CN114487182A - Content determination method of Tianwang heart tonifying preparation - Google Patents
Content determination method of Tianwang heart tonifying preparation Download PDFInfo
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- CN114487182A CN114487182A CN202210063466.0A CN202210063466A CN114487182A CN 114487182 A CN114487182 A CN 114487182A CN 202210063466 A CN202210063466 A CN 202210063466A CN 114487182 A CN114487182 A CN 114487182A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
- G01N2030/146—Preparation by elimination of some components using membranes
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention discloses a content determination method of a Tianwang heart tonifying preparation, and belongs to the technical field of traditional Chinese medicine detection. The method for determining the content of 3,6 ' -dibapinyl sucrose, spinosin and schizandrol A in the Tianwang Buxin preparation is used for simultaneously determining the content of the 3,6 ' -dibapinyl sucrose, the spinosin and the schizandrol A in the Tianwang Buxin preparation under the same chromatographic condition, is simple, accurate, convenient and fast to operate and high in detection efficiency, can conveniently and fast detect the content of the 3,6 ' -dibapinyl sucrose, the spinosin and the schizandrol A in the Tianwang Buxin preparation by adopting the method, is favorable for inspecting the quality condition of the polygala tenuifolia, the fried spina date seed and the schisandra chinensis in the Tianwang Buxin pill, and inspects whether an enterprise has the behaviors of no feeding or less feeding or poor feeding and feeding of medicinal materials, thereby being favorable for further accurately and comprehensively evaluating and controlling the quality of the Tianwang Buxin preparation and ensuring the clinical efficacy.
Description
Technical Field
The invention belongs to the technical field of traditional Chinese medicine detection, and particularly relates to a content determination method of a Tianwang heart tonifying preparation.
Background
The Tianwang heart tonifying preparation has the effects of nourishing yin and blood, tonifying heart and soothing nerves; the traditional Chinese medicine composition is clinically used for treating heart-yin deficiency, palpitation, amnesia, insomnia, dreaminess and dry stool. The TIANWANGBUXIN preparation comprises TIANWANGBUXIN pill and TIANWANGBUXIN pill (concentrated pill), wherein the two prescriptions are composed of 16 medicinal materials such as salvia miltiorrhiza, angelica, acorus gramineus, codonopsis pilosula, poria cocos, schisandra chinensis, ophiopogon japonicus, asparagus, rehmannia glutinosa, radix scrophulariae, polygala tenuifolia (prepared), spina date seed (fried), platycladi seed, platycodon grandiflorum, liquorice, cinnabar and the like. The TIANWANGBUXIN pill is brown black water honeyed pill, brown black small honeyed pill or large honeyed pill; slightly fragrant smell, sweet and slightly bitter taste; the TIANWANGBUXIN pill (concentrated pill) is brown black concentrated pill; slightly fragrant smell, sweet and bitter taste. The prescription can be traced from Song generation Chen Ming self Ming (women's big whole good prescription) Ju Liu, and later through Ming generation Xue Ji. Ming Dynasty Hongjiu (general essentials for life) also records the treatment of heart-blood deficiency, restlessness, exhaustion of body fluids, amnesia, severe palpitation, constipation, sores on the mouth and tongue, etc. The modern medical report shows that the Tianwang Buxin pill can be used for treating insomnia, anxiety, depression, neurasthenia, vertigo caused by hyperthyroidism and the like in clinic, and is collected in a patent medicine preparation of the national formulary 2015 edition.
In the current standard of the Tianwang Buxin preparation (content determination), the index for controlling the Tianwang Buxin pill is only schizandrol A in schisandra chinensis, and the index for controlling the Tianwang Buxin pill (concentrated pill) is only salvianolic acid B in salvia miltiorrhiza, so that the quality of the Tianwang Buxin preparation cannot be effectively and integrally evaluated. Therefore, the research on the determination of the contents of the components such as the polygala tenuifolia, the fried spina date seed and the schisandra chinensis in the prescription of the Tianwang heart tonifying preparation is beneficial to investigating the quality conditions of the polygala tenuifolia, the fried spina date seed and the schisandra chinensis in the Tianwang heart tonifying pill, better and comprehensively controlling the quality of the Tianwang heart tonifying preparation and ensuring the clinical efficacy.
Disclosure of Invention
The invention aims to provide a content determination method of a Tianwang heart tonifying preparation aiming at the defects of the prior art. The method for determining the content of the polygala tenuifolia (3, 6 '-dibapine acyl sucrose), the fried spina date seed (spinosin) and the schisandra chinensis (schizandrol A) in the Tianwang heart tonifying preparation is used for simultaneously determining the content of the polygala tenuifolia (3, 6' -dibapine acyl sucrose), the fried spina date seed (spinosin) and the schisandra chinensis (schizandrol A) in the Tianwang heart tonifying preparation under the same chromatographic condition.
