CN112113929A - Quality control method for extraction process of children's oral liquid for removing food retention and relieving cough - Google Patents
Quality control method for extraction process of children's oral liquid for removing food retention and relieving cough Download PDFInfo
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Abstract
The invention belongs to the field of traditional Chinese medicine preparation analysis, relates to a quality control method for an extraction process of an oral liquid for removing food retention and relieving cough of children, and particularly relates to a method for performing quality control on an oral extraction process for removing food retention and relieving cough of children by using a near infrared spectrum analysis technology. The quality control method for the extraction process is the combination of the spectral measurement technology and the chemometrics, has the advantages of rapidness, no damage and green, can realize simultaneous determination of multiple components, is suitable for the decoction process of the oral liquid for removing food retention and relieving cough of children, realizes online real-time quality monitoring in the production process, and has an important promotion effect on improving the digitization, intellectualization and greening levels of the production process of the oral liquid for removing food retention and relieving cough of children.
Description
Technical Field
The invention relates to a quality control method for an extraction process of an oral liquid for removing food retention and relieving cough of children, in particular to a method for performing quality control on an oral extraction process for removing food retention and relieving cough of children by using a near infrared spectrum analysis technology, and belongs to the field of analysis of traditional Chinese medicine preparations.
Background
The oral liquid (approved character: national standard Z10970022) for removing food retention and relieving cough for children is an exclusive product of traditional Chinese medicines of Lunan Kangpu pharmaceutical Co Ltd, is prepared from 10 traditional Chinese medicine raw materials of fried hawthorn, areca nut, immature bitter orange, loquat leaf, snakegourd fruit, fried radish seed, fried lepidium seed, platycodon root, weeping forsythia and cicada slough, has the effects of clearing heat and purifying lung, removing food retention and relieving cough, has independent intellectual property rights of prescription, process, quality standard and use core technology, is collected from the first tonic book of the Chinese pharmacopoeia 2010 edition and the national basic medicine catalog (2012 edition), and has the trade name of
The oral liquid for removing food retention and relieving cough for children is clinically special for cough, exacerbation at night, wheezy phlegm in throat, abdominal distension, halitosis and the like caused by food retention and phlegm-heat in lung of children, has definite curative effects on mycoplasma pneumonia of children, cough variant asthma of children, cough recovery of children after upper respiratory tract infection and the like, is the only approved targeted medicine for treating the cough due to food retention of children at present, and years of clinical application shows that the curative effect of the oral liquid is remarkable and well-valued by doctors and patients.
At present, the problems of long medicine placing time, high energy consumption, low production efficiency, poor batch quality consistency and the like exist in the conventional traditional Chinese medicine oral preparation extraction production process, the digital intelligent manufacturing technology and the advanced traditional Chinese medicine pharmacy technology are fused and popularized and applied to the traditional Chinese medicine extraction production process, and the problems can be effectively solved. However, most of the traditional Chinese medicines are lack of stable and reliable process control means and methods at present, the quality control in the production process mainly depends on experience and a traditional quality analysis method, and effective index component content real-time monitoring means are lacked, so that the quality assurance in the medicine extraction process is very passive. Moreover, the extraction time in actual production is often unfixed, the extraction end point is advanced or lagged basically without considering the quality difference of the raw materials and the medicinal materials and the fluctuation of working conditions, the quality of the extracting solution of different batches is easy to be unstable, the quality difference among the batches of the traditional Chinese medicine preparation is caused, and the waste of energy, time and labor, the reduction of the utilization rate of the medicinal materials and the like are caused. Therefore, the method is simple and convenient to operate, low in cost, simple in pretreatment and even a spectrum analysis technology without pretreatment becomes a preferred method for controlling the quality of the extraction process.
Near Infrared Spectroscopy (NIRs) is a combination of spectroscopic measurement techniques and chemometrics, and because of its rapidity, non-destructive, green, it can achieve simultaneous measurement of multiple components, and is particularly suitable for non-destructive measurement, on-line analysis, and the like. The accuracy of the near-infrared online monitoring mainly depends on the accuracy of the measuring method adopted before modeling, and is also related to instrument system errors, measuring environment, modeling sample quantity, sample representativeness and timeliness. In the face of numerous influencing factors in the process of near-infrared quantitative analysis, how to control the change of the factors, reduce the error of the quantitative analysis, ensure the reliability of the near-infrared quantitative analysis and reduce the risk of the near-infrared quantitative analysis in daily application is an urgent problem to be solved when the near-infrared analysis is used for controlling the actual extraction process of the pediatric food retention removing and cough relieving oral liquid.
