CN115112797A - Method for detecting quality of children's granule for removing food retention and relieving cough and application thereof - Google Patents
Method for detecting quality of children's granule for removing food retention and relieving cough and application thereof Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The invention relates to the field of traditional Chinese medicine preparation analysis, and in particular relates to a quality detection method and application of children's food retention removal and cough relieving granules. The quality detection method established by the invention is stable and controllable, and the detection method in the quality standard can be used for exclusively, repeatedly and effectively controlling the quality of the product, thereby ensuring the safety and effectiveness of clinical medication.
Description
Technical Field
The invention relates to a quality detection method of children's indigestion eliminating cough relieving granules and application thereof, belonging to the field of traditional Chinese medicine preparation analysis.
Background
The infantile stagnation-removing cough-relieving granule is loaded in an SFDA standard promulgated piece (2010), is prepared from 10 raw medicinal materials of hawthorn, areca seed, immature bitter orange, loquat leaf, snakegourd fruit, fructus forsythiae, radish seed, semen lepidii, periostracum cicadae and platycodon grandiflorum, has the effects of clearing heat, purifying lung, removing stagnation and relieving cough, is clinically used for treating cough, exacerbation at night, wheezy phlegm, abdominal distension and halitosis caused by infantile food stagnation and phlegm heat accumulation in the lung, and has obvious clinical effect. The medicine of the invention is named as Xiao 'er Xiao Jie Zhi Keli (approved article: Chinese medicine standard Z20060159), which are Chinese patent medicine products of Lu' nan thicket pharmaceutical Co Ltd, and the trade name is
The children's granule for removing food retention and relieving cough aims at the cough caused by the children's dyspepsia and stagnated heat, has reasonable prescription, has double effects of promoting digestion and removing food retention, and reducing phlegm and relieving cough, provides a treatment method for removing food retention and relieving cough for the first time, opens up a new way for the traditional Chinese medicine to treat the dyspepsia and cough, fills the blank of the medicines for treating the dyspepsia and cough in the market, and perfects the traditional Chinese medicine theoretical system of cough. Years of clinical application show that the traditional Chinese medicine composition has definite curative effect, is particularly suitable for children patients with food retention and cough, and is well received by doctors and patients.
At present, no patent publication and literature report exists for researching the quality detection method of the infantile indigestion eliminating and cough relieving granules. The invention discloses a method for detecting naringin in children's food retention removing and cough relieving granules by an HPLC method, and also discloses a method for qualitatively identifying betel nut, immature bitter orange and weeping forsythia in children's food retention removing and cough relieving granules by a TLC method, thereby filling the blank of the research on the quality detection method of the children's food retention removing and cough relieving granules.
Disclosure of Invention
The invention aims to provide a quality detection method of a Chinese patent medicine infantile food retention removing and cough relieving granule for treating food retention and cough, and the infantile food retention removing and cough relieving granule is prepared by extracting and purifying 10 raw material medicinal materials of hawthorn, areca seed, immature bitter orange, loquat leaf, snakegourd fruit, weeping forsythia capsule, radish seed, pepperweed seed, cicada slough and platycodon root.
The invention adopts HPLC to measure the naringin content in the preparation, and simultaneously adopts thin-layer chromatography to qualitatively detect 3 raw medicinal materials of areca, immature bitter orange and forsythia in the preparation, thereby realizing accurate evaluation and control of the quality of the infantile indigestion and cough relieving granules, and providing accurate basis for true and false identification and internal quality detection of the infantile indigestion and cough relieving granules.
