CN113834895A - Quality control method of amygdalin in infantile lung heat cough and asthma granules - Google Patents
Quality control method of amygdalin in infantile lung heat cough and asthma granules Download PDFInfo
- Publication number
- CN113834895A CN113834895A CN202110998947.6A CN202110998947A CN113834895A CN 113834895 A CN113834895 A CN 113834895A CN 202110998947 A CN202110998947 A CN 202110998947A CN 113834895 A CN113834895 A CN 113834895A
- Authority
- CN
- China
- Prior art keywords
- solution
- amygdalin
- asthma
- mobile phase
- cough
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- 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
Abstract
The invention provides a quality control method of amygdalin in particles for treating cough and asthma caused by lung heat of children, and a thin-layer chromatography identification method has the advantages of small quantity of samples, good separation effect, clear spots, moderate specific displacement value and good reproducibility. The amygdalin component in the infantile lung-heat cough and asthma granules is quantitatively analyzed by content measurement, the content measurement chromatographic conditions of the method can accurately and efficiently detect the amygdalin content in the infantile lung-heat cough and asthma granules by verification, and the content of the amygdalin in the infantile lung-heat cough and asthma granules can be effectively controlled by combining a thin-layer chromatography identification method and the content measurement, so that the medication safety of the infantile lung-heat cough and asthma granules is ensured.
Description
Technical Field
The invention relates to the field of amygdalin detection, in particular to a quality control method of amygdalin in particles for treating infantile lung heat cough and asthma.
Background
The semen Armeniacae amarum is dried mature seed of Prunus Armeniaca, Prunus sibirica, Prunus northeast or Prunus armeniaca of Rosaceae. Bitter in nature, slightly warm, and slightly toxic; it enters lung and large intestine meridians. Has the effects of depressing qi, relieving cough and asthma, and relaxing bowel, and is mainly used for cough and asthma, fullness in chest and excessive phlegm, and constipation due to intestinal dryness.
Amygdalin is a common cyanogenic glycoside substance, is also an effective component in the traditional Chinese medicine of bitter apricot kernel, and has become a commonly used phlegm-eliminating cough-relieving agent and an auxiliary anticancer drug in medicine so far. Besides amygdalin, amygdalin also contains beta-glucosidase. Amygdalin produces glucose and mandelonitrile under the action of beta-glucosidase, and mandelonitrile can produce hydrocyanic acid and benzaldehyde spontaneously or via hydroxyl nitrile lyase. A small amount of hydrocyanic acid has a sedative effect, can paralyze the cough center, and shows the effects of the almond such as relieving asthma and cough; and a large amount of hydrocyanic acid enters the human body and then has a poisoning risk. The cyano group is easy to combine with Fe3+ in the oxidation type cytochrome oxidase molecule, blocks oxygen reduction electron transfer, inhibits the activity of respiratory enzyme, causes cell asphyxia and finally leads to respiratory paralysis and death. Therefore, the amygdalin contained in the bitter almond is not only an effective component but also an endogenous toxic component. Therefore, a quality control method is needed for identifying and detecting the amygdalin content in the particles for treating cough and asthma due to lung heat in children, for example, CN201510160159.4 is used for determining the content of the active ingredient amygdalin in cough loquat syrup, 20% methanol aqueous solution is used as a mobile phase, octadecylsilane chemically bonded silica is used as a filler, wherein the flow rate of the mobile phase is 1.0mL/min, the column temperature is 30 ℃, the wavelength is 210nm, the simultaneous determination method of jasminoidin and amygdalin in CN202011391537.7 plaster for treating cough and asthma due to lung heat in children is performed by using a mixed solution of 207nm, 25 ℃ ± 1 ℃ and mobile phase as mobile phase a and mobile phase B, the mobile phase a is acetonitrile or methanol, and the mobile phase B is phosphoric acid solution or formic acid solution. Because the raw materials and the auxiliary materials in the medicine are different from the invention, the amygdalin peak separation effect is poor by using the method.
Disclosure of Invention
Therefore, the invention provides a quality control method of amygdalin in the infantile lung-heat cough and asthma granules, which tests the amygdalin in the infantile lung-heat cough and asthma granules by thin-layer chromatography and content measurement.