In order to achieve the purpose, the invention adopts the following technical scheme:
a content determination method of a Tianwang Buxin preparation comprises a Tianwang Buxin pill and a Tianwang Buxin pill (concentrated pill), the determination method is to simultaneously determine the content of 3, 6' -dibapigenin sucrose, spinosin and schizandrol A in the Tianwang Buxin preparation under the same chromatographic condition, and the specific method comprises the following steps:
(1) chromatographic conditions and system applicability test: octadecylsilane chemically bonded silica was used as a filler (Agilent Eclipse Plus C18, 1.8 μm, 2.1X 100 mm); acetonitrile is taken as a mobile phase A, water is taken as a mobile phase B, and gradient elution is carried out according to the specification in the following table 1; the flow rate was 0.2ml per minute; the detection wavelength is 335nm and 250 nm; the number of theoretical plates is not less than 30000 calculated according to the schizandrol A peak;
(2) preparation of control solutions: accurately weighing appropriate amount of spinosin reference substance, 3,6 '-dibapinyl sucrose reference substance, and schizandrol A reference substance, and adding 80% methanol to obtain mixed reference substance solution containing 10 μ g of spinosin, 10 μ g of 3, 6' -dibapinyl sucrose, and 80 μ g of schizandrol A per 1 ml;
(3) preparation of test solution
Tianwang heart tonifying pill: taking a water-honeyed pill of the product, grinding, taking 4g, and precisely weighing; or cutting honeyed pill into pieces, and precisely weighing 5g of the honeyed pill; or cutting large honeyed pill with different weights into pieces, and precisely weighing 5g of the honeyed pill; placing in a conical flask with a plug, adding 20ml of 80% methanol solution precisely, weighing, heating and refluxing for 2 hr, taking out, cooling, weighing again, adding 80% methanol solution to make up for the lost weight, shaking, filtering (0.22 μm filter membrane), and collecting the filtrate;
tianwang Buxin pills (concentrated pills): precisely weighing 1.5g of the product, placing the product in a conical flask with a plug, precisely adding 20ml of 80% methanol solution, weighing, ultrasonically extracting (320W, 40 kHz) for 60 minutes, taking out, cooling, weighing again, shaking up, filtering (0.22 mu m filter membrane), and taking out the subsequent filtrate;
(4) and (3) determination: precisely sucking 2 μ l of the reference solution and the sample solution, respectively, injecting into an ultra-high performance liquid chromatograph, and measuring.
The content determination method of the Tianwang heart tonifying preparation comprises the following steps: the product contains parched semen Ziziphi Spinosae and spinosin (C)28H32O15) Measured, every 1g of the water-honeyed pill is not less than 0.035 mg; 1g of small honeyed pill should not be less than 0.027 mg; the content of big honeyed pill should not be less than 0.24 mg; contains 3, 6' -mustard acyl sucrose (C) as polygala root36H46O17) Measured, every 1g of the water-honeyed pill is not less than 0.065 mg; 1g of small honeyed pill should not be less than 0.050 mg; the content of big honeyed pill should not be less than 0.45mg per pill; schisandra chinensis and schizandrol A (C)24H32O7) Measured, every 1g of the water-honeyed pill is not less than 0.19 mg; 1g of small honeyed pill should not be less than 0.13 mg; the dosage of big honeyed pill should not be less than 1.22 mg. Tianwang Buxin pills (concentrated pills): the product contains parched semen Ziziphi Spinosae and spinosin (C)28H32O15) In terms of each 1g, the amount of the active carbon is not less than 30.9 mu g; contains 3, 6' -mustard acyl sucrose (C) as polygala root36H46O17) Measured, each 1g of the extract should not be less than 44.6 mug; the schisandra fruit is prepared with schisandrin A (C)24H32O7) It should be measured that the content of the compound should not be less than 93.4. mu.g per 1 g.
The invention has the beneficial effects that:
the invention provides a content determination method of a Tianwang heart-tonifying preparation, which utilizes ultra-high performance liquid chromatography (UPLC) to simultaneously determine the contents of polygala tenuifolia (3, 6' -dibapigenin sucrose), fried spina date seed (spinosin) and schisandra chinensis (schizandrol A) in the Tianwang heart-tonifying preparation under the same chromatographic condition.
The method provided by the invention is verified by methodology, and has the advantages of high precision, high sensitivity, strong specificity, good reproducibility, good stability, high recovery rate and accurate measurement result. The method is favorable for inspecting the quality conditions of the polygala tenuifolia, the fried spina date seed and the schisandra chinensis in the Tianwang heart tonifying pill and checking whether the enterprise has the behaviors of no feeding or less feeding and feeding of inferior medicinal materials, thereby being favorable for further accurately and comprehensively evaluating and controlling the quality of the Tianwang heart tonifying preparation. The content determination method of the Tianwang heart tonifying preparation provided by the invention perfects the quality detection standard of the Tianwang heart tonifying preparation, can provide a basis for comprehensively evaluating and controlling the quality of the Tianwang heart tonifying preparation, and lays a foundation for establishing the quality standard of the Tianwang heart tonifying preparation.
Drawings
FIG. 13, a full wavelength scan of 6' -dibapinyl sucrose, spinosin, salvianolic acid B, and schizandrin A;
FIG. 2 is a graph showing the standard curves of spinosin, 3, 6' -dibapinyl sucrose, salvianolic acid B, and schizandrin A;
FIG. 3 is a chromatogram of a mixed solution of reference substances, wherein 1, spinosin, 2, 3, 6' -dibapinyl sucrose, 3, salvianolic acid B, 4, and schizandrol A;
FIG. 4 is a negative sample map of Tianwang Buxin Wan lack-parched semen Ziziphi Spinosae and lack-cortex et radix Polygalae, in which 1, spinosin; 2.3, 6' -dibapinyl sucrose;
FIG. 5 is a graph of a fructus Schisandrae chinensis negative sample lacking in TIANWANGBUXIN pill, in which 3-salvianolic acid is shown; 4-schizandrol A;
FIG. 6 is a chromatogram of TIANWANGBUXIN pill (Shanxi Zhendong Kaiyuan pharmaceutical Co., Ltd., batch No. 20200401);
FIG. 7 chromatogram of Tianwang Buxin pill (Jilin province Yinnoko pharmaceutical Co., Ltd., lot number 20200603);
FIG. 8 chromatogram of Tianwang Buxin pill (concentrated pill) (Fuci, Lanzhou, manufactured by pharmaceutical Co., Ltd., lot No. 20081).
Detailed Description
Example 1
1. Instrument and reagent
Waters high performance liquid chromatograph ACQUITY UPLC H-CLASS; model ML204 electronic analytical balance (mertler-toledo instruments shanghai ltd). 3, 6' -two mustard seed acyl sucrose (provided by China food and drug testing institute for assay, batch number: 111848-202006, content 96.5%), spinosin (provided by China food and drug testing institute for assay, batch number: 111869-202005, content 94.8%), salvianolic acid B (provided by China food and drug testing institute for assay, batch number: 111848-202006, content 96.5%), schisandrin (provided by China food and drug testing institute for assay, batch number: 110857-201815, content 99.7%), acetonitrile is chromatographically pure, and other reagents are analytically pure. 127 batches of Tianwang Buxin pills (35 batches of water-honeyed pills, 62 batches of big honeyed pills and 30 batches of small honeyed pills) are all samples tested by the national appraisal test in 2021 years. Method survey the adopted Tianwang Buxin pill (big honeyed pill) is Beijing Tongrentang pharmaceutical Co., Ltd, and the batch number is as follows: 20015236, respectively; tianwang Buxin pills (water-honeyed pills) are the taiji group Chongqing Tongjunge pharmaceutical factory ltd, batch number: 2101001.
2. examination of experimental conditions and methodological verification
2.1 selection of mobile phase: the effects of elution with methanol-water, acetonitrile-water, methanol-0.1% phosphoric acid solution, and acetonitrile-0.1% phosphoric acid solution as mobile phases and different gradients and flow rates were compared, respectively. After groping, the gradient of acetonitrile as mobile phase A and 0.1% phosphoric acid as mobile phase B is determined as shown in Table 1, and under the gradient, the separation effect is good and the peak shapes are symmetrical.
2.2 selection of detection wavelength: performing full-wavelength scanning on index components 3, 6' -erucyl sucrose, spinosin, schizandrol and salvianolic acid B for preparing polygala tenuifolia, fried spina date seed, schisandra chinensis and salvia miltiorrhiza by using a DAD detector, as shown in figure 1, and finally selecting the schizandrol detection wavelength of 250nm by referring to detection wavelengths of polygala tenuifolia, spina date seed, schisandra chinensis and salvia miltiorrhiza [ content determination ] in 2020 edition of Chinese pharmacopoeia; the detection wavelength of 3, 6' -dibapinyl sucrose and spinosin is 335 nm.
2.3 examination of the preparation of test solution (selection of extraction method and extraction time)
2.3.1 comparing the ultrasonic extraction and different heating reflux time.
Ultrasonic extraction of big honeyed pills (1): collecting big honeyed pill, cutting, collecting 5g, precisely weighing, placing into conical flask with plug, precisely adding 80% methanol solution 20ml, weighing, ultrasonic treating for 120 min (power 320W, frequency 40 kHz), taking out, cooling, weighing again, supplementing with 80% methanol solution, shaking, filtering (0.22 μm filter membrane), and collecting filtrate. (2) Heating reflux extraction: collecting big honeyed pill, cutting, collecting 5g, precisely weighing, placing in conical flask with plug, precisely adding 80% methanol solution 20ml, weighing, heating and refluxing for 60 min, 120 min and 150 min, respectively, taking out, cooling, weighing again, supplementing with 80% methanol solution, shaking, filtering (0.22 μm filter membrane), and collecting the filtrate.
Ultrasonic extraction of water-honeyed pills (1): taking the water-honeyed pill, grinding, taking 4g, precisely weighing, placing in a conical flask with a plug, precisely adding 20ml of 80% methanol solution, weighing, performing ultrasonic treatment for 120 minutes (power 320W and frequency 40 kHz), taking out, cooling, weighing again, complementing the weight loss with 80% methanol solution, shaking up, filtering (0.22 mu m filter membrane), and taking the subsequent filtrate. (2) Heating reflux extraction: taking the water-honeyed pill, grinding, taking 4g, precisely weighing, placing in a conical flask with a plug, precisely adding 20ml of 80% methanol solution, weighing, heating and refluxing for 60 min, 120 min and 150 min respectively, taking out, cooling, weighing again, complementing the weight loss with 80% methanol solution, shaking uniformly, filtering (0.22 mu m filter membrane), and taking the subsequent filtrate to obtain the product.
Ultrasonic extraction of the concentrated pill (1): weighing 1.5g of the product, precisely weighing, placing in a conical flask with a plug, precisely adding 20ml of 80% methanol solution, weighing, performing ultrasonic treatment for 120 min (power 320W, frequency 40 kHz), taking out, cooling, weighing again, supplementing the lost weight with 80% methanol solution, shaking up, filtering (0.22 μm filter membrane), and taking the subsequent filtrate. (2) Heating reflux extraction: precisely weighing 1.5g of the product, placing the product in a conical flask with a plug, precisely adding 20ml of 80% methanol solution, weighing the weight, heating and refluxing for 60 minutes, 120 minutes and 150 minutes respectively, taking out, cooling, weighing the weight again, supplementing the loss weight with 80% methanol solution, shaking up, filtering (0.22 mu m filter membrane), and taking the subsequent filtrate to obtain the product.
The results show that the content of the components to be detected in the large honeyed pills and the water honeyed pills are extracted by heating and refluxing for 120 minutes, which is higher than that in ultrasonic extraction, the components are completely extracted, and the content of salvianolic acid B is inversely proportional to the extraction time, so that the components are extracted by refluxing for 120 minutes, which is detailed in tables 2 and 3. Concentrating the pill, heating, refluxing, and ultrasonically extracting for 60 min, so that the ultrasonic extraction is performed for 60 min, and the details are shown in Table 4.
2.3.2 selection of extraction solvent (examining the extraction effect of 6 solvents, methanol 80%, methanol 50%, anhydrous ethanol, ethanol 80%, and ethanol 50%)
Collecting big honeyed pill, cutting into pieces, collecting 5g, precisely weighing, placing into conical flask with plug, precisely adding each 20ml of the above 6 solvents, weighing, heating and refluxing for 2 hr, taking out, cooling, weighing again, adding 80% methanol solution to balance, shaking, filtering (0.22 μm filter membrane), and collecting filtrate.
Taking a water-honeyed pill, grinding, taking 4g, precisely weighing, placing in a conical flask with a plug, precisely adding 20ml of each of the 6 solvents, weighing, heating and refluxing for 2 hours, taking out, cooling, weighing again, supplementing the weight loss by 80% methanol solution, shaking uniformly, filtering (0.22 μm filter membrane), and taking the subsequent filtrate.
Collecting concentrated pill, grinding, collecting 4g, precisely weighing, placing into conical flask with plug, precisely adding each 20ml of the above 6 solvents, weighing, ultrasonic extracting (320W, 40 kHz) for 1 hr, taking out, cooling, weighing again, supplementing with 80% methanol solution, shaking, filtering (0.22 μm filter membrane), and collecting filtrate.
The determination result shows that the water-honeyed pills have the methanol extraction contents of different concentrations which are relatively close to each other but higher than the ethanol extraction contents of different concentrations, while the large honeyed pills have the contents of the components to be detected extracted by 80% methanol and 50% methanol which are obviously higher than the contents of other 4 solvents, but the viscosity of 50% methanol extract is difficult to pass through a 0.22 mu m filter membrane, so 80% methanol is selected as the extraction solvent, and the details are shown in tables 5-1 and 5-2. The concentrated pill has high content of components to be detected by 80% methanol and methanol extraction, and is consistent with the extraction solvent of TIANWANGBUXIN pill, so 80% methanol is used as the extraction solvent, and is shown in Table 5-3.
2.3.3 selection of sample size
Collecting big honeyed pill, cutting, collecting 2.5g, 5g, 10g, precisely weighing, placing in conical flask with plug, precisely adding 80% methanol solution 20ml, weighing, heating under reflux for 120 min, taking out, cooling, weighing again, supplementing with 80% methanol solution, shaking, filtering (0.22 μm filter membrane), and collecting filtrate.
Taking the water-honeyed pill, grinding, respectively taking 2g, 4g and 8g, precisely weighing, placing in a conical flask with a plug, precisely adding 20ml of 80% methanol solution, weighing, heating and refluxing for 120 minutes, taking out, cooling, weighing again, complementing the weight loss with 80% methanol solution, shaking uniformly, filtering (0.22 mu m filter membrane), and taking the subsequent filtrate to obtain the product.
Taking a proper amount of the concentrated pill, grinding, respectively taking 1g, 1.5g and 3g, precisely weighing, placing in a conical flask with a plug, precisely adding 20ml of 80% methanol solution, weighing, ultrasonically extracting (320W, 40 kHz) for 60 minutes, taking out, cooling, weighing again, supplementing the lost weight with 80% methanol solution, shaking up, filtering (0.22 μm filter membrane), and taking the subsequent filtrate.
The results show that when the sampling amount of the large honeyed pill is 2.5g and 5g, and the sampling amount of the water honeyed pill is 2g and 4g, the extraction of the component to be detected is complete, but when the sampling amount of the large honeyed pill is 2.5, and the sampling amount of the water honeyed pill is 2g, the peak area of the chromatographic peak is small, so that the sampling amount of the large honeyed pill is 5g, and the sampling amount of the water honeyed pill is 4g, which are detailed in tables 6-1 and 6-2. When the sampling amount of the concentrated pill is 3g, the content of the characteristic component spinosad in the spina date seed is obviously lower than that of 1g and 1.5g of the concentrated pill, so 1.5g with a larger peak area is selected, and the detail is shown in tables 6-3.
Because the preparation method of the small honeyed pill is completely consistent with that of the large honeyed pill, the extraction conditions of the small honeyed pill are consistent with those of the large honeyed pill.
In combination with the above studies, the preparation method of the proposed test solution is as follows:
tianwang Buxin Wan: taking a water-honeyed pill, grinding, taking 4g, and precisely weighing; or cutting honeyed pill into pieces, and precisely weighing 5g of the honeyed pill; or shearing big honeyed pill with different weight, collecting 5g, precisely weighing, placing in a conical flask with a plug, precisely adding 80% methanol solution 20ml, weighing, heating and refluxing for 2 hr, taking out, cooling, weighing again, shaking, filtering (0.22 μm filter membrane), and collecting the filtrate.
Tianwang Buxin pills (concentrated pills): precisely weighing 1.5g of the product, placing the product in a conical flask with a plug, precisely adding 20ml of 80% methanol solution, weighing, ultrasonically extracting (320W, 40 kHz) for 60 minutes, taking out, cooling, weighing again, shaking up, filtering (0.22 mu m filter membrane), and taking out the subsequent filtrate.
2.4 methodological validation
2.4.1 examination of the Linear relationship
Preparation of each control stock solution: accurately weighing 10.15mg (content: 94.8%) of spinosin reference substance, 12.25mg (content: 96.5%) of 3, 6' -dibastinyl sucrose reference substance, 22.82mg of salvianolic acid B (content: 96.6%), taking 10.11mg (content: 99.7%) of schizandrol reference substance, putting into a 20ml measuring flask, respectively adding methanol to dilute to scale, and shaking uniformly to obtain the final product. (pinocembrin: 0.4811mg/ml, 3, 6' -dibapinyl sucrose: 0.5911mg/ml, salvianolic acid B: 0.1102mg/ml, schizandrol A: 0.5040 mg/ml).
Preparation of mixed control solution: precisely measuring 100 μ l of reference stock solutions of spinosin and 3, 6' -dibastinyl sucrose and 0.80ml of schizandrol A, placing in a 5ml measuring flask,adding methanol to dilute to scale, and using as mixed reference solution
. Precisely measuring mixed reference substance solution
1.00ml, placing in a 5ml measuring flask, adding methanol to dilute to scale, and using as mixed reference solution
。
Respectively and precisely sucking the reference substance mixed solution
1. mu.l, 2. mu.l, 3. mu.l, 10. mu.l; comparative sample solution
Injecting into a liquid chromatograph, measuring, and drawing a standard curve by taking the peak area as the ordinate and the log value of the sample amount of the reference substance as the abscissa.
The results show that: the linear relationship between the spinosin reference substance and the 3,6 '-dibapinyl sucrose reference substance is 96.2 ng-3.848 ng, the linear relationship between the spinosin reference substance and the 3, 6' -dibapinyl sucrose reference substance is 118.2 ng-4.728 mu ng, and the linear relationship between the schisandrin reference substance and the 881.6 n-35.264 ng is good. The results are shown in Table 7, FIG. 2.
2.4.2 repeatability test
Tianwang Buxin pills (water-honeyed pills): taking a proper amount of water-honeyed pills, grinding, taking 4g, precisely weighing, placing in a conical flask with a plug, taking 6 parts in total, preparing 6 parts of test solution according to the preparation method of the test solution, precisely sucking 10 mu l of each test solution, injecting into a liquid chromatograph, analyzing according to the chromatographic conditions, measuring the peak area, calculating the content, and obtaining the result shown in Table 8.
Tianwang heart tonifying pill (big honeyed pill): taking large honeyed pills with different weights, cutting into pieces, taking 5g of the honeyed pills, precisely weighing, placing the honeyed pills in a conical flask with a plug, preparing 6 parts of test solution according to the preparation method of the test solution, precisely sucking 10 mu l of the test solution, injecting the test solution into a liquid chromatograph, analyzing according to the chromatographic conditions, measuring the peak area, calculating the content, and obtaining the result shown in table 9.
Tianwang Buxin pills (concentrated pills): taking 1.5g of the product, precisely weighing, placing in a conical flask with a plug, taking 6 parts in total, preparing 6 parts of test solution according to the preparation method of the test solution, precisely sucking 2 mu l of each test solution, injecting into a liquid chromatograph, analyzing according to the chromatographic conditions, measuring peak area, calculating content, and obtaining the result shown in Table 10.
The results show that the RSD of the contents of the spinosin, the 3, 6' -dibapinyl sucrose, the paeonol and the schizandrol A measured by 6 samples of the Tianwang Buxin pill (big honeyed pill) and the Tianwang Buxin pill (small honeyed pill) are all less than 3 percent, which accords with the requirement of methodology and shows that the method has good repeatability. RSD of the contents of the spinosin, the 3, 6' -dibapinyl sucrose and the schizandrol A measured by 6 samples of the Tianwang heart tonifying pills (concentrated pills) is less than 3 percent, meets the requirement of methodology and shows that the method has good repeatability.
2.4.3 precision review: and taking the same sample solution under the repeatability term, repeatedly sampling for 6 times, measuring the peak area, calculating the RSD, and obtaining the result that the RSD of the peak areas of the spinosad, the 3, 6' -dibapigenin sucrose, the paeonol and the schisandrin A are all less than 3 percent, thereby meeting the requirement of methodology and showing that the method has good precision, and the method is shown in tables 11-13.
2.4.4 stability considerations: taking a sample solution under the item of '2.4.2 repeatability inspection', respectively injecting samples for 0h, 4h, 8h, 16h, 20h and 24h, recording peak areas, calculating RSD, and finding results in tables 14-16.
The results show that the peak areas RSD of the spinosad, the 3, 6' -dibapinyl sucrose and the schizandrol in the test solution are all less than 3 percent within 24 hours, which indicates that the test solution is stable within 24 hours.
2.4.5 specialization study: negative samples of the bessinomin, the 3, 6' -dibapinyl sucrose and the schizandrol A are respectively prepared according to the prescription of the Tianwang heart tonifying pill, and the negative sample solution is prepared according to the preparation of the test sample solution. Respectively sucking 2 mul of each of the reference substance solution and the negative sample solution, injecting the solutions into a liquid chromatograph, measuring and analyzing, wherein the result negative sample has no corresponding chromatographic peak at the corresponding position of the chromatographic peak of the component to be measured of the test sample, which indicates that the sample is negative and has no interference, and the method has good specificity. See fig. 3-5.
2.4.6 recovery test
Tianwang Buxin pills (water-honeyed pills): precisely weighing 21.37mg (content: 99.7%) of schizandrol A, placing in a 10ml measuring flask, adding methanol to dissolve and dilute to scale, precisely weighing 7ml of the above schizandrol A reference solution, 2ml of a Schizandrol B reference stock solution under 2.4.1, and 4.5ml of a 3,6 '-dibapinyl sucrose reference stock solution, precisely weighing 14.46mg of salvianolic acid B reference, placing in a same 200ml measuring flask, adding 80% methanol to dissolve and dilute to scale, and using as sample application reference solution (the schisandrin: 4.811. mu.g/ml, the 3, 6' -dibapinyl sucrose: 13.30. mu.g/ml, the salvianolic acid B: 69.84. mu.g/ml, and the schizandrol A: 36.15. mu.g/ml).
Taking a proper amount of water-honeyed pills (0.0551 mg/g of spinosin, 0.1294mg/g of 3, 6' -dibapine acyl sucrose, 0.6784mg/g of salvianolic acid B and 0.3717mg/g of schizandrol A) with known content, grinding, taking about 2g, precisely weighing, precisely adding 20ml of the sample-adding reference solution, weighing, and preparing into a sample-adding sample solution according to the preparation method of the sample solution.
Precisely absorbing 10 mu l of the two sample-adding sample solutions, injecting the two sample-adding sample solutions into a liquid chromatograph, measuring peak areas, calculating the recovery rate, and obtaining the result that the recovery rates of the spinosad, the 3, 6' -dibapinyl sucrose and the schizandrin in the samples are good and meet the requirement of methodology, which is shown in Table 17.
Tianwang Buxin pills (big honeyed pills): precisely weighing 1.5ml of the stipinol reference stock solution, 2.5ml of the 3,6 '-dibapinyl sucrose reference stock solution and 12ml of the schizandrol A reference stock solution under the condition of 2.4.1, precisely weighing 12.56mg of the salvianolic acid B reference stock solution, placing the reference stock solution in a same 200ml measuring flask, adding 80% methanol to dilute to scale, and using the reference stock solution as a sample adding reference solution (stipinol: 3.61. mu.g/ml, 3, 6' -dibapinyl sucrose: 7.39. mu.g/ml, salvianolic acid B: 60.68. mu.g/ml, schizandrol A: 30.24. mu.g/ml).
Taking a proper amount of large honeyed pills with known content (0.2706 mg/pill of spinosin, 0.5168 mg/pill of 3, 6' -dibapinyl sucrose, 4.9696 mg/pill of salvianolic acid B and 2.2818 mg/pill of schizandrol), cutting into pieces, taking about 2.5g, precisely weighing, precisely adding 20ml of the sample-adding control solution, weighing, and preparing the sample-adding sample solution according to the preparation method of the sample solution.
Precisely absorbing 10 mu l of the two sample-adding sample solutions, injecting the two sample-adding sample solutions into a liquid chromatograph, measuring peak areas, calculating the recovery rate, and obtaining the result that the recovery rates of the spinosad, the 3, 6' -dibapinyl sucrose and the schizandrin in the samples are good and meet the requirement of methodology, which is shown in Table 18.
Tianwang Buxin pills (concentrated pills): precisely measuring 0.70ml of a spinosin reference stock solution, 0.50ml of a 3, 6' -dibapinyl sucrose and 0.50ml of a schizandrol reference stock solution under the draft item of content measurement, putting the solution into a 200ml measuring flask, and adding methanol to dilute the solution to a scale to obtain the spinosin reference stock solution serving as a reference solution for sample adding. (pinocembrin: 3.27. mu.g/ml, 3, 6' -erucyl sucrose: 2.96. mu. gmg/ml, schizandrol A: 2.51. mu.g/ml)
Taking a proper amount of water-honeyed pills (0.0436 mg/g of spinosin, 0.0394 mg/g of 3, 6' -dibapinyl sucrose and 0.0335mg/g of schizandrol), grinding, taking about 0.75g, precisely weighing, precisely adding 20ml of the sample-adding reference substance solution, weighing, and preparing the sample-adding sample solution according to the preparation method of the sample solution. The results are detailed in Table 19.
2.4.7 System suitability test: when samples are measured by using Agilent Eclipse Plus C18 (1.8 mu m, 2.1X 100 mm), the theoretical plate number of the peaks of large honeyed pills, small honeyed pills and water-honeyed pills is more than 30000, see Table 20, and when the peaks are measured by using ACQUITY UPLC HSS T3 (1.8 mu m, 2.1X 100 mm) and ACQUITY UPLC Peptide BEH C18 (1.7 mu m, 2.1X 100 mm), the peaks of the spinosyns and adjacent peaks can not be effectively separated, so the chromatographic column is prepared to be Agilent Eclipse Plus C18 (1.8 mu m, 2.1X 100 mm), and the theoretical plate number is not less than 30000 calculated by using schizandrol A peak.
And sample measurement
A content determination method of a Tianwang Buxin preparation comprises a Tianwang Buxin pill and a Tianwang Buxin pill (concentrated pill), and the specific method comprises the following steps:
(1) chromatographic conditions and system applicability test: octadecylsilane chemically bonded silica was used as a filler (Agilent Eclipse Plus C18, 1.8 μm, 2.1X 100 mm); acetonitrile is taken as a mobile phase A, water is taken as a mobile phase B, and gradient elution is carried out according to the specification in the table 1; the flow rate was 0.2ml per minute; the detection wavelength is 335nm and 250 nm; the number of theoretical plates is not less than 30000 calculated according to the schizandrol A peak;
(2) preparation of control solutions: accurately weighing appropriate amount of spinosin reference substance, 3,6 '-dibapinyl sucrose reference substance, and schizandrol A reference substance, and adding 80% methanol to obtain mixed reference substance solution containing 10 μ g of spinosin, 10 μ g of 3, 6' -dibapinyl sucrose, and 80 μ g of schizandrol A per 1 ml;
(3) preparation of test solution
Tianwang Buxin Wan: taking a water-honeyed pill, grinding, taking 4g, and precisely weighing; or cutting honeyed pill into pieces, and precisely weighing 5g of the honeyed pill; or cutting large honeyed pill with different weights into pieces, and precisely weighing 5g of the honeyed pill; placing in a conical flask with a plug, adding 20ml of 80% methanol solution precisely, weighing, heating and refluxing for 2 hr, taking out, cooling, weighing again, adding 80% methanol solution to make up for the lost weight, shaking, filtering (0.22 μm filter membrane), and collecting the filtrate;
tianwang Buxin pills (concentrated pills): precisely weighing 1.5g of the product, placing the product in a conical flask with a plug, precisely adding 20ml of 80% methanol solution, weighing, ultrasonically extracting (320W, 40 kHz) for 60 minutes, taking out, cooling, weighing again, shaking up, filtering (0.22 mu m filter membrane), and taking out the subsequent filtrate;
(4) and (3) determination: precisely sucking 2 μ l of the reference solution and the sample solution, respectively, injecting into an ultra-high performance liquid chromatograph, and measuring.
The content determination method of the Tianwang Buxin preparation is adopted to detect 91 Tianwang Buxin pills h with different batches of different manufacturers and 31 Tianwang Buxin pills (concentrated pills) with different batches of 8 manufacturers, the determination results are shown in tables 21-24, the chromatogram of the mixed solution of the reference substance is shown in figure 3, and the typical chromatogram of a sample of part of manufacturers is shown in figures 6-8.
4. Limit determination
Tianwang Buxin Wan: 127 batches of Tianwang Buxin pill samples without repeated batch numbers for the evaluation and spot test, wherein 35 batches of water-honeyed pills come from 9 production enterprises; 30 batches of small honeyed pills, which are from 3 production enterprises; 62 batches of big honeyed pills, which come from 17 production enterprises. According to the prescription of Tianwang Buxin pill, fried spina date seed, prepared polygala tenuifolia and schisandra chinensis are fine powder and are directly used as medicine, so the theoretical content of spinosad and 3,6 ' -dibastine acyl sucrose is calculated according to the items of fried spina date seed and prepared polygala tenuifolia under the first part of ' Chinese pharmacopoeia ' 2015 edition, the maximum transfer rate is formulated to a limit according to 80%, wherein the limit of schizandrol A adopts the limit of ' Chinese pharmacopoeia ' 2020 edition, and the result is as follows:
(1) the product contains parched semen Ziziphi Spinosae and spinosin (C)28H32O15) Measured, every 1g of the water-honeyed pill is not less than 0.035 mg; 1g of small honeyed pill should not be less than 0.027 mg; the content of big honeyed pill should not be less than 0.24 mg. (2) The product contains cortex et radix Polygalae and 3, 6' -DIsinapoyl sucrose (C)36H46O17) Measured, every 1g of the water-honeyed pill is not less than 0.065 mg; 1g of small honeyed pill should not be less than 0.050 mg; the dosage of big honeyed pill should not be less than 0.45 mg. (3) The product contains salvianolic acid B (C) from Saviae Miltiorrhizae radix36H30O16) Measured, every 1g of the water-honeyed pill is not less than 0.65 mg; 1g of the small honeyed pill should not be less than 0.50 mg; the dosage of the big honeyed pill should not be less than 4.47 mg. (4) The product contains fructus Schisandrae chinensis and schisandrin (C)24H32O7) Measured, every 1g of the water-honeyed pill is not less than 0.19 mg; 1g of small honeyed pill should not be less than 0.13 mg; the dosage of big honeyed pill should not be less than 1.22 mg.
Tianwang Buxin pills (concentrated pills): in the preparation method of Tianwang Buxin pill (concentrated pill), 3 medicinal materials of spina date seed, polygala root, schisandra fruit and the like are all decocted with water to prepare thick paste, so 80% of the average value of 31 batches of samples is used as a limit. The average value of the content of the spinosyns in 31 batches of samples is 38.68 mu g/g; the average value of the content of the 3, 6' -dibapinyl sucrose is 55.69 mu g/g; the average value of the schizandrol A content is 93.41 μ g/g, and 80% is taken as a limit, and the concrete steps are as follows:
the product contains parched semen Ziziphi Spinosae and spinosin (C)28H32O15) Measured by no less than 30.9 mug per 1 g; contains 3, 6' -mustard acyl sucrose (C) as polygala root36H46O17) Measured in each 1g, theLess than 44.6 μ g; the schisandra fruit is prepared with schisandrin A (C)24H32O7) The content of the compound should not be less than 93.4. mu.g per 1 g.
5. Determination of results
In the experimental process, the stability of the sample used in the methodology meets the requirement of the methodology, but the content stability of the salvianolic acid B in the salvia miltiorrhiza in part of enterprises and part of batches is poor, the sample injection results of the samples in the same batch at different time are greatly different, the salvianolic acid B is considered to be unstable, and the extraction time and the operation time of the method proposed by the text are long, so the content measurement data of the salvianolic acid B in the salvia miltiorrhiza obtained in the research is only used for reference, the standard text is not listed temporarily, the production enterprises are recommended to further enhance the quality control of the salvia miltiorrhiza in the production, the content of the salvianolic acid B in the Tianwang Buxin pill salvia miltiorrhiza is further researched subsequently, and a proper method is established for carrying out the quality control.
Carrying out content measurement on 127 batches of Tianwang Buxin pills of 29 production enterprises and after the weight batch number is removed, wherein the result shows that 24 batches of fried spina date seed content do not meet the regulation (wherein the water-honeyed pills are 19 batches, the small honeyed pills are 1 batch, and the large honeyed pills are 4 batches), and the failure rate is 18.6%; the 3, 6' -dibapinyl sucrose content of 22 batches does not meet the specification (wherein the water-honeyed pill is 18 batches, the small honeyed pill is 2 batches, and the large honeyed pill is 2 batches), and the reject ratio is 17.1%; 30 batches of fried spina date seed and 30 batches of polygala tenuifolia are not in accordance with the specifications of the samples of the manufacturers, the total unqualified rate is 23.3 percent, 35 batches of samples of water-honeyed pills are in accordance with the specifications, 21 batches of samples are not in accordance with the specifications, and the unqualified rate is 60.0 percent; the small honeyed pills comprise 30 batches of samples, 2 batches of the samples do not meet the specification, and the reject ratio is 6.7 percent; the large honeyed pills comprise 62 batches of samples, 6 batches of samples do not meet the specification, and the reject ratio is 9.5%. Wherein, 15 batches of products of Wuhu Zhang Hengchun pharmaceutical Co Ltd, 4 batches of products of Hubei Nuodesheng pharmaceutical Co Ltd, 1 batch of Xinjiang pharmaceutical Co Ltd of the national medicine group, 3 batches of products of Shiyao Shiyitang pharmaceutical factory, and 1 batch of products of Shanxi Huakang pharmaceutical Co Ltd are not in accordance with the regulations; 16 batches of Zhang Hengchun pharmaceutical Co Ltd in West lake, 2 batches of Yunan Teng pharmaceutical Co Ltd, 1 batch of Heilongjiang ginseng Pigeon pharmaceutical Co Ltd, 2 batches of Xinjiang pharmaceutical Co Ltd in national pharmaceutical group, 1 batch of Qinghai Baozhen Tang national pharmaceutical Co Ltd, and 1 batch of Yuanxi Zhengdong Kaiyuan pharmaceutical Co Ltd, are not in compliance with the regulations.
The method comprises the steps of measuring 31 repeated batches of Tianwang Buxin pills (concentrated pills) of 8 enterprises, wherein 1 batch of each of fried spina date seed, Jiangxi medicine, Duzhang camphor tree pharmaceutical company and Maanshan Tianfukang pharmaceutical company do not meet the regulations; there were 11 lots of nonconforming specifications for polygala tenuifolia (4 lots of Jiangxi Yadu camphor tree pharmaceutical Co., Ltd.; 3 lots of Zhongjingtongxi pharmaceutical Co., Ltd.; 1 lot of each of Anhui Tai Enkang pharmaceutical Co., Ltd., sunflower pharmaceutical group (Xiangyang) Longzhong Co., Ltd., Maanshan Tianfu kang pharmaceutical Co., Ltd., Nanjing Tongren Tang pharmaceutical Co., Ltd.); the fructus Schisandrae 7 batches are not in compliance (Jiangxi Yadu camphor tree pharmaceutical Co., Ltd. 4 batches; Shanghai Jinzai Kan Lankan pharmaceutical Co., Ltd., Maanshan Tianfukang pharmaceutical Co., Ltd., Nanjing Tongrentang pharmaceutical Co., Ltd. 1 batch each).
6. Discussion and analysis
The content determination method of the Tianwang heart tonifying preparation uses the ultra-high performance liquid chromatography to simultaneously determine the contents of the spinosin in the fried spina date seed and the schisandrin in the prepared polygala tenuifolia in the Tianwang heart tonifying preparation, the 6' -dibapinyl sucrose and the schisandrin in the schisandra chinensis, compared with the method of determining the content of the schisandrin only in the 2020 edition of Chinese pharmacopoeia, the method can more comprehensively reflect the quality of medicines, and the ultra-high performance liquid chromatography is used, so that the analysis time is shorter, and the solvent dosage is less.
Claims (2)
1. A content determination method of a Tianwang heart tonifying preparation is characterized in that the Tianwang heart tonifying preparation comprises a Tianwang heart tonifying pill and a Tianwang heart tonifying pill (concentrated pill), the determination method is to simultaneously perform content determination on 3, 6' -dibastin acyl sucrose, spinosin and schizandrol A contained in the Tianwang heart tonifying preparation under the same chromatographic condition, and the specific method comprises the following steps:
(1) chromatographic conditions and system applicability test: octadecylsilane chemically bonded silica is used as a filler, Agilent Eclipse Plus C18, 1.8 mu m and 2.1 multiplied by 100 mm; acetonitrile is taken as a mobile phase A, water is taken as a mobile phase B, and gradient elution is carried out according to the specification in the following table 1; flow rate 0.2ml per minute; the detection wavelength is 335nm and 250 nm; the number of theoretical plates is not less than 30000 calculated according to schizandrol A peak;
(2) preparation of control solutions: accurately weighing appropriate amount of spinosin reference substance, 3,6 '-dibapinyl sucrose reference substance, and schizandrol A reference substance, and adding 80% methanol to obtain mixed reference substance solution containing 10 μ g of spinosin, 10 μ g of 3, 6' -dibapinyl sucrose, and 80 μ g of schizandrol A per 1 ml;
(3) preparation of test solution
Tianwang Buxin Wan: taking a water-honeyed pill of the product, grinding, taking 4g, and precisely weighing; or cutting honeyed pill into pieces, and precisely weighing 5g of the honeyed pill; or cutting large honeyed pill with different weights into pieces, and precisely weighing 5g of the honeyed pill; placing in a conical flask with a plug, adding 20ml of 80% methanol solution precisely, weighing, heating and refluxing for 2 hr, taking out, cooling, weighing again, supplementing the weight loss with 80% methanol solution, shaking, filtering with 0.22 μm filter membrane, and collecting the filtrate;
tianwang Buxin pills (concentrated pills): precisely weighing 1.5g of the product, placing the product in a conical flask with a plug, precisely adding 20ml of 80% methanol solution, and weighing; ultrasonic extraction is carried out for 60 minutes, the ultrasonic power is 320W, and the frequency is 40 kHz; taking out, cooling, weighing, shaking, filtering with 0.22 μm filter membrane, and collecting the filtrate;
(4) and (3) determination: precisely sucking 2 μ l of the reference solution and the sample solution, respectively, injecting into an ultra-high performance liquid chromatograph, and measuring.
2. The method for measuring the content of the Tianwang Buxin preparation according to claim 1,
tianwang Buxin Wan: the product contains parched semen Ziziphi Spinosae and spinosin (C)28H32O15) Measured, every 1g of the water-honeyed pill is not less than 0.035 mg; 1g of small honeyed pill should not be less than 0.027 mg; the size of big honeyed pill should not be less than 0.24mg; contains 3, 6' -mustard acyl sucrose (C) as polygala root36H46O17) Measured, every 1g of the water-honeyed pill is not less than 0.065 mg; 1g of small honeyed pill should not be less than 0.050 mg; the content of big honeyed pill should not be less than 0.45mg per pill; schisandra chinensis and schizandrol A (C)24H32O7) Measured, every 1g of the water-honeyed pill is not less than 0.19 mg; 1g of small honeyed pill should not be less than 0.13 mg; the content of big honeyed pill should not be less than 1.22mg per pill;
tianwang heart tonifying pill (concentrated pill): the product contains parched semen Ziziphi Spinosae and spinosin (C)28H32O15) Measured by no less than 30.9 mug per 1 g; contains 3, 6' -mustard acyl sucrose (C) as polygala root36H46O17) Not less than 44.6 μ g per 1 g; the schisandra fruit is prepared with schisandrin A (C)24H32O7) It should be measured that the content of the compound should not be less than 93.4. mu.g per 1 g.
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