A quality detection method for XIAO ER XIAO JI ZHI KE LI (infantile dyspepsia relieving and cough relieving granule) comprises determining naringin content in the preparation by HPLC, and comprises the following steps:
1) preparing a test solution: weighing infantile indigestion eliminating cough relieving granule, adding methanol solution, ultrasonic extracting, weighing, supplementing methanol to reduce weight loss, filtering, and collecting filtrate to obtain test solution;
2) preparation of a reference solution: collecting naringin reference substance, and adding methanol to obtain reference substance solution;
3) HPLC chromatographic conditions: octadecylsilane chemically bonded silica is used as a filling agent; methanol is taken as a mobile phase A, and water is taken as a mobile phase B; the theoretical plate number is not less than 3000 calculated according to naringin peak;
4) the determination method comprises the following steps: respectively sucking the reference solution and the test solution, injecting into a liquid chromatograph, measuring and calculating.
Preferably, the content of naringin in the preparation is determined by HPLC method, and the steps are as follows:
1) preparing a test solution: taking infantile indigestion eliminating cough relieving granules, grinding, taking 0.3g, precisely weighing, placing into a conical flask with a plug, precisely adding 50mL of 50% methanol, weighing, carrying out ultrasonic treatment at the power of 250W and the frequency of 40kHz for 30 minutes, cooling, weighing again, complementing the weight loss by 50% methanol, shaking up, filtering, and taking the subsequent filtrate to obtain the infantile cough relieving granules;
2) preparation of a reference solution: taking a proper amount of naringin reference substance, precisely weighing, and adding 50% methanol to prepare a solution containing 60 μ g of naringin reference substance per 1 mL;
3) HPLC chromatographic conditions: octadecylsilane chemically bonded silica is used as a filling agent; the mobile phase is methanol-water (35: 65); the detection wavelength is 283 nm; the flow rate is 0.8 mL/min; the column temperature was 40 ℃; the theoretical plate number is not less than 3000 calculated according to naringin peak;
4) the determination method comprises the following steps: precisely sucking 5 μ L of each of the reference solution and the sample solution, injecting into liquid chromatograph, and measuring.
Preferably, the immature bitter orange medicinal material in the children indigestion removing granule is naringin (C) 27 H 32 O 14 ) The content of the product should not be less than 15.0mg per bag.
The treatment and detection method of the infantile indigestion eliminating and cough relieving granules also comprises a qualitative identification method of at least one raw material medicinal material of areca, immature bitter orange and weeping forsythia:
1) the identification of the areca nut serving as a raw material medicine in the granules for removing food retention and relieving cough of children:
taking 10g of children's indigestion-eliminating cough-relieving granules, grinding, adding 3mL of concentrated ammonia test solution and 30mL of trichloromethane, heating and refluxing for 1 hour in a water bath, filtering, taking a trichloromethane layer, adding 5mL of dilute hydrochloric acid and 20mL of water, shaking for extraction, separating an acid water layer, adjusting the pH value to 8-9 by using the concentrated ammonia test solution, adding the trichloromethane for shaking for extraction twice, each time by 20mL, combining the trichloromethane solutions, steaming to be nearly dry, and adding 0.5mL of methanol to dissolve residues to obtain a test solution; taking 1g of areca catechu reference medicinal material, and preparing a reference medicinal material solution according to the same method in the step 1); respectively sucking 10 mu L of test solution and 5 mu L of reference medicinal material solution, respectively dropping on the same silica gel G thin layer plate, adding cyclohexane: ethyl acetate: and (3) putting the concentrated ammonia test solution (7.5: 7.5: 0.2) as a developing agent into a developing cylinder pre-saturated by ammonia vapor, developing, taking out, drying in the air, fumigating in iodine vapor until spots are clear, and inspecting in the sun. Spots of the same color appear in the chromatogram of the test solution at the positions corresponding to those in the chromatogram of the reference solution;
2) identification of immature bitter orange serving as a raw material medicine in the children's granules for removing food retention and relieving cough:
taking 3g of the children's indigestion removing and cough relieving granules, grinding, adding 25mL of methanol, carrying out ultrasonic treatment for 40 minutes, filtering, and steaming on a water bath to about 5mL to obtain a test solution; taking synephrine reference substance, adding methanol to prepare a solution containing 0.5mg per 1mL as reference substance solution; respectively sucking 10 mu L of test solution and 2 mu L of reference solution, respectively dropping on the same silica gel G thin layer plate prepared by 4% sodium acetate solution, adding chloroform: methanol: developing the lower layer solution of concentrated ammonia solution at a ratio of 20:5:1.5 as developing agent, taking out, air drying, heating in a 60 ℃ oven for about 15 minutes, taking out, cooling, spraying with 0.2% ninhydrin ethanol solution, heating at 105 ℃ until the spots are clearly developed, and inspecting in sunlight. Spots with the same color appear on the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference solution;
3) the identification of the fructus forsythiae serving as the raw material in the granules for removing food retention and relieving cough of children comprises the following steps:
taking 3g of the infantile indigestion removing and cough relieving granules, grinding, adding 25mL of methanol, carrying out ultrasonic treatment for 40 minutes, filtering, and steaming on a water bath to about 5mL to be used as a test solution; collecting fructus forsythiae control material 2g, adding water 20mL, heating under reflux for 30 min, filtering, extracting the filtrate with water saturated n-butanol under shaking for 3 times, each time 15mL, mixing n-butanol extractive solutions, evaporating to dryness, and dissolving the residue with methanol 2mL to obtain control solution; respectively sucking 5 mul of test solution and control solution, respectively, and respectively dropping on the same silica gel G thin layer plate, adding chloroform: developing with methanol 20:3 as developing agent, taking out, air drying, spraying 5% vanillin sulfuric acid solution, heating at 105 deg.C until the spots are clearly developed, and inspecting in sunlight. The main spots of the same color appear on the chromatogram of the test solution at the positions corresponding to those on the chromatogram of the reference solution.
Preferably, the infantile food retention removing and cough relieving granule is prepared from the following traditional Chinese medicine components:
preferably, the hawthorn is fried hawthorn, the loquat leaves are loquat leaves, the radish seeds are fried radish seeds, and the lepidium seeds are fried lepidium seeds.
Compared with the prior art, the invention has the following beneficial technical effects:
1) the invention establishes a quality detection method for the children's food retention removing and cough relieving granules for the first time, and simultaneously adopts the thin-layer chromatography to qualitatively detect 3 raw medicinal materials of areca nuts, immature bitter oranges and forsythia fruits in the preparation, thereby realizing the accurate evaluation and control of the quality of the children's food retention removing and cough relieving granules and filling the blank of the detection method for the children's food retention removing and cough relieving granules;
2) the method has the advantages of rapidness, sensitivity, good repeatability and the like, can accurately detect the content of the naringin in the children's food retention removing and cough relieving granules, can accurately and directionally identify 3 raw medicinal materials in the preparation, has strong specificity and good reproducibility, can comprehensively and effectively control the quality of the children's food retention removing and cough relieving granules, is beneficial to stabilizing the quality of products, ensures the safety and effectiveness of clinical medication, and better meets the requirements of medical treatment and market.
Drawings
FIG. 1 is HPLC chromatogram of XIAO ER XIAO JI ZHI KE LI, wherein the upper part, middle part and lower part are respectively naringin reference chromatogram, negative reference chromatogram and sample chromatogram;
FIG. 2 is a standard curve diagram of determination of naringin in XIAO ER XIAO JI ZHI KE LI by HLPC method;
FIG. 3 is a chromatogram of Tianjin Denner Kromasil C18 (250X 4.6mm, 5 μm);
FIG. 4 is an Agilent ExtendedC 18 (250X 4.6mm, 5 μm) chromatogram;
FIG. 5 is an Agilent ZorbaxSBC18 (250X 4.6mm, 5 μm) chromatogram;
FIG. 6 is a chromatogram of thin layer of Arecae semen in XIAOERSXIAOJIZHIKE granule; wherein a is areca control medicinal material, b is negative control, c is sample, and d is areca control medicinal material;
FIG. 7 is a thin layer chromatogram of Citrus aurantium; wherein a is synephrine reference substance, b is test substance, c is negative reference substance, d is synephrine reference substance;
FIG. 8 is a thin layer chromatogram of Forsythia suspensa; wherein a fructus forsythiae control medicinal material, b negative control, c test sample and d fructus forsythiae control medicinal material.
Detailed Description
The present invention will be further described below by way of exemplary embodiments in order to more fully understand the present invention. The invention discloses a children's food retention and cough relieving granule in the specification and the claims, which refers to a sample produced by Luonanpu pharmaceutical Co., Ltd, and the prescription proportion and the preparation method thereof are clearly defined in the above invention content.
Example 1 HPLC determination methodology study of naringin in XIAO ER XIAO JI ZHI KE LI
1 instrument and reagent Agilent1100 high performance liquid chromatograph, VWD detector.
2 chromatographic conditions an Tianjin Terna Kromasil C18 chromatographic column (4.6 mm. times.250 mm,5 μm); the mobile phase is methanol-water (35: 65); the detection wavelength is 283 nm; the flow rate is 0.8 mL/min; the column temperature was 40 ℃.
3 preparation of test solution A proper amount of XIAO ER XIAO JI ZHI KE LI (batch No. 180204) is ground, 0.3g is taken, precisely weighed, placed in a conical flask with a plug, 50mL of 50% methanol is precisely added, the weight is weighed, ultrasonic treatment (power 250W, frequency 40kHz) is carried out for 30 minutes, cooling is carried out, the weight is weighed again, the lost weight is complemented with 50% methanol, shaking is carried out uniformly, filtering is carried out, and a subsequent filtrate is taken, thus obtaining the test solution.
4 preparation of reference solution A proper amount of naringin reference (batch No. 110722-201312, China institute for food and drug testing) was weighed precisely, and 50% methanol was added to prepare solutions containing 0.060072mg per 1 mL.
5 preparation of negative control solution A negative control solution without immature bitter orange is prepared by the same method as the preparation of the test solution, and the position of naringin is not interfered as can be seen from the chromatogram. See figure 1.
6 Linear relationship examination precisely absorb the naringin reference solution of 0.5006mg/mL, precisely absorb 1mL, 2mL, 3mL, 4mL and 5mL respectively, put into 25mL measuring flask respectively, add 50% methanol to dilute to the scale, shake up, sample injection, determine peak area, as table 1. And drawing a standard curve by taking the measured peak area as an abscissa and the reference sample concentration (mg/mL) as an ordinate, wherein the regression equation Y is 190124435.67719X-33294.5, R2 is 0.99995, and the naringin sample concentration is in the range of 0.020024-0.100120mg/mL, and has good linearity. The results are shown in FIG. 2.
TABLE 1 results of linear relationship examination
7 precision test the control solution was precisely aspirated, and the sample injection was repeated 6 times, 5 μ L each time, with a peak area RSD of 0.455%, indicating good instrument precision. The results are shown in Table 2.
TABLE 2 results of precision tests
8, the stability test takes the same test solution, and the test is carried out for 0h, 2h, 4h, 6h and 8h after the preparation, and the result shows that the test solution is stable within 8 h. The results are shown in Table 3.
TABLE 3 stability test results
9 repeatability test 6 samples of the same batch were taken, respectively measured according to the sample preparation method under the item of "preparation of test sample solution", and the calculated content was 1.004%. The results are shown in Table 4.
TABLE 4 results of the repeatability tests
10 percent recovery test 0.5006mg/mL reference substance solution was precisely measured, 6 parts each of 2mL were precisely aspirated, placed in conical flasks, the solvent was volatilized, 6 parts each of 0.15g of sample was precisely weighed, placed in the conical flasks, 50mL of 50% methanol was precisely added, sonication was performed for 30 minutes, cooling, complementing, shaking, filtration, and sample injection was performed, and the average naringin recovery rate was 99.29% and RSD was 1.156%. The results are shown in Table 5.