The technical scheme of the invention is realized as follows:
(1) thin layer chromatography identification test
S1: cyclohexane, trichloromethane, formic acid and toluene are used as developing agents.
S2: test solution: taking the particles for treating the cough and asthma caused by the lung heat of the children, adding acetonitrile, carrying out vortex oscillation, and filtering to obtain a test solution with the concentration of 0.1-1 mg/mL.
S3: control solution: taking amygdalin reference substance, adding acetonitrile, shaking up, filtering to prepare a reference solution with the concentration of 0.1-1 mg/mL.
S4: control solution: crushing bitter apricot seeds, adding acetonitrile, carrying out vortex oscillation, centrifuging, taking supernate and filtering to obtain a reference medicinal material solution with the concentration of 0.1-1 mg/mL.
S5: negative control sample solution: and taking the negative control, adding acetonitrile, carrying out vortex oscillation, and filtering to obtain a negative control sample solution with the concentration of 0.1-1 mg/mL.
S6: absorbing 6-8 mu l of each of a test solution, a control medicinal material solution and a negative control sample solution, respectively dotting the test solution, the control medicinal material solution and the negative control sample solution on the same silica gel G thin-layer plate, putting the silica gel G thin-layer plate into a developing agent, developing for 6-8 h, taking out, drying at the drying temperature of 80-100 ℃ for 5-10 min, detecting under an ultraviolet lamp at 365nm, spraying an ninhydrin sulfuric acid ethanol solution when main spots appear, and heating an oven until the spots are clear;
(2) determination of content
A1: test solution: dissolving the particles for treating the cough and asthma caused by the lung heat of the children in a solvent, carrying out vortex oscillation, and filtering to obtain a test solution with the concentration of 0.1-1 mg/mL.
A2: control solution: taking amygdalin reference substance, adding a solvent to dissolve, shaking up, and filtering to obtain a reference solution with the concentration of 0.1-1 mg/mL.
A3: negative control sample solution: and taking a negative control, adding a solvent for dissolving, carrying out vortex oscillation, and filtering to obtain a negative control sample solution with the concentration of 0.1-1 mg/mL.
A4: chromatographic conditions
Mobile phase A: lithium bromide with the volume percentage of 0.1-0.5%, acetone with the volume percentage of 10-20% and the balance acetonitrile are taken as a mobile phase A;
mobile phase B: taking an N, N-dimethylformamide aqueous solution with the mass concentration of 0.2-0.5% as a mobile phase B;
a chromatographic column: the stationary phase is a Boston Green ODS chromatographic column;
detection wavelength: 210 nm;
the elution conditions were:
0-15.0 min, wherein the volume ratio of the mobile phase A to the mobile phase B is 5-15: 85-95;
15.01-25.0 min, wherein the volume ratio of the mobile phase A to the mobile phase B is 20-30: 70-80;
25.01-40.0 min, wherein the volume ratio of the mobile phase A to the mobile phase B is 42-48: 52-58;
40.01-70.0 min, wherein the volume ratio of the mobile phase A to the mobile phase B is 5-15: 85-95.
Further, in the step (1), the volume fraction of the acetonitrile is 35-45%.
Further, in the step (1), the developing agent is prepared from cyclohexane, trichloromethane, formic acid and toluene in a volume ratio of 12:0.5:3: 7.
Further, a polytetrafluoroethylene filter membrane is adopted for filtration.
Further, in the step (2), the solvent is 1-2 wt% of sodium metabisulfite aqueous solution.
Furthermore, the rotational speed of the vortex oscillation is 500-1000 r/min, and the vortex oscillation time is 1-3 min.
Further, in the step (1), the usage amount of the developing agent is 150-200 mL.
Further, in the step (1), the ninhydrin sulfuric acid ethanol solution is prepared from 3-5% of ninhydrin, 10-15% of sulfuric acid and the balance of ethanol by mass percent.
Further, the mass fraction of the sulfuric acid is 75%.
Further, in the step (2), the column temperature is 25-35 ℃.