Disclosure of Invention
Aiming at the problem that an effective index component content real-time monitoring means is lacked in the digital and intelligent extraction process of the infantile food retention removing and cough relieving oral liquid, the invention aims to provide a quality control method for the infantile food retention removing and cough relieving oral extraction process by using a near infrared spectrum analysis technology. Taking index components of synephrine, naringin, neohesperidin and phillyrin in the oral liquid for removing food retention and relieving cough of children as quantitative research objects, simulating the extraction process of the oral liquid for removing food retention and relieving cough of children, establishing a High Performance Liquid Chromatography (HPLC) which is simple, convenient, sensitive and high in accuracy, taking the measured content of the HPLC as a chemical truth value, establishing a fast and quantitative near infrared spectrum analysis model, applying a near infrared technology to the decoction process of the oral liquid for removing food retention and relieving cough of children, and realizing online real-time quality monitoring in the production process of the oral liquid.
A quality control method for the extraction process of an oral liquid for removing food retention and relieving cough for children adopts a near infrared spectrum technology, collects the near infrared spectrogram data of a decoction liquid in an integrating sphere diffuse reflection mode, and establishes a quantitative analysis model of index components of the decoction liquid, namely synephrine, naringin, neohesperidin and phillyrin in the decoction process by combining a partial least square method and a chemical truth value, so as to realize the online real-time quality monitoring of the production process of the oral liquid for removing food retention and relieving cough for children.
A quality control method for an extraction process of an oral liquid for removing food retention and relieving cough for children specifically comprises the following steps:
A. respectively weighing 10 raw medicinal materials of fried hawthorn, areca nut, immature bitter orange, loquat leaf, snakegourd fruit, fried radish seed, fried lepidium seed, platycodon root, weeping forsythia and cicada slough in an amount which is 10 times of the prescription amount of the oral liquid for removing food retention and relieving cough for sample collection, processing the medicinal materials by simulating an actual production process, sequentially putting the medicinal materials into a multifunctional extraction tank, adding water for decocting for 2 times, and regulating steam to keep a slightly boiling state after liquid medicine is boiled; sampling from boiling, sampling once every 10 minutes, filtering by 300-mesh electric spinning, and sampling for 29 times in total; repeating for 4 batches to obtain 116 parts of decoction samples;
B. collecting near infrared spectrum data, namely collecting a decoction sample in the step A, and collecting the near infrared spectrum by adopting a Bruker MPA II multifunctional Fourier transform near infrared spectrometer integrating sphere diffuse reflection, wherein the optimal main component numbers of synephrine, naringin, neohesperidin and phillyrin are respectively 4, 3 and 3; scanning times 64, resolution 16cm-1；
C. Determining chemical truth values of index component contents of the decoction in the extraction process, and determining the chemical truth values of the index components of synephrine, naringin, neohesperidin and phillyrin in the decoction in the step A by HPLC;
D. establishing a near infrared spectrum quantitative analysis model C chemical truth values of contents of synephrine, naringin, neohesperidin and phillyrin, bringing the chemical truth values into OPUS quantitative processing software to correspond to a spectrogram obtained by NIR scanning, and adopting a Kennard-Stone method to take 26% of multiple samples as a verification set and the rest 74% as a correction set; a quantitative correction model of near infrared spectrum and synephrine, naringin, neohesperidin and phillyrin is established by adopting a Partial Least Squares (PLS), and the established model is adopted to predict the content of 4 components in a sample.