TABLE 5 recovery test results
11 durability test different brands and models of chromatographic columns are used, and the test is carried out according to the text test method, which is shown in the attached figures 3, 4 and 5 respectively, and the separation is good and the negative is free from interference. In the figure, the upper part, the middle part and the lower part are respectively a naringin reference substance, a negative reference substance and a sample chromatogram
12 sample content measurement samples were taken according to the same method as the above sample treatment method, and the results are shown in table 6.
TABLE 6 results of content measurement of samples
13 content limit this application is for adjuvant change application, and methodology research shows that adjuvant change has no influence on content determination, and each bag of the product contains fructus Aurantii Immaturus and naringin (C) 27 H 32 O 14 ) Calculated, the content of the active ingredients should not be less than 15.0 mg.
EXAMPLE 2 methodological study of thin layer chromatography to identify Areca catechu in formulations
Taking 10g of children's indigestion eliminating cough relieving granules (batch number: 180204), grinding, adding 3mL of concentrated ammonia test solution and 30mL of trichloromethane, placing in a water bath, heating and refluxing for 1 hour, filtering, taking a trichloromethane layer, adding 5mL of dilute hydrochloric acid and 20mL of water, shaking for extraction, separating an acid water layer, adjusting the pH value to 8-9 by using the concentrated ammonia test solution, adding 20mL of trichloromethane for shaking for extraction twice, each time, combining the trichloromethane solution, steaming to be nearly dry, adding 0.5mL of methanol to dissolve residues to obtain a test solution. Taking another 1g of Arecae semen as control, and making into control solution by the same method. Taking 10G of areca negative control particles, preparing a negative control solution by the same method, sucking 10 mul of a test solution, 10 mul of the negative control solution and 5 mul of a control medicinal material solution, respectively dropping the solution on the same silica gel G thin-layer plate, placing the plate in a developing tank pre-saturated with ammonia vapor by taking cyclohexane-ethyl acetate-concentrated ammonia solution (7.5: 7.5: 0.2) as a developing agent, developing, taking out, drying in the air, placing the plate in iodine vapor for fumigating until spots are clear, and inspecting the plate under the sunlight. In the chromatogram of the test solution, spots with the same color appear at the corresponding positions of the chromatogram of the reference medicinal material, and the negative is not interfered, and the standard is listed. See figure 6.
Example 3 methodological study of thin layer chromatography to identify Poncirus trifoliata in formulations
Taking 3g of XIAOERGANXIAOZHIKE granule (batch number: 180204), adding 25mL of methanol, performing ultrasonic treatment for 40 min, filtering, and steaming on water bath to about 5mL to obtain test solution. Preparing a negative control solution from the immature bitter orange negative control particles by the same method. Methanol was added to a synephrine control (lot: 110727-201608, China institute for food and drug testing), and the solution containing 0.5mg of synephrine per 1mL was used as a control solution. Pipetting 10 mu L of each test solution, 10 mu L of each negative control solution and 2 mu L of each control solution, respectively dropping the solution on the same silica gel G thin-layer plate prepared by 4% sodium acetate solution, and adding chloroform: methanol: developing with concentrated ammonia solution (20: 5: 1.5) as developing agent, taking out, air drying, spraying 0.2% ninhydrin ethanol solution, heating until the spots are clearly developed, and inspecting in sunlight. Spots of the same color appear in the chromatogram of the test solution at positions corresponding to those in the chromatogram of the control solution. Negative without interference, the standard was included. See fig. 7.