Further, in the step (2), the flow rate is 0.8-1.2 mL/min.
Further, in the step (2), the injection volume is 20. mu.l.
Further, in the step (2), the specification diameter of the chromatographic column is 4.6mm, the column length is 250mm, and the particle size of the filler is 5 um.
Further, in the step (1) S5, the temperature of the oven is 30-50 ℃.
Furthermore, the specification of a polytetrafluoroethylene filter membrane adopted for filtration is 0.45 μm.
Furthermore, the negative control is the infantile lung heat cough and asthma particle without amygdalin.
Compared with the prior art, the invention has the beneficial effects that:
the thin-layer chromatography identification method provided by the invention is used for qualitatively analyzing the amygdalin in the infantile lung heat cough and asthma granules by taking the amygdalin medicinal material and the amygdalin reference substance as the reference substances, and has the advantages of small sample quantity, good separation effect, clear spots, moderate specific displacement value and good reproducibility, and compared with negative reference, the amygdalin component is not interfered by other components in the preparation, and the specificity is strong. The amygdalin content in the particles for treating infantile lung heat cough and asthma is quantitatively analyzed through content measurement, the chromatographic conditions of the method can accurately and efficiently detect the amygdalin content in the particles for treating infantile lung heat cough and asthma through verification, the amygdalin content is not interfered by other raw materials and auxiliary materials, and the methodological verification result shows that the test results of a linear relation test, a repeatability test, a precision test, a solution stability test, a recovery rate test and the like all accord with the detection standard of Chinese pharmacopoeia. The invention can effectively control the content of the amygdalin in the infantile lung heat cough and asthma granules by a thin-layer chromatography identification method and content measurement, and ensure the medication safety of the infantile lung heat cough and asthma granules.
Drawings
FIG. 1 thin layer chromatogram of example 1
In the figure, spots from left to right are a test solution 1, a test solution 2, a test solution 3 and a reference solution
Detailed Description
In order to better understand the technical content of the invention, specific examples are provided below to further illustrate the invention.
The experimental methods used in the examples of the present invention are all conventional methods unless otherwise specified.
The materials, reagents and the like used in the examples of the present invention can be obtained commercially without specific description.
Amygdalin reference: batch number: 110820 and 201004; specification: 20 mg/count; the content is 93.6 percent; provided by the china pharmaceutical biologicals assay.
EXAMPLE 1 identification test of amygdalin in infantile Lung-Heat cough and asthma granule
(1) 200mL of developing agent is prepared, and the developing agent is prepared by mixing cyclohexane, trichloromethane, formic acid and toluene in a volume ratio of 12:0.5:3: 7.
(2) Test solution: dissolving 3 batches of infantile lung heat cough and asthma granules respectively by using acetonitrile with volume fraction of 40%, carrying out vortex oscillation at the rotating speed of 700r/min for 2min, and filtering by using a 0.45-micron polytetrafluoroethylene filter membrane to prepare a test solution with the concentration of 0.1 mg/mL.
(3) Control solution: dissolving amygdalin control with acetonitrile with volume fraction of 40%, shaking, and filtering with 0.45 μm polytetrafluoroethylene filter membrane to obtain control solution with concentration of 0.1 mg/mL.
(4) Sucking a test solution 1, a test solution 2, a test solution 3, a control solution and 7 mul of each solution, respectively dotting the solutions on the same silica gel G thin-layer plate, putting the silica gel G thin-layer plate into a developing agent, developing for 7 hours, taking out, drying at 90 ℃ for 8min, detecting under an ultraviolet lamp at 365nm, spraying ninhydrin sulfuric acid ethanol solution when main spots appear, heating at 50 ℃ in an oven until the spots are clear, wherein the ninhydrin sulfuric acid ethanol solution is prepared from 3% of ninhydrin, 12% of sulfuric acid with the mass fraction of 75% and the balance of ethanol by mass percent.
The experimental result shows that the thin-layer chromatography identification method has good separation effect, clear spots, moderate specific displacement value and good reproducibility.
