CN113759021A - Method for evaluating mass value transmission rule in honeysuckle and screening method - Google Patents
Method for evaluating mass value transmission rule in honeysuckle and screening method Download PDFInfo
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- G—PHYSICS
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- 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
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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
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8679—Target compound analysis, i.e. whereby a limited number of peaks is analysed
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Abstract
The invention provides a method for evaluating a quality value transmission rule in honeysuckle and a screening method, wherein the method comprises the following steps: evaluating the quantity value transfer rule of each substance of a sample prepared from the honeysuckle decoction pieces by adopting an evaluation index K value; the acquisition process of the K value is as follows: obtaining the dry paste amount of a sample prepared from honeysuckle decoction pieces; acquiring the decoction piece concentration of a decoction piece solution prepared from honeysuckle decoction pieces, the sample concentration of a sample solution prepared from a sample, and the fingerprint or characteristic spectrum of the decoction piece solution and the sample solution, and acquiring the decoction piece characteristic peak area and the sample characteristic peak area of corresponding characteristic peaks according to the acquired fingerprint or characteristic spectrum; the method comprises the steps of calculating the amount of dry paste, the characteristic peak area of decoction pieces, the characteristic peak area of samples, the concentration of the decoction pieces and the concentration of a sample to be tested. The K value can scientifically analyze the quality value transfer rule of the standard decoction, and the K value can be obtained without introducing a component reference substance, so that the analysis is simpler and more convenient.
Description
Technical Field
The invention relates to the field of traditional Chinese medicines, in particular to a method for evaluating quality value transmission regulation in honeysuckle and a screening method.
Background
As is known, the Chinese medicinal preparation keeps the characteristic of diversification of chemical components of the Chinese medicinal herbs, the effectiveness is the result of combined action of various chemical components, various chemical components in the Chinese medicinal preparation are required to be kept in certain relative proportion, the drug effect is difficult to be exerted if some components are too low, toxic and side effects are likely to be generated if some components are too high, and the Chinese medicinal preparation has potential safety hazard; the delivery of the chemical constituents should be controlled and the magnitude trends and magnitude ranges of the chemical constituents delivery should be described. During the process, attention is paid to whether phenomena such as conversion, degradation and the like exist in each component, and the transmission of chemical components is controlled. When the quantity value of the substance component is transferred lower, the component is relatively poor in transfer or decomposed (namely negative conversion) in the traditional Chinese medicine preparation, and if the component is a main active component, the control is needed in the production to ensure the clinical efficacy of the component; when the mass transfer value is obviously too high, the forward conversion process of the component in the traditional Chinese medicine preparation is enriched or exists, and the concentration or the forward conversion degree is mainly monitored and controlled, so that the safety of the clinical application of the component is ensured. Therefore, understanding the mass value transmission is a key pathway for guiding the Chinese medicinal preparation.
The flos Lonicerae is dried bud or flower with initial bloom of Lonicera japonica Thunb. Is cold in nature and sweet in taste, enters lung, heart and stomach meridians, and has the effects of clearing away heat and toxic materials, dispelling wind and heat and the like. Organic acids, flavonoids and iridoid glycosides are the main active ingredients of honeysuckle and the material basis for exerting the curative effect, wherein the organic acids are easily soluble in water, and have more isomers, such as neochlorogenic acid, chlorogenic acid and cryptochlorogenic acid which are isomers, isochlorogenic acid A, B, C which is an isomer, and in the extraction process of honeysuckle decoction pieces-standard decoction, the conversion between the isomers is easy to occur through hydrolysis and intramolecular ester group migration under the influence of temperature, pH and unstable structures in the compounds.
For the quantity value transfer rule of the substances in honeysuckle, the prior research usually adopts the methods of similarity, peak relative retention time, peak number and the like to carry out qualitative evaluation, or adopts the traditional index component transfer rate to carry out quantitative evaluation. When the quantitative evaluation is carried out by adopting the index component transfer rate, reference needs to be carried out on a reference substance, and for components without reference of the reference substance, the quantity condition of corresponding substance transfer cannot be effectively obtained, so that the evaluation of the substance transfer rule is greatly limited.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is as follows: the problem that the existing method cannot be effectively used for evaluating the quantity value transmission rule of various substances in honeysuckle under the condition of no reference of reference substances in the prior art is solved; thereby providing a method for evaluating the quality value transmission rule in the honeysuckle; the evaluation index can effectively evaluate the quantity value transfer rule of the substances in the sample prepared from the honeysuckle decoction pieces without a reference substance, and meanwhile, the invention also discloses a method for screening the process parameters by adopting the evaluation method.