Example 4 methodological study of thin layer chromatography to identify Forsythia suspensa in formulation
Taking 3g of XIAOERGANXIAOZHIKE granule (batch number: 180204), adding 25mL of methanol, performing ultrasonic treatment for 40 min, filtering, and steaming on water bath to about 5mL to obtain test solution. Preparing negative control solution from fructus forsythiae negative particles by the same method. And 2g of fructus forsythiae control medicinal material is taken, 20mL of water is added, heating reflux is carried out for 30 minutes, filtration is carried out, the filtrate is shaken and extracted for 3 times by using normal butanol, 15mL of the filtrate is taken each time, normal butanol extract is combined and evaporated to dryness, and 2mL of methanol is added into residue to dissolve the residue to be used as a control medicinal material solution. Sucking 5 mul of each of the test solution, the negative control solution and the control solution, respectively dropping on the same silica gel G thin layer plate, adding chloroform: developing with methanol 20:3 as developing agent, taking out, air drying, spraying 5% vanillin sulfuric acid solution, heating at 105 deg.C until the spots are clearly developed, and inspecting in sunlight. The main spots of the same color appear on the chromatogram of the test solution at the positions corresponding to those on the chromatogram of the reference solution. Negative without interference, the standard was included. See figure 8.
Claims (10)
1. A quality detection method for children's granules for resolving food stagnation and relieving cough is characterized in that the method comprises the following steps of determining the naringin content in the preparation by an HPLC method:
1) preparing a test solution: weighing infantile indigestion eliminating cough relieving granule, adding methanol solution, ultrasonic extracting, weighing, supplementing methanol to reduce weight loss, filtering, and collecting filtrate to obtain test solution;
2) preparation of a reference solution: collecting naringin reference substance, and adding methanol to obtain reference substance solution;
3) HPLC chromatographic conditions: octadecylsilane chemically bonded silica is used as a filling agent; methanol is taken as a mobile phase A, and water is taken as a mobile phase B; the theoretical plate number is not less than 3000 calculated according to naringin peak;
4) the determination method comprises the following steps: respectively sucking the reference solution and the test solution, injecting into a liquid chromatograph, measuring and calculating.
2. The quality detection method of claim 1, wherein the content of naringin in the preparation is determined by HPLC, comprising the following steps:
1) preparing a test solution: taking infantile indigestion eliminating cough relieving granules, grinding, taking 0.3g, precisely weighing, placing into a conical flask with a plug, precisely adding 50mL of 50% methanol, weighing, carrying out ultrasonic treatment at the power of 250W and the frequency of 40kHz for 30 minutes, cooling, weighing again, complementing the weight loss by 50% methanol, shaking up, filtering, and taking the subsequent filtrate to obtain the infantile cough relieving granules;
2) preparation of a control solution: taking a proper amount of naringin reference substance, precisely weighing, and adding 50% methanol to prepare a solution containing 60 μ g of naringin reference substance per 1 mL;
3) HPLC chromatographic conditions: octadecylsilane chemically bonded silica is used as a filling agent; the mobile phase is methanol-water; the flow rate is 0.6-1.2 mL/min; the theoretical plate number is not less than 3000 calculated according to naringin peak;
4) the determination method comprises the following steps: precisely sucking 5 μ L of each of the reference solution and the sample solution, injecting into liquid chromatograph, and measuring.
3. The quality inspection method according to claim 1, wherein the methanol-water volume ratio in step 3) is 35: 65; the detection conditions are as follows: the detection wavelength is 283 nm; the flow rate is 0.8 mL/min; the column temperature was 40 ℃.
4. The quality detection method of claim 1, wherein the amount of Citrus aurantium in the XIAOERGA XIAO JIE KE LI is not less than 15.0mg per bag, calculated as naringin.
5. The quality detection method according to claim 1 or 2, wherein the quality detection method for the infantile indigestion removing and cough relieving granule further comprises a qualitative identification method for at least one raw material drug selected from the following areca nut, immature bitter orange and forsythia fruit.