Specifically, the step C of measuring the chemical truth values of the index components synephrine, naringin, neohesperidin and phillyrin in the decoction obtained in the step A by using HPLC comprises the following steps:
chromatographic conditions are as follows: the chromatographic column is Phenomenex
PFP; taking 0.1% perchloric acid as a mobile phase A, and calculating the ratio by volume as acetonitrile: carrying out linear gradient elution by taking methanol as a mobile phase B at a ratio of 9: 1;
preparation of control solutions: precisely weighing synephrine reference substance 16.70mg, naringin reference substance 24.03mg, neohesperidin reference substance 15.53mg and phillyrin reference substance 21.78mg, placing in the same 25ml measuring flask, adding 50% methanol, and ultrasonic dissolving to obtain mixed reference substance stock solution; precisely transferring 1ml of the mixed reference substance stock solution into a 25ml measuring flask, adding water to dilute to scale, shaking up, and filtering to obtain a reference substance solution;
preparation of a test solution: placing 5ml of each of the first and second decoction in step A in a 10ml measuring flask, diluting with ultrapure water to scale, centrifuging at 12000r/min for 10min, collecting supernatant, and filtering with 0.22 μm microporous membrane;
the determination method comprises the following steps: respectively and precisely absorbing 10 mul of each of the reference solution and the sample solution, injecting into a high performance liquid chromatograph, recording the chromatogram, and calculating the content by an external standard method to obtain the chemical truth value of the content of index components of the decoction, namely synephrine, naringin, neohesperidin and phillyrin.
Preferably, the HPLC chromatographic conditions in step C are:
the chromatographic column is Phenomenex
PFP (2), 4.6 x 250mm, 5 μm; taking 0.1% perchloric acid as a mobile phase A, and calculating the ratio by volume as acetonitrile: methanol 9: 1, performing linear gradient elution for the mobile phase B, wherein the elution procedure is as follows:
| time (min) | Mobile phase A (%) | Mobile phase B (%) |
| 0-5 | 100％ | 0％ |
| 5-10 | 100％→98％ | 0％→2％ |
| 10-15 | 98％→95％ | 2％→5％ |
| 15-35 | 95％→80％ | 5％→20％ |
| 35-55 | 80％→75％ | 20％→25％ |
| 55-80 | 75％→60％ | 25％→40％ |
| 80-81 | 60％→100％ | 40％→0％ |
| 81-90 | 100％ | 0％ |
The column temperature is 35 ℃; the sample amount is 10 mul; the flow rate is 0.8 ml/min; the detection wavelength was 225 nm.
Preferably, the selecting of a suitable modeling band in step D is: the optimal spectral ranges of naringin, neohesperidin and phillyrin are all 9400-7496cm-1The wave band, the spectral range of synephrine is 9400-7496cm-1、6104-5448cm-1And (4) dual wave bands.
Preferably, the spectrum preprocessing method in step D is: the pretreatment methods of synephrine and forsythin are both to eliminate constant deviation values, and both naringin and neohesperidin adopt non-spectral pretreatment.
Compared with the prior art, the invention has the following beneficial effects:
1) on the basis of the existing quality detection method of the pediatric food retention removing and cough relieving oral liquid, the invention adds HPLC content measurement of naringin, neohesperidin and phillyrin, perfects the quality detection system of the pediatric food retention removing and cough relieving oral liquid and realizes the purpose of multi-component combined detection and control of the preparation.
2) The invention adopts an HPLC method to simultaneously determine the content of 4 components of synephrine, naringin, neohesperidin and phillyrin in the oral liquid for removing food retention and relieving cough of children, and the established method has high accuracy, good stability and simple operation, can relieve the problem of high detection cost, saves consumables, improves detection efficiency and saves labor cost.
3) According to the composition characteristics of the oral liquid for removing food retention and relieving cough for children, the acquisition mode is determined as integrating sphere diffuse reflection, the optimal modeling wave band and spectrum pretreatment method are selected, the optimal number of main components is optimized, the NIRS rapid nondestructive detection method for 4 components in the decoction process of the oral liquid for removing food retention and relieving cough for children is established, the method is simple and convenient to operate, dynamic changes in the decoction process can be monitored in real time, judgment of abnormal conditions is facilitated, and uniformity and stability of preparation quality can be guaranteed.
4) The application of the quality control method in the extraction process can realize the online real-time quality monitoring in the production process of the oral liquid for removing food retention and relieving cough for children, promote the digitization, the intellectualization and the greening of the extraction production process of the oral liquid for removing food retention and relieving cough for children, and promote the improvement of the manufacturing level of equipment in the pharmaceutical industry.
