins (internal diameter 1.5cm, long 20cm), water 70ml eluting discards eluent, reuse 70% ethanol 80ml eluting, collect eluent, put and be concentrated into driedly in the water-bath, residue adds water makes dissolving, be transferred in the 10ml measuring bottle, thin up shakes up to scale, with microporous filter membrane (water, 0.45 μ m) filter, promptly;
Or B method: precision is measured SHENQI FUZHENG ZHUSHEYE sample 25ml, with water saturated n-butanol extraction four times, and each 20ml, merge n-butyl alcohol liquid, leave standstill, after treating to clarify fully, discard residual water layer, n-butyl alcohol liquid is put and is concentrated into driedly in the water-bath, and residue adds water makes dissolving, be transferred in the 10ml measuring bottle, thin up shakes up to scale, with microporous filter membrane (water, 0.45 μ m) filter, promptly.
3, according to method according to claim 2, A, B method all can, preferred B method.
4, method according to claim 1, it is characterized in that: the preparation method of saponins finger printing test solution is: the A method: precision is measured SHENQI FUZHENG ZHUSHEYE sample 200ml, put and be concentrated into about 10ml in the water-bath, slowly by AB-8 macroporous adsorptive resins (internal diameter 1.5cm, long 20cm), water 70ml eluting discards eluent, reuse 70% ethanol 80ml eluting, collect eluent, put and be concentrated into driedly in the water-bath, residue adds methanol makes dissolving, be transferred in the 5ml measuring bottle, add methanol and be diluted to scale, shake up, with microporous filter membrane (organic facies, 0.45 μ m) filter, as need testing solution;
Or B method: precision is measured SHENQI FUZHENG ZHUSHEYE sample 200ml, puts and is concentrated into about 20ml in the water-bath, with water saturated n-butanol extraction four times, each 25ml merges n-butyl alcohol liquid, uses twice of the saturated water washing of n-butyl alcohol, each 20ml, discard water layer, n-butyl alcohol liquid is put and is concentrated into driedly in the water-bath, and residue adds 80% dissolve with ethanol and is transferred in the 5ml measuring bottle, be diluted to scale, shake up, filter with 0.45 μ m microporous filter membrane, promptly.
5, according to method according to claim 4, A, B method all can, preferred B method.
6, according to any one described method among the claim 1-5, 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-pyranglucoside reference substance, add methanol and make the solution that contains 0.06mg in every 1ml solution, as the reference substance solution of phenolic acids finger printing; It is an amount of to get the astragaloside reference substance, adds methanol and makes the solution that contains 0.1mg in every 1ml solution, as the reference substance solution of saponins finger printing.
7, according to any one described method among the claim 1-6, it is characterized in that: the chromatographic condition of step (3) is: chromatographic column is filler with the octadecylsilane chemically bonded silica, model is DiscoveryC18,250 * 4.6mm, 5 μ m, theoretical cam curve is not less than 3000, is not less than 4000 by astragaloside in the saponins finger printing by calycosin-7-O-β-D-pyranglucoside in the phenolic acids finger printing.30 ℃ of column temperatures; The phenolic acids finger printing detects with UV-detector, and the detection wavelength is 208nm, 266nm; The saponins finger printing detects with evaporative light scattering detector, is that mobile phase is carried out gradient elution with second eyeball-water, and the gradient of gradient elution is as follows:
Time (minute) mobile phase A (%) Mobile phase B (%)
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
。
8, according to any one described method among the claim 1-7, it is characterized in that: step (4) high performance liquid chromatography testing process is: accurate each 20 μ l of test solution that draw reference substance solution and SHENQI FUZHENG ZHUSHEYE sample, inject high performance liquid chromatograph, be 70 minutes writing time.
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