CN103245746A - Multi-component process dynamic quality control testing method for injection containing marsdenia tenocissima - Google Patents
Multi-component process dynamic quality control testing method for injection containing marsdenia tenocissima Download PDFInfo
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Abstract
The invention belongs to the field of methodology for studying traditional Chinese medicine preparations, and relates to a multi-component process dynamic quality control testing method for an injection containing marsdenia tenocissima. The method is specifically used for testing and controlling a marsdenia tenocissima herb, an intermediate applied to the process of preparing the injection containing marsdenia tenocissima, and phenolic acid, steroidal saponins and saccharides in the finished injection containing marsdenia tenocissima. When the content sum of the phenolic acid, the steroidal saponins and the saccharides is more than the content of total solids by 50 percent to 95 percent, the content ratio of the phenolic acid to the steroidal saponins to the saccharides is (1 percent-95 percent):(1 percent-95 percent): (1 percent-95 percent); and when the total content of the phenolic acid and the steroidal saponins is not less than 0 percent to 85 percent, the quality of the injection containing marsdenia tenocissima is best. The method overcomes the problem that in a traditional quality control method, only maker components of a finished product are taken into consideration, but the influence of other links of a preparing technological process to product quality is ignored, and the method can effectively improve the quality controllability of traditional Chinese medicine preparations and reduce the content difference of preparation components from batch to batch.
Description
Technical field
The present invention relates to a kind of CAULIS MARSDENIAE TENACISSIMAE parenteral solution polycomponent process dynamic mass control detection method that contains, belong to traditional Chinese medicine preparation research methodology field.
Background technology
The quality control of Chinese medicine preparation is a major issue of paying close attention on the internationalization of tcm road for development always.The complicacy characteristics of traditional Chinese medicine ingredients allow and realize that preparation quality is stable, controlled Chinese medicine preparation has been absorbed in deadlock, also is that Chinese medicine preparation is difficult to by the key issue of international endorsement.Current Chinese medicine/Chinese medicine preparation quality relies on one or several one-tenth of detection to assign to judge that the method for quality good or not can not satisfy international development to the requirement of Chinese medicine.The Chinese medicine of international endorsement must be that curative effect is stable, quality controllable modernized Chinese medicine/Chinese medicine preparation.In the industrialization production run of modern Chinese herbal medicine preparation, enterprise payes attention to the quality of last preparation finished product often singlely, and the error of having ignored in the preparation production run causes the preparation end product quality to be difficult to control.To such an extent as to more can't estimate the process procedure that causes the Chinese medicine preparation quality error.This makes that the Chinese medicine preparation finished medicines heterodyne of each batch of enterprise is different obviously, even substandard product in batch occurs, and enterprise haves no alternative but cause recalling or destroying large quantities of Chinese medicine preparations.The applicant thinks that each link quality control of Chinese medicine preparation production technology all should cause concern, in this complex system of Chinese medicine, only accomplishes to monitor step by step, could guarantee that the finished product of producing at last is quality controllable, and curative effect is stable.The Chinese medicine preparation polycomponent process dynamic mass control that the applicant proposes detects, it is the monitoring from the source medicinal material to the whole process of preparation finished product to Chinese medicine preparation, adopt polycomponent process dynamic mass control model can control the quality that Chinese medicine preparation prepares each link intermediate, when gross error occurring, can in time find the preparation process of makeing mistakes, and analyze reason and in time handle.Realize the quality control of production run and finished product, such pattern can effectively improve the quality controllability of Chinese medicine preparation, the content difference of preparation composition between reducing batch, thus improve the stability of Chinese medicine preparation curative effect.Be expected to solve the control of Chinese medicine preparation difficult quality, the tangible problem of curative effect difference is to reach the standard that internationalization is produced.
Containing the CAULIS MARSDENIAE TENACISSIMAE parenteral solution is prepared from Marsdenia tenacissima extract, be used for the treatment of cancer of the esophagus liver cancer cancer of the stomach etc. clinically, has good efficacy, and it is all harmless to the heart, liver, kidney and hemopoietic system, toxic and side effect is little, and have protect the liver, Li Shui and recovery is put, the effect of blood picture after the chemotherapy, be a kind of up-and-coming Chinese herbal medicine for preventing.CAULIS MARSDENIAE TENACISSIMAE another name Herba seu Radix Metaplexis hemsleyanae, Rajmahal creeper, exceedingly high loose etc., dry stem, rattan, root, leaf for Asclepiadaceae milk Lepidium plant CAULIS MARSDENIAE TENACISSIMAE Marsdeniatenocissima (Roxb.) WightetArn, beginning is stated from " south, top book on Chinese herbal medicine ", the nature and flavor hardship, be slightly cold, have clearing heat and detoxicating, relieving cough and asthma, eliminating stagnation to stop pain, adjusting immunologic function, protect the liver diuresis, step-down, anticancer etc. effect relieves internal heat.Contain the CAULIS MARSDENIAE TENACISSIMAE parenteral solution and contain phenolic acid class component such as gallic acid, coumaric acid, Cryptochlorogenic acid, neochlorogenic acid, vanillic acid, chlorogenic acid, syringic acid, forulic acid etc.; Steroid saponin such as CAULIS MARSDENIAE TENACISSIMAE glycosides A, CAULIS MARSDENIAE TENACISSIMAE glycosides F, 17 β CAULIS MARSDENIAE TENACISSIMAE aglycon B, CAULIS MARSDENIAE TENACISSIMAE aglycon B etc.; Carbohydrate components fructose, glucose, oleandrose etc.At present, the quality control that contains the CAULIS MARSDENIAE TENACISSIMAE parenteral solution is only limited to control the content of phenolic acid compositions such as chlorogenic acid, and steroidal composition and carbohydrate content are embodiment.In addition, Quality Control is also only to final finished product, and production run is all out in the cold.The present invention is for controlling the quality that contains the CAULIS MARSDENIAE TENACISSIMAE parenteral solution more comprehensively, the process dynamic mass control method (Fig. 1) of foundation from CAULIS MARSDENIAE TENACISSIMAE medicinal material, intermediate to final finished parenteral solution effective substance phenolic acid, steroidal, carbohydrate components contains the quality of CAULIS MARSDENIAE TENACISSIMAE parenteral solution and enhances one's market competitiveness raising and have great importance.
Summary of the invention
Goal of the invention:
Problem to be solved by this invention is to overcome the existing deficiency that contains the quality control of CAULIS MARSDENIAE TENACISSIMAE parenteral solution, provides a kind of and contains intermediate the CAULIS MARSDENIAE TENACISSIMAE parenteral solution process to the dynamic phenolic acid of polycomponent process that contains the CAULIS MARSDENIAE TENACISSIMAE parenteral solution, steroid saponin, the carbohydrate components quality control detection method of finished product from CAULIS MARSDENIAE TENACISSIMAE medicinal material, preparation.