Drawings
FIG. 1 is HPLC chart of special test for HPLC determination of XIAO ER XIAO JI ZHI KE ORAL LIQUID
The scores in the figures are as follows: a is synephrine; b, naringin; c, neohesperidin; d, phillyrin; 1-a blank solvent; 2-negative control solution a; 3-test solution a; 4-negative control solution b; 5-test solution b; 6-control solution;
FIG. 2 is a near infrared spectrum of the decoction of XIAO' ERXIAO JIE ZHIKE ORAL LIQUID
FIG. 3 is a comparison of predicted values and measured values in a validation set of 4 components
Detailed Description
In order to more fully understand the technical solution of the present invention, the following further describes the present invention through a typical embodiment. The invention discloses an oral liquid for eliminating indigestion and relieving cough of children, which is prepared from Lunan Kappan pharmaceutical Co.
Example 1 HPLC chromatographic condition optimization of synephrine, naringin, neohesperidin and phillyrin
1 Instrument and reagent
1.1 instruments
Waters Acquity Arc 2695 high performance liquid chromatograph (Watts corporation, USA) equipped with 2998PDA detector, Epower3 chromatographic workstation; H1650-W bench-top minidisk high speed centrifuges (Changshan appearance centrifuge, Inc.); KS-5200DE liquid crystal ultrasonic cleaner (Kunshan Jielimei ultrasonic Instrument Co., Ltd.); a numerical control ultrasonic cleaner (Kunshan ultrasonic instruments Co., Ltd.); an organic filter head (0.22 μm pore size, eismer technologies ltd); pure water/ultrapure water systems.
1.2 materials
Acetonitrile and methanol are chromatographically pure, and are both from Tiandi corporation of America (TEDIA); perchloric acid is analytically pure, Nanjing chemical reagents GmbH; the water is ultrapure water. Synephrine (batch No. 110727-201809), phillyrin (batch No. 110821-201816), naringin (batch No. 110722-201815), neohesperidin (batch No. 111857-201804), and the reference substances were purchased from the China institute for food and drug assay.
1.3 pharmaceutical materials for experiments
The sources of the experimental medicines are shown in table 1, and the experimental medicines meet the requirements under related items of 'Chinese pharmacopoeia' 2015 edition.
TABLE 1 infantile food retention removing and cough relieving oral liquid
2 content determination of synephrine, naringin, neohesperidin and phillyrin
2.1 chromatographic conditions: the chromatographic column is Phenomenex
PFP (2) (4.6 x 250mm, 5 μm); mobile phase A is 0.1% perchloric acid, mobile phase B is acetonitrile-methanol (9: 1), gradient elution (0-5min, 100% A, 5-10min, 100-98% A, 10-15min, 98-95% A, 15-35min, 95-80% A, 35-55min, 80-75% A, 55-80min, 75-60% A, 80-81min, 60-100% A, 81-90min, 100% A); the column temperature was 35 ℃; the sample amount is 10 mul; the flow rate is 0.8 ml/min; the detection wavelength was 225 nm.
2.2 preparation of the solution
2.2.1 preparation of control solutions: accurately weighing synephrine reference substance 16.70mg, naringin reference substance 24.03mg, neohesperidin reference substance 15.53mg and phillyrin reference substance 21.78mg, placing in the same 25ml measuring flask, adding 50% methanol, and ultrasonic dissolving to obtain mixed reference substance stock solution. Precisely transferring 1ml of the mixed reference stock solution into a 25ml measuring flask, adding water to dilute to scale, shaking up, and filtering to obtain a reference solution.
2.2.2 preparation of test solutions: test solution a: taking 5ml of each first decoction sample under the item of sample collection in example 2 and 1, placing the samples in 10ml measuring bottles, adding ultrapure water to dilute to scale, centrifuging at a high speed of 12000r/min for 10min, taking supernate, and filtering with a 0.22 mu m microporous membrane to obtain the product. Sample solution b: taking a second decoction sample under the item of sample collection in example 2 and 1, centrifuging at a high speed of 12000r/min for 10min, taking supernate, and filtering with a 0.22 μm microporous membrane to obtain the final product.
2.2.3 preparation of negative control solution: preparing decoction without fructus Aurantii Immaturus and fructus forsythiae according to the preparation method of the oral liquid for removing food retention and relieving cough for children, and preparing a negative control solution a and a negative control solution b according to the preparation methods of the test solution a and the test solution b.