A method for evaluating a quality value transmission rule in honeysuckle comprises the following steps:
evaluating the quantity value transfer rule of each substance of a sample obtained in the preparation process of the product prepared from the honeysuckle decoction pieces by adopting an evaluation index K value representing the quality value transfer rule in the traditional Chinese medicine;
the acquisition process of the K value is as follows:
obtaining the dry paste amount of a sample prepared from honeysuckle decoction pieces;
acquiring the decoction piece concentration of a decoction piece solution prepared from honeysuckle decoction pieces, the sample concentration of a sample solution prepared from a sample, and the fingerprint or characteristic spectrum of the decoction piece solution and the sample solution, and acquiring the decoction piece characteristic peak area and the sample characteristic peak area of corresponding characteristic peaks according to the acquired fingerprint or characteristic spectrum;
the amount of the dry paste, the characteristic peak area of the decoction pieces, the characteristic peak area of the sample, the concentration of the decoction pieces and the concentration of the sample are calculated by the following calculation formula;
under the condition that the same substance is detected at least two wavelengths by the same method, selecting the peak area of the characteristic peak under the maximum absorption wavelength to calculate the K value.
The chromatographic conditions of the fingerprint spectrum or the characteristic spectrum are as follows:
using octadecylsilane chemically bonded silica as filler, acetonitrile as mobile phase A, and aqueous solution containing 0.2-0.5% phosphoric acid or 0.2-0.5% formic acid as mobile phase B, and performing gradient elution according to the gradient elution procedure specified in the following table; the detection wavelength is 238 nm; the column temperature is 25-35 ℃; the flow rate is 0.35-0.45 ml/min. The theoretical plate number is not less than 7000 calculated according to chlorogenic acid;
the preparation process of the decoction piece solution comprises the following steps: accurately weighing flos Lonicerae decoction pieces, placing into conical flask with plug, accurately adding alcohol solution, weighing, heating under reflux or/and ultrasonic treating, cooling, shaking, weighing, supplementing the weight loss with alcohol solution, shaking, filtering, and collecting the filtrate;
the preparation process of the test solution comprises the following steps: taking a sample, precisely weighing, placing in a conical flask with a plug, precisely adding an alcohol solution, weighing, heating and refluxing or/and ultrasonically treating, cooling, shaking up, weighing again, complementing the weight loss with the alcohol solution, shaking up, filtering, and taking a subsequent filtrate.
When the K value is less than 0.3, the substance represented by the characteristic peak is not easy to transfer or generate negative conversion; when the K value is more than 1, the enrichment or positive conversion of the substance represented by the characteristic peak is shown;
and (4) carrying out key evaluation on the characteristic peaks with the K values less than 0.3 and the K values more than 1.
The sample is intermediate product, standard decoction, Chinese medicinal granule or menstruation formula.
The method for screening the process parameters by adopting the method for evaluating the mass value transfer rule in the honeysuckle comprises the following steps: acquiring a standard decoction of honeysuckle decoction pieces, and acquiring K values of characteristic peaks corresponding to various substances in the standard decoction pieces; obtaining a sample of honeysuckle decoction pieces, obtaining K values of characteristic peaks corresponding to corresponding substances in the sample,
and screening out the K value which is closest to the K value of the characteristic peak corresponding to the same substance as the standard decoction in the sample, wherein the process parameter corresponding to the K value is the optimal process.
The honeysuckle decoction pieces used for preparing the standard decoction and the honeysuckle decoction pieces used for preparing the sample are the same in batch.
The substance comprises at least one of neochlorogenic acid, chlorogenic acid, seco-logenin, cryptochlorogenic acid, swertiamarin, seco-logenin, isochlorogenic acid B, isochlorogenic acid A, and isochlorogenic acid C.
The preparation process of the honeysuckle standard decoction comprises the following steps: soaking flos Lonicerae decoction pieces in casserole for 30 min, adding water 16 times the amount of the decoction pieces, boiling 500w, decocting 200w for 20 min, filtering while hot, and rapidly cooling; adding water with the amount being 12 times of that of the decoction pieces in the second decoction, boiling 500w, decocting 200w for 15 minutes, filtering while hot, and quickly cooling for later use; mixing filtrates, concentrating at below 50 deg.C until the ratio of material to liquid is 1:1, and freeze drying.
The standard decoction contains neochlorogenic acid K value of 2.13-3.72, chlorogenic acid K value of 0.49-0.72, secologenin K value of 0.75-0.89, cryptochlorogenic acid K value of 1.23-1.74, swertiamarin K value of 0.52-0.90, secologenin K value of 0.73-1.08, isochlorogenic acid B K value of 4.65-7.23, isochlorogenic acid A K value of 0.21-0.33, and isochlorogenic acid C K value of 1.11-1.50.
The technical scheme of the invention has the following advantages:
1. the invention provides a method for evaluating a quality value transfer rule in honeysuckle, which comprises the following steps: evaluating the quantity value transmission rule of each substance in the honeysuckle decoction pieces by adopting a K value, wherein the change trend of the K value is consistent with the change trend of the transfer rate of the effective components, and when the K value is more than 1, the positive conversion process of the components to the standard decoction is shown; when the K value is less than 0.3, the components are not easy to transfer or decompose (namely negative conversion) in the standard decoction; the acquisition of the K value does not need to introduce a component reference substance, multi-component analysis can be carried out on the premise of lacking the component reference substance, the influence of multiple factors on result analysis is reduced, and the K value can scientifically analyze the quantity value transfer rule of each substance in the honeysuckle decoction pieces, so that the K value can be used for evaluating the quantity value transfer rule of various known or unknown substances in the honeysuckle traditional Chinese medicine formula granules or intermediate products thereof, or the menstruation formula containing the honeysuckle decoction pieces or the intermediate products thereof, and the safety of clinical application of the honeysuckle formula granules or menstruation formula is better ensured.
2. The invention further optimizes the screening rule of chromatographic conditions, and concretely, under the condition that the same substance is detected by at least two wavelengths in the same method, the peak area of the characteristic peak under the maximum absorption wavelength is selected to calculate the K value; and specific chromatographic conditions are disclosed, and the K values of all substances in the honeysuckle can be more accurately expressed by screening the chromatographic conditions, so that the value transfer rule is more accurate in detection result.
3. The invention also provides a method for controlling the quality of the process parameters by adopting the K value, which specifically comprises the following steps: acquiring a standard decoction of honeysuckle decoction pieces, and acquiring a K value of each characteristic peak in the standard decoction; obtaining a sample prepared from honeysuckle decoction pieces, obtaining the K value of each characteristic peak in the sample, and screening out the process parameter corresponding to the K value which is closest to the K value of the characteristic peak corresponding to the standard decoction in the sample; the method can effectively screen out the process parameter conditions of the sample which is closer to the material basis of the standard decoction, so that the prepared sample is consistent with the material basis of the standard decoction, the consistency of the sample and the standard decoction can be further ensured, and the drug effect and the safety of clinical application are improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the prior art descriptions will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a characteristic map of a standard decoction of the present invention.
FIG. 2 is a characteristic map of example 3 of the present invention.
FIG. 3 is a characteristic map of example 4 of the present invention.
FIG. 4 is a characteristic map of example 5 of the present invention.
Detailed Description
Example 1
A method for evaluating a quality value transfer rule in honeysuckle comprises the following specific processes:
1.1 feature mapping method
Chromatographic conditions and system applicability test: octadecylsilane chemically bonded silica is used as filler, and the chromatographic column is ACQUITY in the embodiment
HST 3, column length 10cm, column inner diameter 2.1mm, particle diameter 1.8 μm. Gradient elution was performed according to the gradient elution procedure specified in table 1 below using acetonitrile as mobile phase a and aqueous solution containing 0.2% formic acid as mobile phase B; the detection wavelength is 238 nm; the column temperature is 30 ℃; the flow rate was 0.4 ml/min. The theoretical plate number is not less than 7000 calculated by chlorogenic acid.
Table 1 mobile phase gradient elution procedure
Preparation of reference solutions: preparation of reference substance solution for reference substance A proper amount of chlorogenic acid, neochlorogenic acid, seco-logenin, cryptochlorogenic acid, swertiamarin, seco-logenin, isochlorogenic acid A, isochlorogenic acid B, isochlorogenic acid C and reference substance are precisely weighed, 70% ethanol is added to prepare solutions containing 0.4mg per 1ml, and the solutions are uniformly shaken to serve as reference substance solutions for the reference substance.
Preparation of reference solution of reference drug: taking a honeysuckle comparison medicinal material, grinding the comparison medicinal material provided by the Chinese traditional medicine, taking about 1.0g, precisely weighing, placing in a conical flask with a plug, precisely adding 50mL of 70% ethanol, weighing, heating and refluxing for 1h, cooling, shaking up, weighing again, complementing the weight loss by 70% ethanol, shaking up, filtering, and taking a subsequent filtrate as a reference solution of the comparison medicinal material.
Preparation of a test solution: taking a proper amount of sample, grinding, precisely weighing about 0.5g, placing into a conical flask with a plug, precisely adding 50mL of 70% ethanol, weighing, heating and refluxing for 1h, cooling, shaking up, weighing again, complementing the lost weight with 70% ethanol, shaking up, filtering, and taking the subsequent filtrate.
Preparing decoction piece solution: is prepared by adopting honeysuckle decoction pieces with the same batch as the test solution and adopting a preparation method of a reference solution of a reference medicinal material.
Wherein, the sample in the test solution is a standard decoction, and the preparation process of the standard decoction of honeysuckle comprises the following steps: soaking honeysuckle decoction pieces in a casserole for 30 minutes, adding water 16 times the amount of the honeysuckle decoction pieces in the first decoction, boiling for 500w, decocting for 20 minutes at 200w, filtering while hot, and rapidly cooling for later use; adding water with the amount being 12 times of that of the decoction pieces in the second decoction, boiling 500w, decocting 200w for 15 minutes, filtering while hot, and quickly cooling for later use; mixing filtrates, concentrating (below 50 deg.C) to obtain a concentrate with a ratio of 1:1, and freeze drying.
The determination method comprises precisely sucking reference solution, decoction piece solution, reference solution of reference medicinal material and sample solution 1 μ l each, injecting into ultra high performance liquid chromatograph, and determining.
At 238nm, the characteristic spectrum of the test solution should show 11 characteristic peaks, as shown in FIG. 1, and should correspond to the retention time of 11 characteristic peaks in the reference chromatogram of the reference drug, the peak corresponding to the peak of the chlorogenic acid reference is the S peak, the relative retention time of the remaining characteristic peaks is calculated, and the relative retention time should be within + -7% of the specified value. The specified values are: 0.49 (peak 1), 1.00 (peak S), 1.10 (peak 3), 1.22 (peak 4), 1.76 (peak 5), 2.11 (peak 6), 2.17 (peak 7), 3.05 (peak 8), 3.17 (peak 9), 3.41 (peak 10), 3.46 (peak 11). Wherein peak 1 is neochlorogenic acid; peak 2 is chlorogenic acid (S); peak 3 is seco-oxologenin; peak 4 is cryptochlorogenic acid; peak 5 is swertiamarin; peak 6 is secologanin oxide; peak 8 is isochlorogenic acid B; peak 9 is isochlorogenic acid a; peak 11 is isochlorogenic acid C.
1.2K value vs. content transfer Rate
Measuring 15 batches of flos Lonicerae decoction pieces and standard decoction pieces by the above characteristic spectrum method to obtain characteristic spectrum data, wherein the measured values include characteristic peak area, decoction piece concentration, sample concentration and paste yield, and K value is calculated according to the following calculation formula, and content transfer rate is calculated according to the existing reference substance, and the detection results are shown in tables 2-4. The calculation methods of the characteristic peak area, the decoction piece concentration, the sample concentration and the paste yield are all conventional detection and calculation methods, and are not described herein again.
TABLE 2
TABLE 3
TABLE 4
Through mass spectrometry, structure inference is carried out on 11 characteristic peaks, and 9 characteristic peaks are determined as follows: neochlorogenic acid (peak 1), chlorogenic acid (peak 2), seco-loganin (peak 3), cryptochlorogenic acid (peak 4), swertiamarin (peak 5), seco-loganin (peak 6), isochlorogenic acid B (peak 8), isochlorogenic acid A (peak 9), isochlorogenic acid C (peak 11).
As shown in tables 2-4, the analysis of the results of mass spectrometry shows that the range of K value of neochlorogenic acid is 2.13-3.72, K value of chlorogenic acid is 0.49-0.72, K value of secologenin is 0.75-0.89, K value of cryptochlorogenic acid is 1.23-1.74, K value of swertiamarin is 0.52-0.90, K value of secologenin is 0.73-1.08, K value of isochlorogenic acid B is 4.65-7.23, K value of isochlorogenic acid A is 0.21-0.33, and K value of isochlorogenic acid C is 1.11-1.50. Wherein the mean value of the transfer rate of the neochlorogenic acid is 3.10, and the mean value of the K value is 3.02; the mean value of the transfer rate of the chlorogenic acid is 0.55, and the mean value of the K value is 0.58; the mean value of the transfer rate of the secologanin acid is 0.78, and the mean value of the K value is 0.81; the mean value of the transfer rate of the cryptochlorogenic acid is 1.60, and the mean value of the K value is 1.47; the average value of the transfer rate of the swertiamarin is 0.73, and the average value of the K value is 0.68; the mean value of the transfer rate of the secologanin oxide is 0.86, and the mean value of the K value is 0.90; the mean value of the transfer rate of isochlorogenic acid B is 6.31, and the mean value of the K value is 6.10; the mean value of the transfer rate of the isochlorogenic acid A is 0.25, and the mean value of the K value is 0.26; the mean value of the transfer rates of isochlorogenic acid C was 1.33, and the mean value of the K values was 1.28. Because the detection conditions of 15 batches of standard decoction and decoction pieces are different, the K value is slightly different from the content transfer rate value, but the K value is consistent with the content transfer rate trend, which shows that the K value can describe the change trend of various component substances on the premise of not using a reference substance.
Through K value analysis, 11 characteristic peaks in the honeysuckle decoction piece-standard decoction process are transmitted, except that K values of each batch of neochlorogenic acid, cryptochlorogenic acid, isochlorogenic acid B and isochlorogenic acid C are all larger than 1, K values of all peaks are smaller than 1, but the K values are occasionally influenced by origin factors to be slightly larger than 1. Literature research shows that organic acid compounds are influenced by three unstable structures of ester bonds, unsaturated double bonds and polyphenol in the extraction process, are isomerized by hydrolysis and intramolecular ester group migration, and chlorogenic acid is isomerized into neochlorogenic acid and cryptochlorogenic acid under neutral and alkaline conditions; the isochlorogenic acid A is isomerized into isochlorogenic acid B and isochlorogenic acid C, so that the K values of the new chlorogenic acid and the cryptochlorogenic acid are more than 1, and the K value of the chlorogenic acid is less than 1, which is probably related to the isomerization of the chlorogenic acid into the new chlorogenic acid and the cryptochlorogenic acid; the K values of the isochlorogenic acid B and the isochlorogenic acid C are more than 1, and the K value of the isochlorogenic acid A is less than 1, which is probably related to the isomerization of the isochlorogenic acid A to generate the isochlorogenic acid B and the isochlorogenic acid C.
Therefore, the transmission rule of the components in the honeysuckle standard decoction conforms to the characteristics of the organic acid components, which shows that the K value can assist in analyzing the substance transmission condition of the decoction piece-standard decoction, and the production and control of the traditional Chinese medicine formula granules can be better guided by utilizing the transmission rule.
Example 2
The method for screening process conditions by using the method for evaluating the mass value transfer rule in the honeysuckle in the embodiment 1 comprises the following specific steps:
because the standard decoction is the material basis of the formula particle, the consistency of the formula particle and the standard decoction can be ensured by taking the material component change rule of the standard decoction as the key process attribute of the formula particle.
As can be seen from tables 2 to 4 in example 1: the K value range of the honeysuckle standard decoction peak 1 is 2.13-3.72, the K value range of the peak 2 is 0.49-0.72, the K value range of the peak 3 is 0.75-0.89, the K value range of the peak 4 is 1.23-1.74, the K value range of the peak 5 is 0.52-0.90, the K value range of the peak 6 is 0.73-1.08, the K value range of the peak 7 is 0.48-1.08, the K value range of the peak 8 is 4.65-7.23, the K value range of the peak 9 is 0.21-0.33, the K value range of the peak 10 is 0.77-0.99, the K value range of the peak 11 is 1.11-1.50, and the K value range of each peak is larger. The analysis is mainly caused by the large quality difference of the current raw materials, and if the range value is taken as a reference, process deviation occurs. In view of the inevitable problem of quality difference of raw materials, K value of the standard decoction prepared from the honeysuckle decoction pieces in the same batch meeting the range of the standard decoction is selected as a reference, and the process parameters are screened to ensure the consistency of the obtained final product and the standard decoction.