Example 2 determination of amygdalin content in particles for treating cough and asthma due to lung-heat in children
Chromatographic conditions
Mobile phase A: lithium bromide with the mass percent of 0.3%, acetone with the mass percent of 15% and acetonitrile with the balance being used as a mobile phase A.
Mobile phase B: taking an N, N-dimethylformamide aqueous solution with the mass concentration of 0.3% as a mobile phase B;
a chromatographic column: the stationary phase was a Boston Green ODS column (4.6X 250mm,5 um).
Detection wavelength: 210 nm.
Sample introduction volume: 20 μ l.
Column temperature: at 30 ℃.
The elution conditions were:
example 3 determination of amygdalin content in particles for cough and asthma due to lung-heat in children
Chromatographic conditions
Mobile phase A: lithium bromide with the mass percent of 0.1%, acetone with the mass percent of 10% and acetonitrile with the balance being used as a mobile phase A.
Mobile phase B: and taking an N, N-dimethylformamide aqueous solution with the mass concentration of 0.2% as a mobile phase B.
A chromatographic column: boston Green ODS (4.6X 250mm,5 um).
Detection wavelength: 210 nm.
Sample introduction volume: 20 μ l.
Column temperature: at 30 ℃.
The elution conditions were:
| time (min) | Mobile phase A (v/v) | Mobile phase B (v/v) |
| 0～15.0 | 5 | 95 |
| 15.01～25.0 | 20 | 80 |
| 25.01～40.0 | 42 | 58 |
| 40.01～70.0 | 5 | 95 |
Example 4 determination of amygdalin content in particles for treating cough and asthma due to lung-heat in children
Chromatographic conditions
Mobile phase A: lithium bromide with the mass percent of 0.5%, acetone with the mass percent of 20% and acetonitrile with the balance being used as a mobile phase A.
Mobile phase B: and taking an N, N-dimethylformamide aqueous solution with the mass concentration of 0.5% as a mobile phase B.
A chromatographic column: the stationary phase was a Boston Green ODS column (4.6X 250mm,5 um).
Detection wavelength: 210 nm.
Sample introduction volume: 20 μ l.
Column temperature: at 30 ℃.
The elution conditions were:
| time (min) | Mobile phase A (v/v) | Mobile phase B (v/v) |
| 0～15.0 | 15 | 85 |
| 15.01～25.0 | 30 | 70 |
| 25.01～40.0 | 48 | 52 |
| 40.01～70.0 | 15 | 85 |
The amygdalin content of the same batch (batch No. 201711) of infantile lung-heat cough and asthma granules was determined by the content determination method of examples 2-4.
(1) Solvent: 1.5% wt aqueous sodium metabisulphite solution.
(2) Test solution: dissolving the infantile lung heat cough and asthma granules with a solvent, carrying out vortex oscillation at a rotation speed of 800r/min for 2min, and filtering with a 0.45-micron polytetrafluoroethylene filter membrane to obtain a test solution with a concentration of 0.5 mg/mL.
(3) Control solution: taking amygdalin reference substance, adding solvent solution, shaking, and filtering with 0.45 μm polytetrafluoroethylene filter membrane to obtain reference solution with concentration of 0.5 mg/mL.
(4) Negative control sample solution: dissolving the negative control with solvent at vortex oscillation speed of 800r/min for 2min, and filtering with 0.45 μm polytetrafluoroethylene filter membrane to obtain negative control sample solution with concentration of 0.5 mg/mL.
Determination result of amygdalin content in infantile lung-heat cough and asthma granules
| Name (R) | Example 1 | Example 2 | Example 3 |
| Amygdalin content mg/bag | 35.12 | 35.20 | 35.04 |
Comparative example 1
On the basis of the example 2, the polytetrafluoroethylene filter membrane was replaced with a polyethersulfone filter membrane, a polyvinyl chloride filter membrane and a polyvinylidene fluoride filter membrane of the same specifications, respectively, and the test was performed.
(1) Secondary filtrate 1 (teflon filter membrane): taking 20mg of the infantile lung-heat cough and asthma particles, adding 100mL of a solvent, carrying out vortex oscillation at the rotating speed of 800r/min for 2min, putting 10mL of a sample solution into an injector, filtering by using a 0.45-micrometer polytetrafluoroethylene filter membrane, respectively removing 2mL and 4mL, and taking a subsequent filtrate for sample injection analysis.
