CN113189245B - Platycodon grandiflorum soup material standard and establishing method thereof - Google Patents
Platycodon grandiflorum soup material standard and establishing method thereof Download PDFInfo
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- CN113189245B CN113189245B CN202110523162.3A CN202110523162A CN113189245B CN 113189245 B CN113189245 B CN 113189245B CN 202110523162 A CN202110523162 A CN 202110523162A CN 113189245 B CN113189245 B CN 113189245B
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Abstract
The invention relates to a platycodon grandiflorum decoction material standard and an establishment method thereof, belonging to the field of traditional Chinese medicine pharmacy quality standard control. The invention carries out decoction and extraction on the platycodon root decoction according to the ancient book prescription, and adopts the modern concentration and drying process to prepare the platycodon root decoction for the first time. The invention also establishes the fingerprint of the platycodon grandiflorum decoction substance standard, the similarity between the platycodon grandiflorum decoction substance standard fingerprint and the comparison fingerprint is as high as 0.940-0.994, the platycodon grandiflorum decoction substance standard fingerprint has strong representativeness, and the platycodon grandiflorum decoction substance standard fingerprint can be used for controlling the quality of the platycodon grandiflorum decoction substance standard. The platycodon grandiflorum decoction substance standard and the established platycodon grandiflorum decoction substance standard fingerprint spectrum have wide application prospects in preparation process and quality control of a novel platycodon grandiflorum decoction substance standard medicinal preparation. The invention also provides a method for measuring the magnitude transfer relationship from the decoction pieces of the index components in the platycodon grandiflorum decoction to the platycodon grandiflorum decoction and then to the platycodon grandiflorum decoction substance standard, and the method is suitable for the whole process system research of the platycodon grandiflorum decoction substance standard.
Description
Technical Field
The invention relates to a platycodon root decoction material standard and an establishment method thereof, belonging to the field of Chinese medicine pharmacy quality standard control.
Background
The development of the classical Chinese medicine famous prescription becomes one of the hot spots of the research in the traditional Chinese medicine field, and the successful development of the material standard of the classical Chinese medicine famous prescription is very critical to the declaration of the whole classical Chinese medicine famous prescription. In 29 months in 2018, the national drug administration issued the simplified registration approval management regulations of ancient classic famous Chinese medicine compound preparations (hereinafter referred to as regulations). The regulation defines two stages of the preparation development of the ancient classic famous prescription: the standard development of the materials of the classical famous prescription and the preparation development. The standard of the classical famous prescription substance is an important medicinal substance standard obtained by referring to the preparation method of the classical famous prescription in ancient books, and the preparation methods except the molding process are basically consistent with the records of the ancient books. Specifically, the material standard of the classical famous prescription is that the quality of raw medicinal materials is controlled from the source by taking the traditional Chinese medicine theory as guidance and clinical application as a basis and combining the traditional preparation method with the modern scientific technology, and the extract with uniform, stable and controllable quality is prepared by the standardized processes of medicinal material pretreatment, decoction piece processing, decoction, concentration, drying and molding and the like. The material standard of the classical famous prescription is not only the standard for detecting the quality of the classical famous prescription preparation, but also the material basis of the whole prescription needs to be reflected. The key to the successful research and development of the classical famous prescription is to break through the quality control technology of the traditional Chinese medicine classical famous prescription based on the substance and to comprehensively and accurately illustrate the transfer rule of the medicinal material-decoction piece-substance based component group quantity value.
The platycodon root decoction consists of platycodon root and liquorice, and is obtained from the miscellaneous diseases part of Shangzhongjing Shang Han Lun (golden lack of essence, japan): one or two platycodons and two or two liquorice. The second one is decocted with three liters of water, one liter is taken after being warmed, and pus and blood are spitted out when the decoction is taken again, which is mainly indicated for treating pulmonary abscess, cough with fullness in chest, rapid pulse due to cold, dry throat without thirst, turbid saliva with stinking smell, and pus spitting for a long time like rice gruel. Wherein, the balloonflower root is pungent and bitter and has the functions of dispersing lung qi and eliminating phlegm, relieving sore throat and expelling pus; licorice root, radix Glycyrrhizae is sweet and neutral, and has effects of invigorating heart and spleen qi, eliminating phlegm, relieving cough, relieving spasm, relieving pain, and removing toxic heat and toxic food. The two medicines are compatible to bring out the best in each other, the liquorice discharges fire and detoxifies to treat the root cause, the platycodon grandiflorum ventilates lung qi, eliminates phlegm and expels pus, and the root cause and symptoms are considered simultaneously, so the functions of dispersing lung and relieving cough, relieving sore throat and detoxifying, and eliminating phlegm and expelling pus are enhanced.
The modern clinical application of a large amount of platycodon root decoction for treating various diseases reports that 48 cases of acute and chronic pharyngitis are treated by the platycodon root and liquorice decoction in Dengshen, the total effective rate is 97.91 percent, and 57 cases of chronic aphonia are treated by adding flavor to the platycodon root and liquorice decoction in Jie. Clinical observation shows that the total effective rate is 92.98%. The Yang quan Sheng adopts Zibai gan Ju Tang to treat exogenous cough for 26 cases. The result is that 16 cases are cured, accounting for 61.54 percent, 10 cases are improved, accounting for 38.46 percent, and the total effective rate is 100.00 percent. Meanwhile, the scholars deeply research the drug effect and the synergistic mechanism of the synergistic compatibility of the platycodon grandiflorum and the liquorice, and the results show that the platycodon grandiflorum and the liquorice have the synergistic effect on the aspects of anti-inflammation and phlegm elimination. For example, the research on Liu Bin shows that the glycyrrhizin and the platycodin can obviously inhibit mouse ear swelling caused by dimethylbenzene and improve mouse tracheal phenol red excretion amount when being used singly or jointly in a certain dosage range, the two medicines show synergistic action, the mechanism is that the platycodon root and the glycyrrhizin synergistically inhibit the production of TNF-alpha and PGE2 in macrophage and show dosage dependence.
At present, most researches on platycodon grandiflorum decoction are focused on pharmacological researches and modern extraction process researches, the ancient preparation method of platycodon grandiflorum decoction, the fingerprint spectrum of the platycodon grandiflorum decoction and the magnitude transfer relationship of effective components of the platycodon grandiflorum decoction are rarely researched, and the reference of platycodon grandiflorum decoction is not reported at present. Therefore, aiming at the current situation that the conventional famous radix platycodonis decoction quality evaluation method is insufficient, establishing a radix platycodonis decoction standard has important significance for promoting the development of the formulated preparation.
Disclosure of Invention
Aiming at the current situation that the conventional famous radix platycodonis soup quality evaluation method is insufficient, one of the purposes of the invention is to provide a radix platycodonis soup substance standard fingerprint spectrum, an establishment method and application thereof, and the other purpose of the invention is to provide a radix platycodonis soup substance standard, an establishment method and application thereof.
The invention provides a balloonflower decoction substance-based fingerprint, which is characterized in that: the fingerprint contains characteristic peaks of apioside liquiritin, apioside isoliquiritin, glycyrrhizic acid and platycodin.
Furthermore, the fingerprint contains more than 30 characteristic peaks.
Further, the fingerprint is shown in fig. 2 b.
The invention also provides an establishment method of the fingerprint, which comprises the steps of taking the balloonflower root decoction substance reference, preparing into balloonflower root decoction substance reference solution, and establishing the fingerprint of the balloonflower root decoction substance reference by adopting a high performance liquid chromatography-evaporative light scattering detection method;
wherein the chromatographic conditions of the high performance liquid chromatography are as follows:
and (3) chromatographic column: octadecylsilane chemically bonded silica is used as a filling agent,
mobile phase: a phase is 0.05 to 0.5 percent of formic acid aqueous solution, B phase is acetonitrile,
the gradient elution conditions are shown in the following table:
in the table, B% represents the volume percentage of the B phase in the mobile phase;
the parameters of the evaporative light scattering detection are as follows: drift tube temperature100～110℃,N 2 The pressure is 12-15 psi;
preferably, the volume percentage of the phase B in the mobile phase between each two adjacent time points in the gradient elution condition is constant along time; phase A is 0.1% formic acid water solution; the flow rate is 0.8-1.2 mL/min, the column temperature is 28-35 ℃, and the sample injection amount is 10 mu L; the parameters of the evaporative light scattering detection are as follows: drift tube temperature 108 deg.C, N 2 Pressure 13.8psi.
Further, the preparation method of the platycodon grandiflorum soup substance reference solution comprises the following steps: taking radix Platycodi soup as reference, adding water to dissolve, adding methanol, ultrasonic extracting, centrifuging, filtering, collecting supernatant, evaporating to dryness, adding water to dissolve residue, adding anhydrous ethanol, standing overnight, centrifuging, filtering, evaporating to dryness, and adding methanol to dissolve;
preferably, the preparation method of the platycodon grandiflorum soup substance reference solution comprises the following steps: taking 1-2 g of platycodon grandiflorum soup substance as a reference in a 50mL volumetric flask, adding 10-30 mL of pure water to dissolve the platycodon grandiflorum soup substance, adding methanol to the scale of the volumetric flask, ultrasonically extracting for 10min, centrifugally filtering, taking supernatant, evaporating to dryness, adding 10-20 mL of water into residues, adding absolute ethanol to a volume of 50mL volumetric flask, standing overnight, centrifuging, filtering, evaporating to dryness, adding 50% methanol to a volume of 5mL volumetric flask to obtain the platycodon grandiflorum soup substance.
The invention also provides a platycodon grandiflorum soup substance standard, and the fingerprint spectrum of the platycodon grandiflorum soup substance standard is as described above.
Further, the method for establishing the platycodon root soup material standard comprises the following steps:
(1) Preparing platycodon root soup: decocting radix Platycodi and Glycyrrhrizae radix in water to obtain decoction, and filtering to obtain radix Platycodi decoction; the mass ratio of the platycodon root medicinal materials to the liquorice medicinal materials is 1:2, the mass-volume ratio of the total mass of the platycodon root medicinal material and the liquorice root medicinal material to the water is 1:14g/mL, wherein the volume ratio of the decoction to water is 1:3;
(2) Preparing a platycodon grandiflorum soup substance standard: and (3) taking the platycodon grandiflorum decoction obtained in the step (1), concentrating to obtain a concentrated decoction, and drying to obtain a platycodon grandiflorum decoction substance standard.
Further, the method for establishing the platycodon grandiflorum soup material standard comprises the following steps:
(1) Preparing platycodon root soup: taking 14g of platycodon grandiflorum decoction pieces and 28g of liquorice decoction pieces, adding 600mL of water, decocting to 200mL of decoction, and filtering to obtain platycodon grandiflorum decoction;
(2) Preparing a platycodon grandiflorum soup substance standard: taking the platycodon grandiflorum soup obtained in the step (1), and performing rotary evaporation by using a rotary evaporator to obtain a concentrated soup with the volume of 30-50 mL; and (5) carrying out freeze drying to obtain the reference substance of the platycodon root decoction.
Further, in the step (1), the decocting conditions are as follows: soaking for 15 min-1 h before decocting, then using an electric furnace to cover for decocting, boiling with strong fire, and then decocting with slow fire to 200mL of decoction; the power of the strong fire is 1000W-2000W, and the power of the slow fire is 50W-100W; and/or the filtration uses a sieve cloth with 50 meshes to 400 meshes;
and/or in the step (2), the rotary evaporation conditions are as follows: steaming at vacuum degree of 0.06-0.10 Mpa, temperature of 40-60 deg.C and rotation speed of 40-80 rpm;
and/or, the freeze-drying conditions are: the temperature of the condenser is minus 80 ℃ to minus 40 ℃, the vacuum degree is 150 mT to 250mT, the pre-freezing temperature is minus 55 ℃ to minus 35 ℃, the pre-freezing time is 1h to 5h, the sublimation temperature is minus 30 ℃ to minus 10 ℃, the sublimation time is 10h to 24h, the desorption drying temperature is 10 ℃ to 35 ℃, and the desorption drying time is 1h to 5h;
preferably, in the step (1), the decocting conditions are as follows: soaking for 30min before decocting, decocting with electric stove cover, boiling with strong fire, and decocting with slow fire to obtain 200mL decoction; the power of strong fire is 1200W, and the power of slow fire is 50W; and/or, the filtration uses a 100 mesh screen cloth;
and/or in the step (2), the rotary evaporation conditions are as follows: steaming at the vacuum degree of 0.08Mpa, the temperature of 50 ℃ and the rotating speed of 60 rpm;
and/or, the freeze-drying conditions are: the condenser temperature is-60 deg.C, the vacuum degree is 200mT, the pre-freezing temperature is-45 deg.C, the pre-freezing time is 3h, the sublimation temperature is-20 deg.C, the sublimation time is 18h, the desorption drying temperature is 30 deg.C, and the desorption drying time is 3h.
Further, the paste yield of the platycodon grandiflorum soup based on the substance standard is 21.41%.
The paste yield = M/M × 100%, wherein M is the mass of the platycodon grandiflorum decoction reference substance, and M is the feeding amount of the decoction pieces.
The invention also provides application of the fingerprint and the platycodon grandiflorum decoction substance standard in platycodon grandiflorum decoction quality control.
The invention also provides a method for measuring the quantity value transfer relationship of the index components in the platycodon grandiflorum decoction, which comprises the following steps:
(a) Establishing a material standard of the platycodon grandiflorum decoction;
(b) Measuring the magnitude transmission relation of the index components: according to chromatographic conditions for detecting index components under the items of detecting the index components on 277 th pages of Chinese pharmacopoeia of 2015 edition and detecting the index components on 86 th to 87 th pages of liquorice, respectively measuring the content of the index components on the basis of platycodon grandiflorum, liquorice and platycodon grandiflorum soup, and calculating the transfer rate according to a formula, wherein the transfer rate is = (W × M)/(W × M) × 100%, W is the content of the index components in the platycodon grandiflorum soup, M is the reference sample amount of the platycodon grandiflorum soup, W is the content of the index components in the medicinal materials, and M is the feeding amount of the medicinal materials;
the index components are 1 or more than 2 of apioside liquiritin, apioside isoliquiritin, isoliquiritigenin, glycyrrhizic acid, and platycodin D.
Further, the medicinal materials are decoction pieces or powder.
The invention also provides an establishment method of the platycodon grandiflorum decoction substance standard, a fingerprint of the platycodon grandiflorum decoction substance standard, and application of the establishment method of the fingerprint in preparation process and quality control of a novel medicinal preparation of the platycodon grandiflorum decoction substance standard.
In the present invention, the vacuum degree unit mT is an abbreviation of millitorr (mTorr).
In the prescription of the invention, the platycodon root decoction pieces and the liquorice decoction pieces are all cut into raw products. The identification meets the relevant regulation under one item of 'Chinese pharmacopoeia' 2015 edition.
Unless otherwise specified, all percentages of the liquids of the present invention are by volume.
The invention is based on the traditional extraction process recorded in ancient medical books, adopts the modern preparation method for concentration and drying, develops the reference of the platycodon root decoction substance, and establishes the fingerprint spectrum of the reference of the platycodon root decoction substance.
Compared with the prior art, the invention has the following advantages:
(1) The invention carries out decoction and extraction on the platycodon root decoction according to ancient book prescriptions, adopts modern concentration and drying processes, and firstly prepares the platycodon root decoction material standard;
(2) The invention establishes HPLC-ELSD fingerprint spectrum of the reference of the platycodon grandiflorum decoction substance, marks 37 chromatographic peaks in total, and identifies 7 chromatographic peaks in the chromatographic peaks by a reference substance: peak 7 is apioside liquiritin, peak 8 is liquiritin, peak 11 is apioside isoliquiritin, peak 13 is isoliquiritin, peak 15 is liquiritigenin, peak 30 is glycyrrhizic acid, and peak 17 is platycodin D;
(3) The similarity between the established platycodon grandiflorum decoction substance reference fingerprint and the reference fingerprint is as high as 0.940-0.994, the fingerprint has strong representativeness, and the method can be used for performing quality control on the platycodon grandiflorum decoction substance reference;
(4) The built platycodon grandiflorum soup substance standard fingerprint spectrum can not only control the quality of the platycodon grandiflorum soup substance standard, but also control the quality of a platycodon grandiflorum medicinal material and a liquorice medicinal material simultaneously;
(5) The invention also provides a method for measuring the magnitude transfer relationship of the index component in the platycodon grandiflorum decoction from the decoction pieces to the platycodon grandiflorum decoction and then to the substance standard of the platycodon grandiflorum decoction.
The platycodon grandiflorum decoction substance standard and the established platycodon grandiflorum decoction substance standard fingerprint spectrum have wide application prospects in preparation process and quality control of a novel platycodon grandiflorum decoction substance standard medicinal preparation.
Obviously, many modifications, substitutions, and variations are possible in light of the above teachings of the invention, without departing from the basic technical spirit of the invention, as defined by the following claims.
The present invention will be described in further detail with reference to the following examples. This should not be understood as limiting the scope of the above-described subject matter of the present invention to the following examples. All the technologies realized based on the above contents of the present invention belong to the scope of the present invention.
Drawings
FIG. 1: a.15 appearance of decoction of radix Platycodi decoction; b.15 appearance of batch of radix Platycodi soup.
FIG. 2: the reference fingerprint of the platycodon root decoction substance is as follows: a. mixing the reference substance maps; b. a platycodon grandiflorum soup substance reference map common mode; wherein 7 represents apigenin, 8 represents liquiritin, 11 represents apigenin, 13 represents isoliquiritin, 15 represents glycyrrhizin, 17 represents platycodin D, and 30 represents glycyrrhizic acid.
FIG. 3:15 batches of platycodon grandiflorum soup material standard similarity maps.
FIG. 4: spectrum of chromatographic peak assignment relationship of each sample: a is the reference of the platycodon root decoction, b is a liquorice medicinal material, and c is a platycodon root medicinal material.
Detailed Description
The raw materials and equipment used in the invention are known products, and are obtained by purchasing products sold in the market.
Example 1: preparation of Platycodon grandiflorum decoction
1.1 preparation of Platycodon grandiflorum decoction base
Weighing 14g of platycodon grandiflorum decoction pieces and 28g of liquorice decoction pieces, adding 600mL of water, soaking for 30min, and using an electric furnace as a heat source to perform covered decocting by using a pottery pot with a diameter-height ratio of 0.8-1.5, wherein the firepower program comprises the following steps: boiling with strong fire (1200W), and decocting with slow fire (50W) to obtain 200mL decoction (named as platycodon grandiflorum decoction). Filtering with 100 mesh sieve, squeezing the medicinal materials to collect decoction, and rotary evaporating with rotary evaporator at vacuum degree of 0.08Mpa, temperature of 50 deg.C and rotation speed of 60rpm to obtain 40mL concentrated decoction. Freeze-drying the concentrated soup, wherein the freeze-drying process comprises the following steps: the condenser temperature is-60 deg.C, vacuum degree is 200mT, prefreezing temperature is-45 deg.C, prefreezing is 3h, sublimation temperature is-20 deg.C, sublimation time is 18h, resolution drying temperature is 30 deg.C, resolution drying time is 3h, to obtain radix Platycodi soup standard.
1.2 determination of cream yield
The platycodon root soup material standard under the item 1.1 is taken, precision weighing is carried out, and the calculated cream yield is 21.41%.
The paste yield = M '/M' × 100%, wherein M 'is the mass of the dried platycodon root decoction, and M' is the total mass of the dried platycodon root decoction pieces and the liquorice root decoction pieces.
Example 2: establishment of reference fingerprint of platycodon grandiflorum decoction
Establishing fingerprint of radix Platycodi soup reference by high performance liquid chromatography-evaporative light scattering detection method (HPLC-ELSD), specifically operating as follows:
1 chromatographic conditions
High performance liquid chromatography parameters: phenomenex Luna C18 (2) column (4.6X 250mm,5 μm) column, mobile phase 0.1% formic acid aqueous solution (A) -acetonitrile (B), gradient elution gradient program (as shown in Table 1): 0-5 minutes, 10% -15% by weight of B; 5-25 minutes, 15% -19% by weight of B; 25-32 minutes, 19% -28% by weight of B; 32-57 minutes, 28% -35% by weight of B; 57-67 minutes, 35% -65% by weight of B; 67-69 minutes, 65% -10% by weight B;69 to 75 minutes, 10 to 10% by weight of B. The flow rate is 1.0mL/min, the column temperature is 30 ℃, and the sample injection amount is 10 mu L.
Evaporative Light Scattering Detector (ELSD) parameters: drift tube temperature 108 ℃, N 2 Pressure 13.8psi.
TABLE 1 fingerprint gradient elution procedure
2 preparation of test solution
Taking about 2g of platycodon grandiflorum soup substance reference powder prepared in example 1 into a 50mL volumetric flask, adding 25mL of pure water for redissolving, adding methanol to scale, performing ultrasonic extraction for 10min, performing centrifugal filtration, taking 20mL of supernatant for evaporation, adding 15mL of water into residue, adding absolute ethanol to a volume of 50mL volumetric flask (the alcohol content is 70%), standing overnight, performing centrifugation, filtration and evaporation, and adding 50% methanol to a volume of 5mL volumetric flask to obtain a test solution.
3 preparation of Mixed control solutions
Taking appropriate amount of apioside liquiritin, apioside isoliquiritin, isoliquiritigenin, platycodin D and monoammonium glycyrrhizinate as reference substances, precisely weighing, and adding methanol to obtain mixed reference substance solutions with concentrations of 40, 50, 60, 70, 55, 40 and 100 μ g/mL respectively.
4 establishing of fingerprint and determining of characteristic peak
Respectively sucking the test solution and the mixed reference solution, and establishing the reference fingerprint of the platycodon grandiflorum decoction by adopting the chromatographic conditions under item 1. 37 chromatographic peaks are marked in the fingerprint of the radix platycodi decoction standard (figure 2 b).
Further comparing the fingerprint of the radix platycodi soup material standard with the spectrum of the mixed reference solution, and carrying out identification through comparison of retention time of chromatographic peaks (figure 2): in the fingerprint of radix Platycodi soup material standard, peak 7 is apioside liquiritin, peak 8 is liquiritin, peak 11 is apioside isoliquiritin, peak 13 is isoliquiritin, peak 15 is liquiritigenin, peak 30 is glycyrrhizic acid, and peak 17 is platycodin D.
Example 3: application of platycodon grandiflorum decoction substance reference fingerprint in quality control of platycodon grandiflorum medicinal material and liquorice medicinal material
In the same chromatographic conditions as in example 2, spectrograms of platycodon grandiflorum and liquorice are tested, and the specific operation is as follows:
1 chromatographic conditions
While working 2.