3 methodology examination
3.1 System suitability and specificity test
Precisely sucking 10 μ l of each of the reference solution, the blank solvent, the sample solution a, the negative reference solution a, the sample solution b and the negative reference solution b, injecting sample under the chromatographic condition of '2.1', and recording chromatogram, as shown in figure 1. And the retention time of chromatographic peaks of synephrine, naringin, neohesperidin and phillyrin in the chromatogram of the test sample is consistent with that of chromatographic peaks of the reference sample, the separation degree of the chromatographic peaks of the effective components and other adjacent components is more than 1.5, and the blank solvent and the negative control solution are not interfered at the corresponding retention time of the chromatographic peaks to be tested.
3.2 precision test
Precisely sucking 10 μ l of control solution under item "2.2.1", continuously injecting sample for 6 times, and measuring chromatographic peak retention time RSD of synephrine, naringin, neohesperidin, and phillyrin to be 0.05%, 0.04%, and 0.03%, respectively; RSD of peak areas of chromatographic peaks are respectively 0.09%, 0.18%, 0.22% and 0.07%, and the result shows that the precision degree of the instrument is good.
3.3 Linearity and Range
Precisely transferring the mixed control stock solutions of '2.2.1' of 0.04ml, 0.08ml, 0.2ml, 0.4ml, 0.8ml, 2ml, 4ml and 8ml into 10ml measuring bottles, adding water to dilute to scale, shaking up, and mixing with the mixed control stock solutions to obtain mixed control solution with serial concentrations. 10. mu.l of the above solution was precisely extracted, injected into a liquid chromatograph, and measured by the method, and linear regression was performed on X with Y as X and Y as Y, using the peak area as Y ordinate and each control concentration as X abscissa, and the regression equation, linear range and correlation coefficient of each index component are shown in Table 2.
TABLE 2 regression equation, linear range and correlation coefficient for each index component
3.4 repeatability test
Taking the same first decoction sample, preparing 6 parts of test solution in parallel according to the method of 'test solution a under 2.2.2' and determining according to the method. The results showed RSDs of synephrine, naringin, neohesperidin and forsythin contents of 0.12%, 0.90%, 0.54% and 0.30%, respectively (n ═ 6). The test has better repeatability.
3.5 stability test
And precisely absorbing 10 mu l of the prepared test solution of 0 hour, 3 hours, 6 hours, 9 hours and 12 hours after the same test solution a is taken, injecting the test solution into a chromatograph, measuring the peak areas of the effective components, and calculating the RSD of the peak areas of synephrine, naringin, neohesperidin and forsythin to be 0.33%, 0.11%, 0.07% and 0.62% respectively. The test solution a is stable within 12 h.
3.6 accuracy test
Precisely measuring 6 parts of the No. 1 decoction sample with known content, respectively adding a corresponding amount of reference substance, preparing sample solution according to the sample solution a under item 2.2.2, and performing recovery rate test. The measured average recovery rates of synephrine, naringin, neohesperidin and phillyrin are respectively 101.5%, 98.6%, 101.3% and 91.0%, and the RSD is respectively 0.52%, 1.60%, 1.25% and 0.71%, which indicates that the method has good accuracy.
4 assay method
Respectively and precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into a high performance liquid chromatograph, recording the chromatogram, and calculating the content by an external standard method, wherein the content results are shown in Table 3.
Table 3: content determination results of synephrine, naringin, neohesperidin and phillyrin
Example 2 establishment of near infrared spectrum quantitative analysis model
1 sample Collection
Weighing the required medicinal materials respectively according to the amount of 10 times of the prescription of the infantile food retention removing and cough relieving oral liquid, processing the medicinal materials by simulating an actual production process, sequentially putting the medicinal materials into a multifunctional extraction tank, adding water for decocting for 2 times, and regulating small steam to keep a slightly boiling state after the liquid medicine is boiled. The sample was taken from boiling, every 10 minutes, filtered through a 300 mesh electric spinning, and taken 29 times in total. The batch was repeated for 4 times to obtain 116 decoction samples.
2 acquisition of near infrared spectra
Taking 40ml of each sample solution under the item of '1 sample collection' in a beaker with the diameter of 51mm, placing the beaker in a small sample rotator, and adopting a Bruker MPA II multifunctional Fourier transform near infrared spectrometer integrating sphere to diffuse and reflect and collect the near infrared spectrum, wherein the spectrum range is 4000--1The obtained near infrared original spectrogram is shown in FIG. 2.