(2) Secondary filtrate 2 (polyethersulfone filter): taking 20mg of the particles for treating the cough and asthma caused by the lung heat of the children, adding 100mL of a solvent, carrying out vortex oscillation at the rotating speed of 800r/min for 2min, taking 10mL of a sample solution, placing the sample solution in an injector, filtering the sample solution by using a 0.45-micrometer polyether sulfone filter membrane, respectively removing 2mL and 4mL, and taking a subsequent filtrate for sample injection analysis.
(3) Secondary filtrate 3 (polyvinyl chloride filter): taking 20mg of the infantile lung-heat cough and asthma particles, adding 100mL of a solvent, carrying out vortex oscillation at the rotating speed of 800r/min for 2min, putting 10mL of a sample solution into an injector, filtering by using a 0.45-micrometer polyvinyl chloride filter membrane, respectively removing 2mL and 4mL, and taking a subsequent filtrate for sample injection analysis.
(4) Secondary filtrate 4 (polyvinylidene fluoride filter membrane): taking 20mg of the infantile lung heat cough and asthma particles, adding 100mL of a solvent, carrying out vortex oscillation at the rotating speed of 800r/min for 2min, putting 10mL of a sample solution into an injector, filtering by using a 0.45-micrometer polyvinylidene fluoride filter membrane, respectively removing 2mL and 4mL, and taking a subsequent filtrate for sample injection analysis.
(5) Centrifuging the solution: taking 20mg of the infantile lung heat cough and asthma particle, adding 100mL of solvent to prepare a test solution 5, carrying out vortex oscillation at the rotating speed of 800r/min for 2min, taking 10mL of the test solution 5, placing the test solution in a centrifuge tube, centrifuging at 3500r/min for 5min, and taking supernatant.
Adsorption rate (%) - (centrifugal solution peak area-continuous filtrate peak area)/centrifugal solution peak area × 100
| Name (R) | 1 | 2 | 3 | 4 |
| Continuing filtrate (2mL) | 0.5 | 0.8 | 0.7 | 0.9 |
| Continuing filtrate (4mL) | 0.6 | 0.9 | 0.7 | 0.9 |
The test result shows that the polytetrafluoroethylene filter membrane used in the invention has better adsorption effect.
Comparative example 2
Based on example 2, Boston Green ODS was replaced with YMC-Pack ODS and Agilent Spherisorb ODS of different specifications and brands for content determination. The results show that YMC-Pack ODS and Agilent Spherisorb ODS have poor separation effect and poor peak pattern.
Test examples
Example 2 methodology investigation was performed according to the appendix of the first part of the Chinese pharmacopoeia, the guidelines for the verification of the quality standard analysis method of Chinese herbs, and the results were as follows:
(1) system suitability test
A control solution was prepared according to the method of preparing the solution of example 2, and 6 needles were continuously injected.
The experimental result shows that the number of theoretical plates of amygdalin peaks is higher than 6000, and the standard requirements (the peak area is not lower than 2000) are met.
(2) Stability test of solution
Control solutions were prepared according to the method of solution preparation in example 2 and analyzed by injection at 0, 2, 4, 6, 8, 12, 16, 20, 24 h.
The experimental results show that the RSD (%) of the control solution is less than 2.0%, and the amygdalin control solution is stable within 24 hours.
(3) Linear relation test
Taking 53.12mg of amygdalin reference substance, precisely weighing, placing in a 50mL measuring flask to obtain a stock solution, and preparing the stock solution of the reference substance into solutions with linear relations of 50%, 75%, 100%, 125% and 150%, wherein the concentration of the 100% solution with linear relation is 0.1 mg/mL.
The experimental results are as follows: and drawing a standard curve by taking the peak area (Y) as an ordinate and the sample injection amount (X, mu g) as an abscissa, wherein a linear equation is as follows: the result shows that the amygdalin reference substance has good linear relation in the range of 50-150%.