Wherein, when the K value is less than 0.3, the substance represented by the characteristic peak is not easy to transfer or generate negative conversion; when the K value is more than 1, the enrichment or positive conversion of the substances represented by the characteristic peak is shown; in the peaks 1 to 11, the K value of the peak 9 is less than 0.3, which indicates that the component is not easy to transfer or decompose (namely, negative conversion) and needs to be monitored in a key way; the K values of peaks 1, 4, 8, 11 are much greater than 1, also requiring significant monitoring. Wherein the K values of the peak 1 (neochlorogenic acid) and the peak 4 (cryptochlorogenic acid) are more than 1 and are mainly converted from the peak 2 (chlorogenic acid); the K values of the peak 8 (isochlorogenic acid B) and the peak 11 (isochlorogenic acid C) are more than 1, and the peak 9 (isochlorogenic acid A) is mainly converted, so that the indexes of process monitoring are simplified only by monitoring the peaks 2 and 9. Therefore, the process-off keying of the honeysuckle is determined to be the components represented by peak 2 and peak 9.
The K value results of each intermediate product in the process of the three batches of honeysuckle formula granules and the final peak 2 and peak 9 of the honeysuckle formula granules are shown in the following table 5:
TABLE 5K value analysis of Lonicera japonica granulation Process
From the results shown in table 5, it can be seen that, in the process conditions obtained by screening the particle preparation process through the process key control point determined by the K value, the K values of peak 2 and peak 9 are both close to the K values of the standard decoction of the corresponding batch and are both within the standard decoction range. The prepared granules have better basic consistency with the drug effect substances of the standard decoction, so that the granules prepared by the three batches of process conditions are further determined to meet the requirements. In conclusion: the key property of the process determined by the K value can ensure the drug effect and safety of the clinical application of the formula granules.
Example 3
The difference between this example and example 1 is that the chromatographic conditions are different, specifically as follows:
the column temperature of the chromatographic column is 35 ℃; acetonitrile is taken as a mobile phase A, and an aqueous solution containing 0.2% formic acid is taken as a mobile phase B; the detection wavelength is 238 nm; the flow rate was 0.45ml/min, and the results are shown in FIG. 2.
Other detection conditions were exactly the same as in example 1, and the detection results are shown in FIG. 2.
Example 4
The difference between this example and example 1 is that the chromatographic conditions are different, specifically as follows:
the column temperature of the chromatographic column is 25 ℃; acetonitrile is taken as a mobile phase A, and an aqueous solution containing 0.5 percent of formic acid is taken as a mobile phase B; the detection wavelength is 238 nm; the flow rate was 0.35 ml/min.
Other detection conditions were exactly the same as in example 1, and the detection results are shown in FIG. 3.
Example 5
The difference between this example and example 1 is that the chromatographic conditions are different, specifically as follows:
acetonitrile is used as a mobile phase A, and an aqueous solution containing 0.2% of phosphoric acid is used as a mobile phase B.
Other detection conditions were exactly the same as in example 1, and the detection results are shown in FIG. 4.
The detection conditions of the above embodiments 3 to 5 are adopted to detect and obtain the characteristic spectrum, the K value is calculated by adopting the calculation method of the invention according to the characteristic spectrum, and the following results can be obtained according to the comparison: the K values obtained in examples 3 to 5 differ from the K value obtained in example 1 by not more than 5%, and therefore the detection conditions of examples 3 to 5 described above also satisfy the detection requirements.
It should be understood that the above-described embodiments are merely examples for clarity of description and are not intended to limit the scope of the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. This list is neither intended to be exhaustive nor exhaustive. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A method for evaluating the quality value transmission rule in honeysuckle is characterized by comprising the following steps:
evaluating the quantity value transfer rule of each substance of a sample prepared from the honeysuckle decoction pieces by adopting an evaluation index K value representing the quality value transfer rule in the traditional Chinese medicine;
the acquisition process of the K value is as follows:
obtaining the dry paste amount of a sample prepared from honeysuckle decoction pieces;
acquiring the decoction piece concentration of a decoction piece solution prepared from honeysuckle decoction pieces, the sample concentration of a sample solution prepared from a sample, and the fingerprint or characteristic spectrum of the decoction piece solution and the sample solution, and acquiring the decoction piece characteristic peak area and the sample characteristic peak area of corresponding characteristic peaks according to the acquired fingerprint or characteristic spectrum;
the amount of the dry paste, the characteristic peak area of the decoction pieces, the characteristic peak area of the sample, the concentration of the decoction pieces and the concentration of the sample are calculated by the following calculation formula;
2. the method for evaluating the transmission law of the mass value of a substance in honeysuckle according to claim 1, wherein the peak area of the characteristic peak at the maximum absorption wavelength is selected for calculating the K value when the same substance is detected at least two wavelengths in the same method.
3. The method for evaluating the quality value transmission rule of honeysuckle according to claim 1 or 2, wherein the chromatographic conditions of the fingerprint or the characteristic spectrum are as follows:
using octadecylsilane chemically bonded silica as filler, acetonitrile as mobile phase A, and aqueous solution containing 0.2-0.5% phosphoric acid or 0.2-0.5% formic acid as mobile phase B, and performing gradient elution according to the gradient elution procedure specified in the following table; the detection wavelength is 238 nm; the column temperature is 25-35 ℃; the flow rate is 0.35-0.45 ml/min; the theoretical plate number is not less than 7000 calculated according to chlorogenic acid;
4. the method for evaluating the quality value transmission law of honeysuckle according to claim 3, wherein the decoction piece solution is prepared by the following steps: accurately weighing flos Lonicerae decoction pieces, adding alcohol solution, weighing, heating under reflux or/and ultrasonic treatment, cooling, shaking, weighing, supplementing the lost weight with alcohol solution, shaking, filtering, and collecting the filtrate;
the preparation process of the test solution comprises the following steps: taking a sample, precisely weighing, adding an alcohol solution, weighing, heating and refluxing or/and carrying out ultrasonic treatment, cooling, shaking up, weighing again, complementing the weight loss by the alcohol solution, shaking up, filtering, and taking a subsequent filtrate to obtain the product.
5. The method for evaluating the transmission law of substance quantity values in honeysuckle according to any one of claims 1 to 4, wherein when the K value is less than 0.3, the substance represented by the characteristic peak is not easy to transfer or generate negative conversion; when the K value is more than 1, the enrichment or positive conversion of the substance represented by the characteristic peak is shown;
and (4) carrying out key evaluation on the characteristic peaks with the K values less than 0.3 and the K values more than 1.
6. The method for evaluating the quality value transmission law of honeysuckle according to any one of claims 1 to 5, wherein the sample is an intermediate product, a standard decoction, a Chinese medicinal formula granule or a menstruation formula.
7. The method for screening the process parameters by adopting the method for evaluating the quality value transmission rule in the honeysuckle as claimed in any one of claims 1 to 6, is characterized by comprising the following steps: acquiring a standard decoction of honeysuckle decoction pieces, and acquiring K values of characteristic peaks corresponding to various substances in the standard decoction pieces; obtaining a sample of honeysuckle decoction pieces, obtaining K values of characteristic peaks corresponding to corresponding substances in the sample,
and screening out the K value which is closest to the K value of the characteristic peak corresponding to the same substance as the standard decoction in the sample, wherein the process parameter corresponding to the K value is the optimal process.
8. The method of claim 7, wherein the honeysuckle decoction pieces used to prepare the standard decoction pieces and the honeysuckle decoction pieces used to prepare the sample are the same lot of honeysuckle decoction pieces.
9. The method of claim 7 or 8, wherein the substance comprises at least one of neochlorogenic acid, chlorogenic acid, secologenin, cryptochlorogenic acid, swertiamarin, secologenin, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C.
10. The method according to any one of claims 7 to 9, wherein the honeysuckle standard decoction is prepared by a process comprising: soaking honeysuckle decoction pieces in a casserole for 30 minutes, adding water 16 times the amount of the honeysuckle decoction pieces in the first decoction, boiling for 500w, decocting for 20 minutes at 200w, filtering while hot, and rapidly cooling for later use; adding water with the amount being 12 times of that of the decoction pieces in the second decoction, boiling 500w, decocting 200w for 15 minutes, filtering while hot, and quickly cooling for later use; mixing filtrates, concentrating at below 50 deg.C until the ratio of material to liquid is 1:1, and freeze drying.
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