Technical scheme:
Of the present invention to containing the polycomponent process dynamic mass control detection method of CAULIS MARSDENIAE TENACISSIMAE parenteral solution, be specially the CAULIS MARSDENIAE TENACISSIMAE medicinal material, preparation contains the intermediate in the CAULIS MARSDENIAE TENACISSIMAE parenteral solution process, phenolic acid, steroid saponin, the carbohydrate that contains in the CAULIS MARSDENIAE TENACISSIMAE parenteral solution finished product detects control;
The main chemical compositions of described phenolic acid is gallic acid, coumaric acid, Cryptochlorogenic acid, neochlorogenic acid, vanillic acid, chlorogenic acid, syringic acid, forulic acid etc., its method of quality control is measured with high-efficient liquid phase technique, and reference substance is selected from 3～8 in gallic acid, coumaric acid, Cryptochlorogenic acid, neochlorogenic acid, vanillic acid, chlorogenic acid, syringic acid, the forulic acid;
The main chemical compositions of described steroid saponin is CAULIS MARSDENIAE TENACISSIMAE glycosides A, CAULIS MARSDENIAE TENACISSIMAE glycosides F, 17 β CAULIS MARSDENIAE TENACISSIMAE aglycon B, CAULIS MARSDENIAE TENACISSIMAE aglycon B etc., its method of quality control is measured with high-efficient liquid phase technique, and reference substance is selected from one or more among CAULIS MARSDENIAE TENACISSIMAE glycosides A, CAULIS MARSDENIAE TENACISSIMAE glycosides F, 17 β CAULIS MARSDENIAE TENACISSIMAE aglycon B, the CAULIS MARSDENIAE TENACISSIMAE aglycon B;
Described carbohydrate is mainly fructose, glucose, oleandrose etc., and its method of quality control PMP pre-column derivatization sugar finger-print, reference substance are selected from one or more in fructose, glucose, the oleandrose;
The content summation of described phenolic acid, steroid saponin, carbohydrate components is greater than the 50%-95% of total solid, it forms structure is phenolic acid than scope: steroid saponin: carbohydrate=(1%-95%): (1%-95%): (1%-95%), wherein phenolic acid and steroid saponin component total content are not less than 0%-85%.
Beneficial effect:
The preparation of traditional Chinese medicine preparation product relates to a plurality of links, as starting material, preparation process, refining purifying etc., and contains various ingredients, is its safe and effective important assurance to its quality control how.Chinese medicine derives from natural products, is subjected to the influence of different physical environments such as the place of production, season, picking time, physiological environment, thereby the strain of Chinese crude drug, quality discrepancy are very big.Chinese medicine preparation is to feed intake with crude drug in addition, in the preparation technical process because solvent, heating and each other influence, make the chemical constitution in the Chinese crude drug that various dynamic changes take place, cause the repeatability of the instability of present Chinese patent drug product quality and clinical efficacy poor.Because the limitation of factors such as the complicacy of Chinese medicine itself, scientific and technical condition, research ideas and methods, have the comprehensive inadequately of traditional Chinese medicine quality standard now, be difficult to confirm result for the treatment of and traditional Chinese medicine quality correlativity, and make traditional Chinese medicine quality can not obtain fine evaluation and control.Medicine is produced rather than is tested out, it is particularly crucial to carry out in the production run control of overall process dynamic mass, therefore, expect that from former the multi-level dynamically overall process of product carries out quality control, i.e. Chinese crude drug, Chinese medicine intermediate (Chinese medicine preparation raw material), finished product.Measure the CAULIS MARSDENIAE TENACISSIMAE medicinal material among the present invention, produce intermediate, finished product and carry out component structure and analyze to determine the quality controllable and stable and controllable in the production run, to obtain the whole finished product of steady quality homogeneous.The present invention has effectively improved the quality of product for the Quality Control that contains the CAULIS MARSDENIAE TENACISSIMAE parenteral solution provides the quality control new model of producing many components process detection of dynamic, provides reliable detection method for control contains CAULIS MARSDENIAE TENACISSIMAE parenteral solution quality.