6. The quality detection method according to claim 5, wherein the identification of the raw material drug betel nut in the Xiao' er Xiao Ji Zhi Ke is as follows:
taking 10g of children's indigestion-eliminating cough-relieving granules, grinding, adding 3mL of concentrated ammonia test solution and 30mL of trichloromethane, heating and refluxing for 1 hour in a water bath, filtering, taking a trichloromethane layer, adding 5mL of dilute hydrochloric acid and 20mL of water, shaking for extraction, separating an acid water layer, adjusting the pH value to 8-9 by using the concentrated ammonia test solution, adding the trichloromethane for shaking for extraction twice, each time by 20mL, combining the trichloromethane solutions, steaming to be nearly dry, and adding 0.5mL of methanol to dissolve residues to obtain a test solution; preparing 1g of Arecae semen reference material, and making into reference material solution by the same method;
respectively sucking 10 mu L of test solution and 5 mu L of reference medicinal material solution, respectively dropping on the same silica gel G thin layer plate, adding cyclohexane: ethyl acetate: the concentrated ammonia solution (7.5: 7.5: 0.2) as developing agent is placed in a developing cylinder presaturated with ammonia vapor, developed, taken out, dried, smoked in iodine vapor until the spots are clear, and inspected in the sun. Spots of the same color appear on the chromatogram of the test solution at the positions corresponding to those on the chromatogram of the control solution.
7. The quality detection method of claim 4, wherein the identification of the medicinal material fructus Aurantii Immaturus in the infantile food stagnation removing and cough relieving granule comprises:
taking 3g of the infantile indigestion removing and cough relieving granules, grinding, adding 25mL of methanol, carrying out ultrasonic treatment for 40 minutes, filtering, and steaming on a water bath to about 5mL to be used as a test solution; taking synephrine reference substance, adding methanol to prepare a solution containing 0.5mg per 1mL as reference substance solution; respectively sucking 10 mu L of test solution and 2 mu L of reference solution, respectively dropping on the same silica gel G thin layer plate prepared by 4% sodium acetate solution, adding chloroform: methanol: developing the lower layer solution of concentrated ammonia solution at a ratio of 20:5:1.5 as developing agent, taking out, air drying, heating in a 60 ℃ oven for about 15 minutes, taking out, cooling, spraying with 0.2% ninhydrin ethanol solution, heating at 105 ℃ until the spots are clearly developed, and inspecting in sunlight. Spots of the same color appear in the chromatogram of the test solution at positions corresponding to those in the chromatogram of the control solution.
8. The quality detection method of claim 5, wherein the identification of fructus forsythiae as the raw material of the infantile indigestion relieving cough granule comprises the following steps:
taking 3g of the infantile indigestion removing and cough relieving granules, grinding, adding 25mL of methanol, carrying out ultrasonic treatment for 40 minutes, filtering, and steaming on a water bath to about 5mL to be used as a test solution; collecting fructus forsythiae control material 2g, adding water 20mL, heating under reflux for 30 min, filtering, extracting the filtrate with water saturated n-butanol under shaking for 3 times, each time 15mL, mixing n-butanol extractive solutions, evaporating to dryness, and dissolving the residue with methanol 2mL to obtain control solution; respectively sucking 5 mul of test solution and control solution, respectively, and respectively dropping on the same silica gel G thin layer plate, adding chloroform: developing with methanol 20:3 as developing agent, taking out, air drying, spraying 5% vanillin sulfuric acid solution, heating at 105 deg.C until the spots are clearly developed, and inspecting in sunlight. The main spots of the same color appear on the chromatogram of the test solution at the positions corresponding to those on the chromatogram of the reference solution.
9. The method of claim 1, wherein the pediatric food stagnation eliminating and cough relieving granules are prepared from the following traditional Chinese medicine components:
200 parts by weight of 120 parts by weight of hawthorn fruit, 120 parts by weight of areca seed, 200 parts by weight of 120 parts by weight of loquat leaf, 200 parts by weight of loquat leaf
120 portions of immature bitter orange, 120 portions of radish seed, 200 portions of snakegourd fruit, 180 portions of snakegourd fruit, 268 portions
150 portions of semen lepidii, 220 portions of balloonflower, 150 portions of balloonflower, 220 portions of forsythia, 150 portions of forsythia, 220 portions
80-130 parts of cicada slough.
10. The method as claimed in claim 8, wherein the hawthorn is parched hawthorn, the loquat leaf is eriobotrya japonica, the radish seed is parched radish seed, and the lepidium seed is parched lepidium seed.
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