(4) Recovery test
Taking amygdalin reference substance, preparing test solution with concentration of 80%, 100% and l 20%, wherein the concentration of the test solution with 100% concentration is 0.1mg/mL, and analyzing by sample injection.
The experimental result shows that the recovery rate is 99.25-100.13% and the RSD is 0.27% within the range of 80-l 20%, and the recovery rate test meets the requirements.
(5) Sample introduction precision test
Taking amygdalin reference substance solution for continuous sampling for 6 needles, and inspecting the retention time and RSD of peak area of the reference substance solution.
The retention time RSD of the experimental result is 0.8 percent, the peak area RSD is 0.5 percent, and the requirement is met.
(6) Intermediate precision test
Different experimenters use different instruments to perform tests on different days, and 6 needles of amygdalin reference substance solution are continuously injected for inspection of the retention time and the RSD of peak area of all reference substance solutions in injection precision tests and intermediate precision tests.
The retention time RSD of the experimental result is 1.1 percent, the peak area RSD is 0.7 percent, and the requirement is met.
(7) Repeatability test
The same batch (batch number: 201711) of infantile lung heat cough and asthma granules 6 bags are prepared into a test solution, and single sample is analyzed by double needles.
The experimental result shows that the peak area RSD is 0.4%, and the method for determining the content of the amygdalin in the particles for treating the cough and asthma with the lung heat of the children has good repeatability.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. The quality control method of the amygdalin in the infantile lung heat cough and asthma granules is characterized by comprising the following steps:
(1) thin layer chromatography identification test
S1: the developing agent is prepared from cyclohexane, trichloromethane, formic acid and toluene;
s2: test solution: taking the particles for treating the cough and asthma caused by the lung heat of the children, adding acetonitrile, carrying out vortex oscillation, and filtering to obtain a test solution with the concentration of 0.1-1 mg/mL;
s3: control solution: taking an amygdalin reference substance, adding acetonitrile, shaking up, and filtering to prepare a reference solution with the concentration of 0.1-1 mg/mL;
s4: control solution: crushing bitter apricot seeds, adding acetonitrile, carrying out vortex oscillation, centrifuging, taking supernate and filtering to obtain a reference medicinal material solution with the concentration of 0.1-1 mg/mL;
s5: negative control sample solution: taking a negative control, adding acetonitrile, carrying out vortex oscillation, and filtering to obtain a negative control sample solution with the concentration of 0.1-1 mg/mL;
s6: absorbing 6-8 mu l of each of a test solution, a control medicinal material solution and a negative control sample solution, respectively dotting the test solution, the control medicinal material solution and the negative control sample solution on the same silica gel G thin-layer plate, putting the silica gel G thin-layer plate into a developing agent, developing for 6-8 h, taking out, drying at the drying temperature of 80-100 ℃ for 5-10 min, detecting under an ultraviolet lamp at 365nm, spraying an ninhydrin sulfuric acid ethanol solution when main spots appear, and heating an oven until the spots are clear;
(2) determination of content
A1: test solution: dissolving the particles for treating the cough and asthma caused by the lung heat of the children with a solvent, carrying out vortex oscillation, and filtering to obtain a test solution with the concentration of 0.1-1 mg/mL;
a2: control solution: taking an amygdalin reference substance, dissolving the amygdalin reference substance in a solvent, shaking up, and filtering to prepare a reference solution with the concentration of 0.1-1 mg/mL;
a3: negative control sample solution: taking a negative control, adding a solvent for dissolving, carrying out vortex oscillation, and filtering to obtain a negative control sample solution with the concentration of 0.1-1 mg/mL;
a4: chromatographic conditions
Mobile phase A: lithium bromide with the volume percentage of 0.1-0.5%, acetone with the volume percentage of 10-20% and the balance acetonitrile are taken as a mobile phase A;
mobile phase B: taking an N, N-dimethylformamide aqueous solution with the mass concentration of 0.2-0.5% as a mobile phase B;
a chromatographic column: the stationary phase is a Boston Green ODS chromatographic column;
detection wavelength: 210 nm;
the elution conditions were:
0-15.0 min, wherein the volume ratio of the mobile phase A to the mobile phase B is 5-15: 85-95;
15.01-25.0 min, wherein the volume ratio of the mobile phase A to the mobile phase B is 20-30: 70-80;
25.01-40.0 min, wherein the volume ratio of the mobile phase A to the mobile phase B is 42-48: 52-58;
40.01-70.0 min, wherein the volume ratio of the mobile phase A to the mobile phase B is 5-15: 85-95.