2 preparation of test solution
Respectively taking about 2g of platycodon grandiflorum decoction pieces and liquorice decoction pieces in a 50mL volumetric flask, adding 25mL of pure water for redissolution, adding methanol to the scales, carrying out ultrasonic extraction for 10min, carrying out centrifugal filtration, taking 20mL of supernatant for evaporation, adding 15mL of water into residues, adding absolute ethyl alcohol for constant volume till the volume of a 50mL volumetric flask (the alcohol content is 70%), standing overnight, centrifuging, filtering, evaporating to dryness, adding 50% of methanol for constant volume till the volume of a 5mL volumetric flask, and obtaining a platycodon grandiflorum medicinal material test solution and a liquorice medicinal material test solution.
3 establishing of fingerprint and determining of characteristic peak
Respectively sucking a licorice medicinal material test solution and a platycodon root medicinal material test solution, and testing by adopting the chromatographic conditions under item 1.
Spectrograms of the Glycyrrhrizae radix and radix Platycodi test solutions are shown in fig. 4b and 4 c. The retention time of the common peak in the fingerprint of the platycodon grandiflorum soup substance standard established in the example 2 is found (fig. 4): in the fingerprint of the radix platycodi decoction substance standard, 13 common peaks come from the radix platycodi medicinal material, 24 common peaks come from the liquorice medicinal material, and the substance bases of the radix platycodi medicinal material and the liquorice medicinal material are completely transmitted to the radix platycodi decoction substance standard.
The result shows that the platycodon grandiflorum soup substance standard fingerprint established by the invention can not only control the quality of the platycodon grandiflorum soup substance standard, but also control the quality of the platycodon grandiflorum medicinal material and the liquorice medicinal material.
Example 4: method for measuring magnitude transfer relationship of index components of platycodon grandiflorum decoction
1. Sample (I)
15 batches of platycodon grandiflorum soup base material reference, numbered S1 to S15, respectively, were prepared according to the method of example 1. The appearance photographs of 15 batches of decoction of radix Platycodi decoction and radix Platycodi decoction are shown in FIG. 1.
Taking the following samples when 15 batches of platycodon root soup are subjected to substance reference respectively: platycodon grandiflorum decoction pieces, liquorice decoction pieces, platycodon grandiflorum decoction liquid and platycodon grandiflorum decoction substance standard.
2. Method for testing transfer rate of index component
According to chromatographic conditions for detecting platycodin D, liquiritin and glycyrrhizic acid under the items of 277 (platycodon grandiflorum) and 86-87 (liquorice) in 'Chinese pharmacopoeia' 2015 edition, the contents of the platycodin D, the liquiritin and the glycyrrhizic acid in platycodon grandiflorum decoction pieces, platycodon grandiflorum decoction liquid and platycodon grandiflorum decoction substance standard are respectively measured, and the transfer rate is calculated according to the following formula: transfer rate = (W × M)/(W × M) × 100%,
wherein W represents the content of the index component in the product sample, M represents the product sample amount, W represents the content of the index component in the raw material sample, and M represents the charged amount of the raw material sample.
For example, when calculating the transfer rate of the index component from the decoction pieces to the platycodon root decoction, W represents the content of the index component in the platycodon root decoction, M represents the sample size of the platycodon root decoction, W represents the content of the index component in the decoction pieces, and M represents the feeding amount of the decoction pieces; when the transfer rate of the index components from the platycodon grandiflorum decoction to the platycodon grandiflorum decoction material standard is calculated, W represents the content of the index components in the platycodon grandiflorum decoction material standard, M represents the platycodon grandiflorum decoction material standard sample size, W represents the content of the index components in the platycodon grandiflorum decoction, and M represents the feeding amount of the platycodon grandiflorum decoction.
3. Results of the experiment
The results show that: in 15 batches of samples, the average transfer rates of liquiritin, glycyrrhizic acid and platycodin D from decoction pieces to decoction pieces of platycodon grandiflorum decoction are respectively 25.95%,20.21% and 51.58%, and the RSD is 16.30%,19.03% and 17.63%; the average transfer rates of glycyrrhizin, glycyrrhizic acid and platycodin D from the decoction of the platycodon root decoction to the standard of the platycodon root decoction are respectively 95.43 percent, 95.33 percent, 97.87 percent and RSD are respectively 5.03 percent, 4.19 percent and 6.51 percent.
The above results show that, in the process of establishing the reference of the platycodon grandiflorum decoction substance of the present invention, the index components platycodin D, liquiritin and glycyrrhizic acid are basically stable from the decoction pieces to the decoction of the platycodon grandiflorum decoction and then to the reference of the platycodon grandiflorum decoction substance, and no discrete data (the discrete data refers to data other than 70-130% of the average value) appears.
The method provided by the invention can accurately measure the quantity transfer relationship of the index components from the decoction pieces to the platycodon grandiflorum decoction (equivalent to the intermediate for preparing the platycodon grandiflorum decoction substance standard) to the substance standard, so that the quantity transfer relationship of the index components between the decoction pieces-the intermediate-the substance standard is clear, and the method is suitable for the whole-process systematic research of the platycodon grandiflorum decoction substance standard.
The beneficial effects of the present invention are demonstrated by the following experimental examples.
Experimental example 1: methodology investigation
15 batches of the platycodon grandiflorum soup obtained in example 4 (nos. S1 to S15) were used as samples.
(1) Precision test
A sample No. S5 is randomly taken to prepare a test solution according to the method of the example 2, HPLC-ELSD measurement is continuously carried out for 6 times under the same chromatographic conditions of the example 2, and the relative retention time of the common peak of the spectrum obtained by 6 times of measurement and the RSD of the relative peak area are calculated.
The result shows that the RSD of the relative retention time of the common peak of the spectrums obtained by 6 times of tests is less than 1 percent, and the RSD of the relative peak area is less than 3 percent, which indicates that the precision of the instrument is good.
(2) Stability test
A reference sample of platycodon grandiflorum soup substance is taken, a test solution is prepared according to the method of the embodiment 2, and after the test solution is respectively kept still for 0,2,4,8,12 and 24h at room temperature, the measurement is carried out under the same chromatographic conditions of the embodiment 2, and the relative retention time of the common peak of each spectrum obtained by the test and the RSD of the relative peak area are calculated.
The results show that the RSD of the relative retention time of the common peak of each map is less than 1 percent, and the RSD of the relative peak area is less than 3 percent, which indicates that the test solution is stable within 24 hours.
(3) Repeatability test
6 parts of test solution is prepared in parallel according to the method of the embodiment 2 by taking the reference freeze-dried powder of the platycodon grandiflorum soup substance, the determination is carried out under the same chromatographic conditions of the embodiment 2, and the relative retention time of the common peak of the chromatogram obtained by 6 times of tests and the RSD of the relative peak area are calculated.
The result shows that RSD of relative retention time of each common peak of the obtained maps in 6 times of tests is less than 1%, and RSD of relative peak area is less than 3%, which indicates that the method has good repeatability.
Experimental example 2: similarity evaluation of fingerprint spectrum of platycodon grandiflorum soup substance standard
The 15 batches of platycodon grandiflorum soup base materials numbered from S1 to S15 in example 4 were tested according to the method of example 2, and 15 fingerprints were obtained.
Introducing 15 batches of radix platycodi decoction substance standard fingerprint data into software of a traditional Chinese medicine chromatogram fingerprint similarity evaluation system (2012 edition), setting a reference spectrum, automatically matching, generating a fingerprint and a reference fingerprint by adopting a median method, and calibrating 37 total peaks in the radix platycodi decoction substance standard fingerprint by taking glycyrrhizic acid (No. 30 peak) as a reference peak S and taking the relative retention time and the relative peak area of the glycyrrhizic acid as standards. The relative retention time and relative peak area of each common peak were calculated (see tables 2 and 3). And calculating the similarity by adopting an automatic matching mode.
TABLE 2, 15 relative retention time of samples
TABLE 3, 15 relative peak areas of the batches
Table 4, 15 batch sample similarity data
The results show that: the similarity between the standard fingerprint of 15 batches of platycodon grandiflorum soup substances and the generated contrast fingerprint is as high as 0.940-0.994 (see table 4 and figure 3).
The results show that the platycodon grandiflorum soup substance standard preparation process established by the invention is stable, and the difference between substance groups is small. Moreover, the similarity between the reference fingerprint of the platycodon grandiflorum decoction substance and the comparison fingerprint established by the invention is as high as 0.940-0.994, and the method has strong representativeness and can be used for controlling the quality of the reference substance of the platycodon grandiflorum decoction.
In conclusion, the platycodon grandiflorum decoction is decocted and extracted according to the ancient book prescription, and the platycodon grandiflorum decoction is prepared for the first time according to the quality standard by adopting the modern concentration and drying process. The invention also establishes the fingerprint of the platycodon grandiflorum decoction substance standard, the similarity between the platycodon grandiflorum decoction substance standard fingerprint and the comparison fingerprint is as high as 0.940-0.994, the fingerprint has strong representativeness, and the method can be used for carrying out quality control on the platycodon grandiflorum decoction substance standard. The prepared platycodon grandiflorum decoction substance standard and the established platycodon grandiflorum decoction substance standard fingerprint have wide application prospects in preparation process and quality control of a novel platycodon grandiflorum decoction substance standard medicinal preparation. The invention also provides a method for measuring the magnitude transfer relationship of the index components in the platycodon grandiflorum decoction from decoction pieces to the platycodon grandiflorum decoction and then to the platycodon grandiflorum decoction substance standard, and the method is suitable for the whole-process systematic research of the platycodon grandiflorum decoction substance standard.
Claims (4)
1. A method for establishing a fingerprint spectrum of a platycodon grandiflorum decoction substance standard is characterized by comprising the following steps: taking a platycodon grandiflorum decoction substance standard, preparing a platycodon grandiflorum decoction substance standard solution, and establishing a fingerprint of the platycodon grandiflorum decoction substance standard by adopting a high performance liquid chromatography-evaporative light scattering detection method;
the preparation method of the platycodon grandiflorum soup substance reference solution comprises the following steps: taking the reference of platycodon grandiflorum decoction, adding water to dissolve, adding methanol, performing ultrasonic extraction, centrifuging and filtering, taking supernatant to dry, adding absolute ethyl alcohol to dissolve residues, standing overnight, centrifuging, filtering, drying by distillation, and adding a methanol water solution to dissolve to obtain the platycodon grandiflorum decoction;
the fingerprint contains characteristic peaks of apioside liquiritin, apioside isoliquiritin, glycyrrhizin, glycyrrhizic acid and platycodin;
the chromatographic conditions of the high performance liquid chromatography are as follows:
a chromatographic column: octadecylsilane chemically bonded silica is used as a filling agent,
mobile phase: the phase A is 0.05-0.5% formic acid water solution, the phase B is acetonitrile,
the gradient elution conditions are shown in the following table:
in the table, B% represents the volume percentage of the B phase in the mobile phase;
the parameters of the evaporative light scattering detection are as follows: the temperature of the drift tube is 100 to 110 ℃, N 2 Pressure of 12 to 15 psi.
2. The method of establishing according to claim 1, wherein: in the gradient elution condition, the volume percentage of the phase B in the mobile phase between every two adjacent time points is changed at a constant speed along with the time; phase A is 0.1% formic acid water solution; the flow rate is 0.8-1.2mL/min, the column temperature is 28-35 ℃, and the sample injection amount is 10 muL; the evaporative light scatteringThe parameters of the shot detection are: drift tube temperature 108 ℃, N 2 Pressure 13.8psi.
3. The method of establishing according to claim 1, wherein: the preparation method of the platycodon grandiflorum soup substance reference solution comprises the following steps: taking 1-2g of platycodon grandiflorum soup material in a 50mL volumetric flask, adding 10-30mL of pure water to dissolve the platycodon grandiflorum soup material, adding methanol to the scale of the volumetric flask, ultrasonically extracting for 10min, centrifugally filtering, taking supernatant, evaporating to dryness, adding 10-20 mL of water into residue, adding absolute ethyl alcohol to a volume of 50mL volumetric flask, standing overnight, centrifuging, filtering, evaporating to dryness, adding 50% methanol to a volume of 5mL volumetric flask, and obtaining the platycodon grandiflorum soup.
4. A method of establishing according to any one of claims 1-3, characterized by: the fingerprint also comprises more than 30 characteristic peaks.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101396425A (en) * | 2007-09-29 | 2009-04-01 | 曾雄辉 | Preparation method of ballon-flower decoction |
| CN109932437A (en) * | 2017-12-19 | 2019-06-25 | 四川济生堂药业有限公司 | A kind of detection method of pharmaceutical composition |
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| Publication number | Priority date | Publication date | Assignee | Title |
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-
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101396425A (en) * | 2007-09-29 | 2009-04-01 | 曾雄辉 | Preparation method of ballon-flower decoction |
| CN109932437A (en) * | 2017-12-19 | 2019-06-25 | 四川济生堂药业有限公司 | A kind of detection method of pharmaceutical composition |
Non-Patent Citations (4)
| Title |
|---|
| Quantitative and Chemical Fingerprint Analysis for the Quality Evaluation of Platycodi Radix Collected from Various Regions in China by HPLC Coupled with Chemometrics;Haiyang Lu等;《Molecules》;20180723;1-12 * |
| UPLC-Q-TOF-MS/MS快速分析杏贝止咳颗粒化学成分;张宁等;《中国中药杂志》;20180808(第22期);4439-4449 * |
| 基于标准汤剂的桔梗汤经典方制备工艺优化研究;张玉玲等;《辽宁中医药大学学报》;20191231;第21卷(第12期);52-56 * |
| 杏桔合剂的质量控制研究;赵学龙等;《江苏中医药》;20160505(第05期);70-73 * |
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