The content of the index components measured by HPLC is taken as a chemical true value, the OPUS quantitative processing software is substituted to correspond to a spectrogram obtained by NIR scanning, and Kennard-Stone method is adopted to take 26% of 116 samples as a verification set, and the rest 74% are a correction set. Preferably, the modeling band and spectral preprocessing methods employ an internal cross-check with a principal component count, a cross-validation Root Mean Square Error (RMSECV), and an internal cross-validation decision coefficient (R)2) To optimize the index, the performance of the model is examined. Establishing a quantitative correction model of near infrared spectrum and synephrine, naringin, neohesperidin and phillyrin by Partial Least Squares (PLS), externally testing the verification set, comparing the results of the true value and the predicted value, and further testing the prediction effect of the model。
3 processing of spectral data
3.1 spectral Pre-processing method and selection of spectral bands
Because the spectrum information obtained by the near infrared spectrum contains excessive redundant information, in order to improve the prediction precision of an analysis model and eliminate the interference of various factors such as noise, stray light, instrument and sample states, the spectrum data is preprocessed by RMSECV and R2As an index, the smaller the RMSECV value, the R2The larger the value, the more stable the model and the better the prediction performance. In addition, because the decoction of the oral liquid for removing food retention and relieving cough of children is extracted by drinking water, hydroxyl in water can form strong water peaks in the near infrared spectral region of 4000-. The research contrasts and researches 8 spectrum preprocessing methods such as no spectrum preprocessing, constant deviation elimination, vector normalization (SNV), minimum-maximum normalization, multiple stray light correction, first derivative + SMC, one line subtraction and the like and the influence of different modeling wave bands on synephrine, naringin, neohesperidin and phillyrin content models in the decoction through OPUS 8.1 quantitative analysis software, and the result is shown in Table 4. The results show that the optimal spectral ranges of naringin, neohesperidin and forsythin are 9400-7496 bands, and the spectral ranges of synephrine are 9400-7496 bands and 6104-5448 bands; the pretreatment methods of synephrine and forsythin are all to eliminate constant deviant; both naringin and neohesperidin are pretreated without spectrum.
TABLE 4 influence of different pretreatment methods and bands on the model
3.2 selection of principal Components
The prediction capability of the established PLS regression model is greatly different by adopting different principal component numbers; if the number of the principal components is too small, modeling information is insufficient, the prediction capability of modeling is low, and if the number of the principal components is too large, an overfitting phenomenon occurs in the model. Taking the RMSECV value as an evaluation index, and selecting the corresponding main component number according to the change relation between the RMSECV value and the main component number when the RMSECV value is minimum, wherein the optimal main component numbers of synephrine, naringin, neohesperidin and phillyrin are respectively 4, 3 and 3.
3.3 results of external examination
The established model is used for carrying out external verification on the prediction results of the contents of the 4 components in the verification set sample, and the results are shown in figure 3. The prediction values of the NIRS of the 4 components are very close to the measured values, and the variation trends are consistent, so that the results of predicting the content of synephrine, naringin, neohesperidin and phillyrin in the decoction of the children's food retention removing and cough relieving oral liquid by adopting NIRS modeling are reliable, and the requirement of rapid detection can be met.
The above examples are only preferred embodiments of the present invention, and the description thereof is more specific and detailed, but not to be construed as limiting the scope of the present invention. It should be noted that various modifications and improvements can be made by those skilled in the art without departing from the principle and spirit of the invention, and these modifications and improvements should also fall into the scope of the invention.
Claims (6)
1. A quality control method for an extraction process of an oral liquid for removing food retention and relieving cough for children is characterized in that a near infrared spectrum technology is adopted, near infrared spectrogram data of a decoction liquid is collected in an integrating sphere diffuse reflection mode, a quantitative analysis model of index components of the decoction liquid, namely synephrine, naringin, neohesperidin and forsythin, in the decoction process is established by combining a partial least square method and a chemical truth value, and online real-time quality monitoring of the production process of the oral liquid for removing food retention and relieving cough for children is realized.
2. The quality control method in the extraction process of the oral liquid for eliminating indigestion and relieving cough for children as claimed in claim 1, comprising the following steps:
A. respectively weighing 10 raw medicinal materials of fried hawthorn, areca nut, immature bitter orange, loquat leaf, snakegourd fruit, fried radish seed, fried lepidium seed, platycodon root, weeping forsythia and cicada slough in an amount which is 10 times of the prescription amount of the oral liquid for removing food retention and relieving cough for sample collection, processing the medicinal materials by simulating an actual production process, sequentially putting the medicinal materials into a multifunctional extraction tank, adding water for decocting for 2 times, and regulating steam to keep a slightly boiling state after liquid medicine is boiled; sampling from boiling, sampling once every 10 minutes, filtering by 300-mesh electric spinning, and sampling for 29 times in total; repeating for 4 batches to obtain 116 parts of decoction samples;
B. collecting near infrared spectrum data, namely collecting a decoction sample in the step A, and collecting the near infrared spectrum by adopting a Bruker MPA II multifunctional Fourier transform near infrared spectrometer integrating sphere diffuse reflection, wherein the optimal main component numbers of synephrine, naringin, neohesperidin and phillyrin are respectively 4, 3 and 3; scanning times 64, resolution 16cm-1；
C. Determining chemical truth values of index component contents of the decoction in the extraction process, and determining the chemical truth values of the index components of synephrine, naringin, neohesperidin and phillyrin in the decoction in the step A by HPLC;
D. establishing a near infrared spectrum quantitative analysis model C chemical truth values of contents of synephrine, naringin, neohesperidin and phillyrin, bringing the chemical truth values into OPUS quantitative processing software to correspond to a spectrogram obtained by NIR scanning, and adopting a Kennard-Stone method to take 26% of multiple samples as a verification set and the rest 74% as a correction set; a quantitative correction model of near infrared spectrum and synephrine, naringin, neohesperidin and phillyrin is established by adopting a Partial Least Squares (PLS), and the established model is adopted to predict the content of 4 components in a sample.
3. The method for quality control in the extraction process of oral liquid for removing food retention and relieving cough in children as claimed in claim 2, wherein the chemical truth value of the contents of the index components synephrine, naringin, neohesperidin and phillyrin of the decoction in the step C is determined by HPLC, which comprises the following steps:
chromatographic conditions are as follows: the chromatographic column is Phenomenex
PFP; taking 0.1% perchloric acid as a mobile phase A, and calculating the ratio by volume as acetonitrile: methanol 9: 1, performing linear gradient elution for a mobile phase B;
preparation of control solutions: precisely weighing synephrine reference substance 16.70mg, naringin reference substance 24.03mg, neohesperidin reference substance 15.53mg and phillyrin reference substance 21.78mg, placing in the same 25ml measuring flask, adding 50% methanol, and ultrasonic dissolving to obtain mixed reference substance stock solution; precisely transferring 1ml of the mixed reference substance stock solution into a 25ml measuring flask, adding water to dilute to scale, shaking up, and filtering to obtain a reference substance solution;
preparation of a test solution: placing 5ml of each of the first and second decoction in step A in a 10ml measuring flask, diluting with ultrapure water to scale, centrifuging at 12000r/min for 10min, collecting supernatant, and filtering with 0.22 μm microporous membrane;
the determination method comprises the following steps: respectively and precisely absorbing 10 mul of each of the reference solution and the sample solution, injecting into a high performance liquid chromatograph, recording the chromatogram, and calculating the content by an external standard method to obtain the chemical truth value of the content of index components of the decoction, namely synephrine, naringin, neohesperidin and phillyrin.
4. The quality control method for the extraction process of the oral liquid for eliminating indigestion and relieving cough of children as claimed in claim 3, wherein the HPLC chromatographic conditions in the step C are as follows: the chromatographic column is Phenomenex
PFP (2), 4.6 x 250mm, 5 μm; taking 0.1% perchloric acid as a mobile phase A, and calculating the ratio by volume as acetonitrile: methanol 9: 1, performing linear gradient elution for the mobile phase B, wherein the elution procedure is as follows:
The column temperature is 35 ℃; the sample amount is 10 mul; the flow rate is 0.8 ml/min; the detection wavelength was 225 nm.
5. The method for controlling quality of an extraction process of an oral liquid for eliminating food stagnation and relieving cough in children according to claim 2, wherein the modeling bands in the step D are as follows: the optimal spectral ranges of naringin, neohesperidin and phillyrin are all 9400-7496cm-1The wave band, the spectral range of synephrine is 9400-7496cm-1、6104-5448cm-1And (4) dual wave bands.
6. The quality control method for the extraction process of the oral liquid for removing food stagnation and relieving cough for children as claimed in claim 4 or 5, wherein the spectrum pretreatment method in step D is as follows: the pretreatment methods of synephrine and forsythin are both to eliminate constant deviation values, and both naringin and neohesperidin adopt non-spectral pretreatment.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113933427A (en) * | 2021-10-15 | 2022-01-14 | 北京中医药大学 | UPLC-based fingerprint spectrum establishment method and quality evaluation method of children's food retention removal and cough relieving oral liquid |
| CN113933427B (en) * | 2021-10-15 | 2024-05-14 | 北京中医药大学 | UPLC-based fingerprint spectrum establishment method and quality evaluation method of children's anti-food retention and cough relieving oral liquid |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1823946A (en) * | 2005-12-28 | 2006-08-30 | 贵州益佰制药股份有限公司 | Quality control method of child speen supporting oral liquid preparation |
| CN103383352A (en) * | 2012-05-03 | 2013-11-06 | 天津天士力之骄药业有限公司 | Near infrared transmitted spectrum detection method of naringin and/or neohesperidin |
| CN106770010A (en) * | 2016-12-15 | 2017-05-31 | 扬子江药业集团有限公司 | A kind of weisu granules extract solution concentration process On-line near infrared analyzer detection method |
| CN107036997A (en) * | 2016-11-11 | 2017-08-11 | 辽宁华润本溪三药有限公司 | Method and application using the preparation process of near infrared spectroscopy quick detection qizhi weitong granules |
| CN107315060A (en) * | 2017-07-19 | 2017-11-03 | 山东省分析测试中心 | A kind of method for building up of " Xiaoer Xiaoji Zhike " Oral Liquor multi objective quantitative finger print atlas |
| CN109856084A (en) * | 2019-03-26 | 2019-06-07 | 河南中医药大学 | A kind of stomach pill of aucklandia and amomum fruit condensed pill preparation process quality monitoring method |
| CN111529608A (en) * | 2020-03-30 | 2020-08-14 | 鲁南制药集团股份有限公司 | Application of preparation for removing food retention and relieving cough for children in preparation of medicine for treating fever and preparation method thereof |
-
2020
- 2020-09-23 CN CN202011009489.0A patent/CN112113929A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1823946A (en) * | 2005-12-28 | 2006-08-30 | 贵州益佰制药股份有限公司 | Quality control method of child speen supporting oral liquid preparation |
| CN103383352A (en) * | 2012-05-03 | 2013-11-06 | 天津天士力之骄药业有限公司 | Near infrared transmitted spectrum detection method of naringin and/or neohesperidin |
| CN107036997A (en) * | 2016-11-11 | 2017-08-11 | 辽宁华润本溪三药有限公司 | Method and application using the preparation process of near infrared spectroscopy quick detection qizhi weitong granules |
| CN106770010A (en) * | 2016-12-15 | 2017-05-31 | 扬子江药业集团有限公司 | A kind of weisu granules extract solution concentration process On-line near infrared analyzer detection method |
| CN107315060A (en) * | 2017-07-19 | 2017-11-03 | 山东省分析测试中心 | A kind of method for building up of " Xiaoer Xiaoji Zhike " Oral Liquor multi objective quantitative finger print atlas |
| CN109856084A (en) * | 2019-03-26 | 2019-06-07 | 河南中医药大学 | A kind of stomach pill of aucklandia and amomum fruit condensed pill preparation process quality monitoring method |
| CN111529608A (en) * | 2020-03-30 | 2020-08-14 | 鲁南制药集团股份有限公司 | Application of preparation for removing food retention and relieving cough for children in preparation of medicine for treating fever and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113933427A (en) * | 2021-10-15 | 2022-01-14 | 北京中医药大学 | UPLC-based fingerprint spectrum establishment method and quality evaluation method of children's food retention removal and cough relieving oral liquid |
| CN113933427B (en) * | 2021-10-15 | 2024-05-14 | 北京中医药大学 | UPLC-based fingerprint spectrum establishment method and quality evaluation method of children's anti-food retention and cough relieving oral liquid |
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