2. The quality control method of amygdalin in the infantile lung heat cough and asthma granule as claimed in claim 1, wherein in step (1), the volume fraction of acetonitrile is 35-45%.
3. The method of claim 1, wherein the filtering is performed with a teflon filter membrane.
4. The method for quality control of amygdalin in the infantile lung heat cough and asthma granule as claimed in claim 1, wherein in the step (2), the solvent is 1-2 wt% sodium metabisulfite aqueous solution.
5. The method for controlling the quality of amygdalin in the infantile lung heat cough and asthma granule as claimed in claim 1, wherein the rotation speed of the vortex oscillation is 500-1000 r/min, and the vortex oscillation time is 1-3 min.
6. The quality control method of amygdalin in the infantile lung heat cough and asthma granule as claimed in claim 1, wherein in step (1), the amount of the developing agent is 150-200 mL.
7. The quality control method of amygdalin in children's lung-heat cough and asthma granules as claimed in claim 1, wherein in the step (1), the ninhydrin sulfuric acid ethanol solution is prepared from 3-5% ninhydrin, 10-15% sulfuric acid and the balance ethanol by mass percentage.
8. The method for quality control of amygdalin in pediatric lung heat cough and asthma granules according to claim 1 or 7, wherein the mass fraction of sulfuric acid is 75%.
9. The method for controlling the quality of amygdalin in the infantile lung heat cough and asthma particle as claimed in claim 1, wherein the developing agent is prepared from cyclohexane, chloroform, formic acid and toluene at a volume ratio of 12:0.5:3: 7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110998947.6A CN113834895B (en) | 2021-08-28 | 2021-08-28 | Quality control method of amygdalin in infantile lung heat cough and asthma granules |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110998947.6A CN113834895B (en) | 2021-08-28 | 2021-08-28 | Quality control method of amygdalin in infantile lung heat cough and asthma granules |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113834895A true CN113834895A (en) | 2021-12-24 |
| CN113834895B CN113834895B (en) | 2023-02-24 |
Family
ID=78961443
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110998947.6A Active CN113834895B (en) | 2021-08-28 | 2021-08-28 | Quality control method of amygdalin in infantile lung heat cough and asthma granules |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113834895B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1772214A (en) * | 2005-01-24 | 2006-05-17 | 王永钧 | Extraction process of effective component for compound Chinese medicine composition of asiaticoside |
| CN1876050A (en) * | 2005-06-03 | 2006-12-13 | 贵阳云岩西创药物科技开发有限公司 | Pharmaceutical preparation for treating prostatitis, its preparation process and quality control method |
| US20100273761A1 (en) * | 2004-10-25 | 2010-10-28 | Shunlin Ren | Nuclear sulfated oxysterol, potent regulator of lipid homeostasis, for therapy of hypercholesterolemia, hypertriglycerides, fatty liver diseases, and atherosclerosis |
| CN102297926A (en) * | 2011-07-12 | 2011-12-28 | 刘金伶 | Rapid TLC identification and three-component simultaneous quantitative determination method for antitussive tablets |
| CN105911211A (en) * | 2016-05-24 | 2016-08-31 | 四川逢春制药有限公司 | Detection method of Maxing cough syrup |
| CN107894488A (en) * | 2017-10-27 | 2018-04-10 | 哈尔滨市康隆药业有限责任公司 | A kind of method of quality control of concentrated type oral liquid for cough and asthma of children |
-
2021
- 2021-08-28 CN CN202110998947.6A patent/CN113834895B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100273761A1 (en) * | 2004-10-25 | 2010-10-28 | Shunlin Ren | Nuclear sulfated oxysterol, potent regulator of lipid homeostasis, for therapy of hypercholesterolemia, hypertriglycerides, fatty liver diseases, and atherosclerosis |