Description of drawings
Phenolic acid, steroid saponin, each component dynamic change trend figure of carbohydrate in Fig. 1 CAULIS MARSDENIAE TENACISSIMAE medicinal material, intermediate, the parenteral solution
Fig. 2 contains the polycomponent process dynamic mass control method of CAULIS MARSDENIAE TENACISSIMAE parenteral solution
Fig. 3 CAULIS MARSDENIAE TENACISSIMAE phenolic acid HPLC fingerprint image spectrogram, (wherein 1, gallic acid 2, forulic acid 3, chlorogenic acid 4, Cryptochlorogenic acid 5, neochlorogenic acid 6, coumaric acid 7, vanillic acid 8, syringic acid)
Fig. 4 CAULIS MARSDENIAE TENACISSIMAE steroid saponin component HPLC chromatogram (wherein 9, CAULIS MARSDENIAE TENACISSIMAE glycosides F10, CAULIS MARSDENIAE TENACISSIMAE glycosides A11,17 β CAULIS MARSDENIAE TENACISSIMAE aglycon B12, CAULIS MARSDENIAE TENACISSIMAE aglycon B)
Fig. 5 PMP pre-column derivatization sugar finger-print (wherein 13, fructose 14, glucose 15, oleandrose)
Fig. 6 different batches CAULIS MARSDENIAE TENACISSIMAE medicinal material steroid saponin finger-print
Fig. 7 different batches CAULIS MARSDENIAE TENACISSIMAE phenolic acid finger-print
The preparation of Fig. 8 different batches contains the interior steroid saponin finger-print of intermediate of CAULIS MARSDENIAE TENACISSIMAE parenteral solution
The preparation of Fig. 9 different batches contains the interior phenolic acid finger-print of intermediate of CAULIS MARSDENIAE TENACISSIMAE parenteral solution
Figure 10 different batches contains CAULIS MARSDENIAE TENACISSIMAE parenteral solution steroid saponin finger-print
Figure 11 different batches contains CAULIS MARSDENIAE TENACISSIMAE parenteral solution phenolic acid finger-print
Embodiment
Embodiment
Fig. 2 is the polycomponent process dynamic mass control method that contains the CAULIS MARSDENIAE TENACISSIMAE parenteral solution, and its concrete steps are:
1, CAULIS MARSDENIAE TENACISSIMAE medicinal material extract
Dry CAULIS MARSDENIAE TENACISSIMAE medicinal material with different batches, comminutor is smashed, cross 40 mesh sieves, precision takes by weighing powder 100g, adds the water of 8 times of amounts, put in the round-bottomed flask and decoct 2h/ time, decoct twice, with filtered through gauze, merging filtrate, 70 ° of C are concentrated into 1g crude drug/ml concentration in the Rotary Evaporators, and-4 ° of C preserve standby.
2, preparation contains the preparation of the intermediate (hereinafter to be referred as intermediate) in the CAULIS MARSDENIAE TENACISSIMAE parenteral solution process
With medicinal substances extract, add ethanol, make to contain the alcohol amount and reach 75%, fully stir, leave standstill, filter; Sediment is added dissolved in distilled water, add ethanol again, carry out the secondary alcohol precipitation, make the alcohol amount of containing reach 75% depositing in water, fully stir, leave standstill, filter.
3, contain the preparation of CAULIS MARSDENIAE TENACISSIMAE parenteral solution finished product (hereinafter to be referred as parenteral solution)
Precipitation with filter obtaining adds 100 times of dissolved in distilled water, crosses hollow fiber column ultrafilter (molecular cut off 5000-100000), transfers pH6.5-7.2, filters, and filtrate adds 0.1% activated charcoal and boils 15min, cools off, and is filtered to clear and brightly, sterilizes gland after the packing.
4, phenolic content condition determination
Phenolic acid component in CAULIS MARSDENIAE TENACISSIMAE medicinal material, intermediate, the parenteral solution is carried out qualitative, quantitative to be characterized.The HPLC chromatogram is seen Fig. 3, Fig. 7, Fig. 9 and Figure 11.
1. instrument and reagent
High performance liquid chromatograph Agilent1200Series series (quaternary pump, online vacuum outgas system, automatic sampler, column oven, DAD detecting device), Agilent Chem Station chem workstation).
Reference substance: gallic acid, coumaric acid, Cryptochlorogenic acid, neochlorogenic acid, vanillic acid, chlorogenic acid, syringic acid, forulic acid are available from Nat'l Pharmaceutical ﹠ Biological Products Control Institute, and purity is all greater than 98%.
Acetonitrile (chromatographically pure, U.S. TEDIA company), Milli-Q ultrapure water.All the other reagent are pure for analyzing.
2. chromatographic condition
Agilent ZORBAX SB-C18 chromatographic column (4.6mm * 250mm, 5 μ m), flowing is acetonitrile (A)-0.1% formic acid mutually, gradient elution: 0-10min, 2%A-2%A; 10-20min, 2%A-15%A; 20-42min, 15%A-30%A.Flow velocity 1ml/min; Sample size 10 μ l; 30 ° of C of column temperature; Detect wavelength 242nm; Analysis time 42min.
3. the configuration of reference substance solution
Precision takes by weighing reference substance gallic acid, coumaric acid, Cryptochlorogenic acid, neochlorogenic acid, vanillic acid, chlorogenic acid, syringic acid, forulic acid, place the brown volumetric flask of 10ml, add the dissolving of chromatographically pure methyl alcohol, and being settled to 10ml, each reference substance concentration is followed successively by 57.44 μ g/ml, 86.33 μ g/ml, 43.06 μ g/ml, 104.76 μ g/ml, 65.98 μ g/ml, 110.66 μ g/ml, 74.56 μ g/ml, 64.45 μ g/ml.Respectively getting 1ml mixes to such an extent that mix reference substance solution.The typical curve of gallic acid, coumaric acid, Cryptochlorogenic acid, neochlorogenic acid, vanillic acid, chlorogenic acid, syringic acid, forulic acid is respectively: y=10.1878x+19.853(R
2=0.9999), y=40.249x-143.23(R
2=0.9996), y=30.853x-8.5178 (R
2=0.9998), y=30.019x+10.5342 (R
2=0.9999), y=19.727x-5.5673 (R
2=0.9999), y=20.445x-4.5371 (R
2=0.9998), y=40.773x+8.0462 (R2
=0.9997), y=25.653x-10.9375 (R
2=0.9999).
4. each phenolic acid component content of sample is measured
Different batches CAULIS MARSDENIAE TENACISSIMAE medicinal substances extract, intermediate, parenteral solution are crossed 0.45 μ m filter membrane respectively, precision is drawn each 10 μ l of need testing solution respectively, inject liquid chromatograph, the total content of decibel measurement gallic acid, coumaric acid, Cryptochlorogenic acid, neochlorogenic acid, vanillic acid, chlorogenic acid, syringic acid, forulic acid the results are shown in Table 1.
5, steroid saponin component qualitative, quantitative characterizes
Steroid saponin component in CAULIS MARSDENIAE TENACISSIMAE medicinal material, intermediate, the parenteral solution is carried out qualitative, quantitative to be characterized.The HPLC chromatogram is seen Fig. 4, Fig. 6, Fig. 8 and Figure 10.
1. instrument and reagent
High performance liquid chromatograph Agilent1200Series series (quaternary pump, online vacuum outgas system, automatic sampler, column oven, DAD detecting device), Agilent Chem Station chem workstation).
Reference substance: CAULIS MARSDENIAE TENACISSIMAE glycosides A, CAULIS MARSDENIAE TENACISSIMAE glycosides F, CAULIS MARSDENIAE TENACISSIMAE aglycon B are available from Nat'l Pharmaceutical ﹠ Biological Products Control Institute, and purity is all greater than 98%.17 β CAULIS MARSDENIAE TENACISSIMAE aglycon B are self-control, and purity is greater than 98%.
Acetonitrile (chromatographically pure, U.S. TEDIA company), Milli-Q ultrapure water.All the other reagent are pure for analyzing.
2. chromatographic condition
Agilent ZORBAX SB-C18 chromatographic column (4.6mm * 250mm, 5 μ m), flowing is acetonitrile (A)-0.1% formic acid mutually, gradient elution: 0-15min, 5%A-15%A, 15-60min, 15%A-35%A; Flow velocity 1ml/min; Sample size 10 μ l; 30 ° of C of column temperature; Detect wavelength 330nm.
3. the configuration of reference substance solution
Precision takes by weighing reference substance CAULIS MARSDENIAE TENACISSIMAE glycosides A, CAULIS MARSDENIAE TENACISSIMAE glycosides F, CAULIS MARSDENIAE TENACISSIMAE aglycon B, 17 β CAULIS MARSDENIAE TENACISSIMAE aglycon B, place the brown volumetric flask of 10ml, add the dissolving of chromatographically pure methyl alcohol, and being settled to 10ml, each reference substance concentration is followed successively by 100.04 μ g/ml, 56.78 μ g/ml, 82.08 μ g/ml, 57.42 μ g/ml.Respectively getting 1ml mixes to such an extent that mix reference substance solution.The typical curve of CAULIS MARSDENIAE TENACISSIMAE glycosides A, CAULIS MARSDENIAE TENACISSIMAE glycosides F, CAULIS MARSDENIAE TENACISSIMAE aglycon B, 17 β CAULIS MARSDENIAE TENACISSIMAE aglycon B is respectively: y=100.647x+11.004 (R
2=0.9998), y=80.362x-15.631 (R
2=0.9997), y=40.693x-20.457 (R
2=0.9999), y=122.045x+30.957 (R
2=0.9999).
4. each phenolic acid component content of sample is measured
Different batches medicinal substances extract, intermediate, parenteral solution are crossed 0.45 μ m filter membrane respectively, precision is drawn each 10 μ l of need testing solution respectively, inject liquid chromatograph, measure the total content of CAULIS MARSDENIAE TENACISSIMAE glycosides A, CAULIS MARSDENIAE TENACISSIMAE glycosides F, 17 β CAULIS MARSDENIAE TENACISSIMAE aglycon B, CAULIS MARSDENIAE TENACISSIMAE aglycon B respectively, the results are shown in Table 1.
6, the carbohydrate content qualitative, quantitative is measured
Carbohydrate content in CAULIS MARSDENIAE TENACISSIMAE medicinal material, intermediate, the parenteral solution is carried out qualitative, quantitative to be characterized.PMP pre-column derivatization HPLC chromatogram is seen Fig. 5.
PMP pre-column derivatization condition determination
1. instrument and reagent:
High performance liquid chromatograph Agilent1200Series series (quaternary pump, online vacuum outgas system, automatic sampler, column oven, DAD detecting device), Agilent Chem Station chem workstation).
Reference substance: fructose, glucose, oleandrose are available from Nat'l Pharmaceutical ﹠ Biological Products Control Institute, and purity is all greater than 98%.
Methyl alcohol (chromatographically pure, U.S. TEDIA company), Milli-Q ultrapure water.All the other reagent are pure for analyzing.
2. chromatographic condition
Chromatographic column: Agilent Zorbax SB-C18(4.6 * 250mm, 5 μ m) chromatographic column; Flowing is methyl alcohol (A)-0.05M potassium dihydrogen phosphate aqueous solution mutually, and the gradient elution program is: 1-10min, 15%A-30%A; 10-30min, 30%-55%A; Flow velocity: 1.0ml/min; Be 30min analysis time; Detect wavelength: 245nm; Column temperature: 25 ° of C; Sample size: 10 μ l.
3. the preparation of standard solution
Precision takes by weighing fructose, glucose, oleandrose monose reference substance, adds dissolved in distilled water and is settled to 10ml, and the concentration of fructose, glucose, oleandrose is followed successively by 6.97mg/ml, 5.84mg/ml, 10.08mg/ml.Respectively get the 0.5ml reference substance solution and mix, insert the NaOH solution 1.5ml of 0.15M, mixing, the 1-phenyl-3-methyl-5-pyrazolones ketone (PMP) of adding 1ml is methanol solution (0.1M), places 70 ° of C water-baths, and isothermal reaction 30min takes out and is cooled to room temperature; Add the neutralization of 0.075M hydrochloric acid; Add 7ml distilled water and 10ml methenyl choloride then, leave standstill behind the vortex 2min, take out the methenyl choloride layer; The residue water layer adds the vibration of 1ml methenyl choloride vortex again and mixes, and repeats above experimentation 3 times.Water intaking layer solution, 0.45 μ m membrane filtration, standby.
4. the preparation of sample solution
Get CAULIS MARSDENIAE TENACISSIMAE medicinal material, intermediate, the injection liquid samples 0.5ml of different batches, add 0.5ml distilled water respectively, the vortex mixing, the NaOH solution (0.15M) that adds 1ml then, the vortex mixing, 1-phenyl-3-methyl-5-pyrazolones ketone (PMP) the methanol solution 0.5ml of adding 0.2M places 70 ° of C water-baths, isothermal reaction 30min takes out and is cooled to room temperature; Add the neutralization of 0.075M hydrochloric acid; Add 7ml distilled water and 10ml methenyl choloride then, leave standstill behind the vortex 2min, take out the methenyl choloride layer; The residue water layer adds the vibration of 1ml methenyl choloride vortex again and mixes, and repeats above experimentation 3 times.Water intaking layer solution, 0.45 μ m membrane filtration, standby.
5. sugared assay:
Get reference substance and CAULIS MARSDENIAE TENACISSIMAE medicinal material, intermediate, injection liquid samples solution, analyze by the chromatographic condition of setting up, compare with fructose, glucose, oleandrose reference substance, calculate the total content of carbohydrate components in CAULIS MARSDENIAE TENACISSIMAE medicinal material, intermediate, the parenteral solution.The results are shown in Table 1.
The applicant finds, when the detection step that adopts as above, phenolic acid in CAULIS MARSDENIAE TENACISSIMAE medicinal material, intermediate, parenteral solution, steroid saponin, when carbohydrate detects, phenolic acid, steroid saponin, carbohydrate components content are controlled at the 50%-95% of summation greater than total solid, it forms structure is phenolic acid than scope: steroid saponin: carbohydrate=(1%-95%): (1%-95%): (1%-95%), and when wherein phenolic acid and steroid saponin component total content were not less than 0%-85%, the quality that contains the CAULIS MARSDENIAE TENACISSIMAE parenteral solution that finally obtains was for best.
The polycomponent process dynamic mass control method of table 1 CAULIS MARSDENIAE TENACISSIMAE medicinal material, intermediate, parenteral solution
Claims (1)
1. polycomponent process dynamic mass control detection method that contains the CAULIS MARSDENIAE TENACISSIMAE parenteral solution is characterized by: to the CAULIS MARSDENIAE TENACISSIMAE medicinal material, preparation contains the intermediate in the CAULIS MARSDENIAE TENACISSIMAE parenteral solution process, phenolic acid, steroid saponin, the carbohydrate that contains in the CAULIS MARSDENIAE TENACISSIMAE parenteral solution finished product detects control;
The main chemical compositions of described phenolic acid is gallic acid, coumaric acid, Cryptochlorogenic acid, neochlorogenic acid, vanillic acid, chlorogenic acid, syringic acid, forulic acid etc., its method of quality control is measured with high-efficient liquid phase technique, and reference substance is selected from 3～8 in gallic acid, coumaric acid, Cryptochlorogenic acid, neochlorogenic acid, vanillic acid, chlorogenic acid, syringic acid, the forulic acid;
The main chemical compositions of described steroid saponin is CAULIS MARSDENIAE TENACISSIMAE glycosides A, CAULIS MARSDENIAE TENACISSIMAE glycosides F, 17 β CAULIS MARSDENIAE TENACISSIMAE aglycon B, CAULIS MARSDENIAE TENACISSIMAE aglycon B etc., its method of quality control is measured with high-efficient liquid phase technique, and reference substance is selected from one or more among CAULIS MARSDENIAE TENACISSIMAE glycosides A, CAULIS MARSDENIAE TENACISSIMAE glycosides F, 17 β CAULIS MARSDENIAE TENACISSIMAE aglycon B, the CAULIS MARSDENIAE TENACISSIMAE aglycon B;
Described carbohydrate is mainly fructose, glucose, oleandrose etc., and its method of quality control PMP pre-column derivatization sugar finger-print, reference substance are selected from one or more in fructose, glucose, the oleandrose;
The content summation of described phenolic acid, steroid saponin, carbohydrate components is greater than the 50%-95% of total solid, it forms structure is phenolic acid than scope: steroid saponin: carbohydrate=(1%-95%): (1%-95%): (1%-95%), wherein phenolic acid and steroid saponin component total content are not less than 0%-85%.
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