| CN1772214A (en) * | 2005-01-24 | 2006-05-17 | 王永钧 | Extraction process of effective component for compound Chinese medicine composition of asiaticoside |
| CN1876050A (en) * | 2005-06-03 | 2006-12-13 | 贵阳云岩西创药物科技开发有限公司 | Pharmaceutical preparation for treating prostatitis, its preparation process and quality control method |
| CN102297926A (en) * | 2011-07-12 | 2011-12-28 | 刘金伶 | Rapid TLC identification and three-component simultaneous quantitative determination method for antitussive tablets |
| CN105911211A (en) * | 2016-05-24 | 2016-08-31 | 四川逢春制药有限公司 | Detection method of Maxing cough syrup |
| CN107894488A (en) * | 2017-10-27 | 2018-04-10 | 哈尔滨市康隆药业有限责任公司 | A kind of method of quality control of concentrated type oral liquid for cough and asthma of children |
Non-Patent Citations (4)
| Title |
|---|
| 何佩等: "清金消咳胶囊的工艺改进及质量标准", 《实用医药杂志》 * |
| 刘文龙等: "苦杏仁苷溶度参数测定方法的比较研究", 《湖南中医药大学学报》 * |
| 胡英婕: "小儿肺热咳喘口服液中苦杏仁苷的提取工艺研究", 《广州化学》 * |
| 胡英婕: "小儿肺热咳喘颗粒的薄层色谱鉴别研究", 《辽宁医学院学报》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113834895B (en) | 2023-02-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US20210109068A1 (en) | Fingerprint detection method for antidepressant drug | |
| CN110736799B (en) | Quality detection method of traditional Chinese medicine children's cold-relieving granules | |
| CN109387587B (en) | Detection method of L-2-amino-5-guanidino valeric acid enantiomer | |
| CN107315059A (en) | The content assaying method of rifampin and its impurity in a kind of rifampicin capsules | |
| CN114252532B (en) | Method for establishing fingerprint of Fangfengsheng particles and fingerprint thereof | |
| CN113834895B (en) | Quality control method of amygdalin in infantile lung heat cough and asthma granules | |
| CN102078403A (en) | Detection method of Chinese traditional medicine preparation of oral liquid for treating infant cough with lung heat | |
| CN108414667B (en) | Method for detecting quality standard of Shengui Yixin granules | |
| CN112924583B (en) | Method for determining pyrrolizidine alkaloid in eupatorium | |
| CN110596274A (en) | Method for detecting 2-mercaptobenzothiazole in ceftriaxone sodium | |
| CN111707768B (en) | Method for detecting 22 organochlorine pesticide residues in total glucosides of paeony bulk drug | |
| CN112666278A (en) | Limit detection method for strychnine in Huatuo reconstruction pills | |
| CN113504326A (en) | Detection method of changyanning preparation | |
| CN115015452B (en) | Method for measuring content of allantoin and adenosine in Chinese yam by adopting one-measurement-multiple-evaluation method | |
| CN112618630A (en) | Compound thrombus-invigorating soft capsule and quality detection method thereof | |
| CN113655135A (en) | Quantitative detection method and limiting method of aristolochic acid I | |
| CN111239319A (en) | Method for measuring content of panax japonicus saponin IVa in laryngopharynx clearing oral liquid | |
| CN111337599A (en) | Pretreatment method, morphine detection method and application | |
| CN114414672B (en) | Method for determining and analyzing content of dioscin in Longxiang asthma relieving capsules | |
| CN117147738B (en) | Method for detecting aristolochic acid I in refreshment and reconstruction pill | |
| CN102841153B (en) | Quality control method of dandeng brain dredging pharmaceutic preparation | |
| CN113899841B (en) | Method for detecting pinoresinol diglucoside in ginkgo leaf extraction intermediate or preparation thereof | |
| CN111272916B (en) | Method for detecting content of penicillin V acid | |
| CN113820404B (en) | UPLC analysis method of ipratropium bromide aerosol | |
| CN115166083B (en) | Method for detecting fosfomycin trometamol related substances and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |