CN111830172A - Quality control method of pinellia ternata syrup - Google Patents
Quality control method of pinellia ternata syrup Download PDFInfo
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Images
Classifications
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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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
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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
- G01N2030/065—Preparation using different phases to separate parts of sample
Abstract
The invention relates to a quality control method of pinellia ternate syrup, which comprises the following steps: preparation of a test solution: adding a pinellia ternate syrup sample to be tested into an aqueous solution of sodium hydroxide, distilling, collecting distillate by using an aqueous solution of hydrochloric acid, filtering, and taking a subsequent filtrate to prepare a sample solution; preparation of control solutions: dissolving ephedrine hydrochloride and pseudoephedrine hydrochloride as reference substances in solvent to obtain reference substance solution; injecting the test solution and the reference solution into a liquid chromatograph for determination; the mobile phase of the liquid chromatograph is as follows: the volume ratio is 3.5-7: 93 to 96.5 acetonitrile-0.3 to 0.7 wt% phosphoric acid aqueous solution. The method realizes good separation effect of ephedrine hydrochloride and pseudoephedrine hydrochloride, has no interference to other substances, and has strong specificity, high accuracy and good reproducibility.
Description
Technical Field
The invention relates to the field of pharmaceutical analysis, in particular to a quality control method of pinellia ternate syrup.
Background
Pinellia ternate syrup is collected in "drug standards of Ministry of health" and Chinese medicinal preparations in the eighth book, the standard number is WS3-B-1527-93, the prescription consists of 9 Chinese herbal medicines such as raw pinellia ternate, ephedra, aster, platycodon grandiflorum, polygala tenuifolia, loquat leaf, dried orange peel, liquorice and peppermint oil, has the functions of relieving cough and reducing sputum, and is clinically used for treating cough with excessive phlegm and bronchitis. The ephedra herb has the effects of sweating, dispelling cold, dispersing lung qi and relieving asthma, is one of the ministerial drugs in the prescription, and has the effective components of ephedrine and pseudoephedrine which are extracts of the ephedra herb.
In the ministerial standards, only a physicochemical method is adopted to identify the pinellia ternate syrup, but no content measurement index exists, the controllability of the quality standard is too low, the internal quality of the product is difficult to monitor, and the quality control method needs to be improved. Because the effective components of the ephedra herb, namely the ephedrine and the pseudoephedrine, in the ephedra herb have better water solubility and the water extract has high content, the finished product is easy to detect, the ephedra herb is the monarch drug in the prescription of the pinellia tuber syrup, and the ephedrine and the pseudoephedrine are one of the effective components of the pinellia tuber syrup, so that the selection of the ephedrine and the pseudoephedrine in the ephedra herb as index components is favorable for controlling the quality of the pinellia tuber syrup.
In the existing literature, a plurality of methods for measuring the content of a single component of ephedrine or pseudoephedrine in a traditional Chinese medicine preparation are provided, such as measuring the content of ephedrine in pinellia ternate syrup by HPLC (high performance liquid chromatography) in Chenjihai and the like, and measuring the content of ephedrine hydrochloride in pinellia ternate cough syrup by HPLC (high performance liquid chromatography) in Xuyangli and the like, but a multi-component content measuring method with a good detection effect is not provided.
Disclosure of Invention
Based on the above, the invention aims to provide a quality control method of pinellia ternate syrup with strong specificity and good separation effect.
The specific technical scheme is as follows:
a quality control method of pinellia ternate syrup comprises the following steps:
preparation of a test solution: taking a pinellia ternate syrup sample, adding a sodium hydroxide aqueous solution, distilling, collecting distillate by using a hydrochloric acid aqueous solution, filtering, and taking a subsequent filtrate to prepare a sample solution;
preparation of control solutions: dissolving ephedrine hydrochloride and pseudoephedrine hydrochloride as reference substances in solvent to obtain reference substance solution;
injecting the test solution and the reference solution into a liquid chromatograph for determination;
the mobile phase of the liquid chromatograph is as follows: the volume ratio is 3.5-7: 93 to 96.5 acetonitrile-0.3 to 0.7 wt% phosphoric acid aqueous solution.
In some of these embodiments, the mobile phase is: the volume ratio is 5-6: 94 to 95 parts of acetonitrile-0.3 to 0.5 wt% of phosphoric acid aqueous solution.
In some embodiments, the mass concentration of the sodium hydroxide aqueous solution is 10% to 40%.
In some embodiments, the mass concentration of the sodium hydroxide aqueous solution is 25% to 40%.
In some embodiments, the mass concentration of the sodium hydroxide aqueous solution is 30-35%.
In some of these embodiments, the liquid chromatograph is a DIAMOND ODS C18 column; the detector of the liquid chromatograph is a VWD detector.
In some embodiments, the concentration of the hydrochloric acid aqueous solution is 0.05-0.5 mol/L; the concentration of the hydrochloric acid aqueous solution is preferably 0.05 to 0.15mol/L, and the concentration of the hydrochloric acid aqueous solution is more preferably 0.05 to 0.10 mol/L.
In some of these embodiments, the size of the column is: the length is 200 plus or minus 10mm multiplied by the diameter is 4.6 plus or minus 0.2mm, and the grain diameter is 5 plus or minus 0.2 mu m.
In some of these embodiments, the chromatographic conditions of the liquid chromatograph comprise:
the detection wavelength is 207 +/-5 nm;
the sample volume is 20 +/-2 mu L;
the column temperature is 25 +/-2 ℃;
the flow rate was 1. + -. 0.2 ml/min.
In some of these embodiments, the solvent is water.
In some embodiments, in the preparation process of the test solution, 1 to 3ml of sodium hydroxide aqueous solution is added to 1ml of the pinellia ternata syrup sample to be tested, and 1 to 3ml of distillate is collected by using 0.05 to 0.15ml of hydrochloric acid aqueous solution.
In some embodiments, the effective components of the pinellia ternate syrup are prepared from raw materials including raw pinellia ternate, ephedra, aster, platycodon grandiflorum, polygala tenuifolia, loquat leaf, tangerine peel, liquorice and peppermint oil.
Compared with the prior art, the invention has the following beneficial effects:
the invention adopts high performance chromatography, selects acetonitrile-phosphoric acid aqueous solution as a mobile phase according to the property characteristics of the pinellia ternate syrup, and precisely controls the concentration of the phosphoric acid aqueous solution to be 0.3-0.7 wt%, and the volume ratio of the acetonitrile to the phosphoric acid aqueous solution to be 3.5-7: 93-96.5, under the very suitable chromatographic condition, the method is matched with a specific preparation method of a test solution to be tested, so that the simultaneous determination of the contents of ephedrine hydrochloride and pseudoephedrine hydrochloride in the pinellia ternate syrup is finally realized, the good separation of the ephedrine hydrochloride and the pseudoephedrine hydrochloride is realized, the interference of other substances in the pinellia ternate syrup is eliminated, and the method is strong in specificity, high in accuracy and good in reproducibility.
Drawings
FIG. 1 is a chromatogram of ephedrine hydrochloride control (207 nm);
FIG. 2 is a chromatogram (207nm) of a mixed reference substance of ephedrine hydrochloride and pseudoephedrine hydrochloride;
FIG. 3 is a chromatogram of a sample of pinellia ternata syrup (207 nm);
FIG. 4 is a chromatogram of a herba Ephedrae negative control sample (207 nm).
Detailed Description
Experimental procedures according to the invention, in which no particular conditions are specified in the following examples, are generally carried out under conventional conditions, or under conditions recommended by the manufacturer. The various chemicals used in the examples are commercially available.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The terms "comprising" and "having," and any variations thereof, are intended to cover non-exclusive inclusions. For example, a process, method, apparatus, article, or device that comprises a list of steps is not limited to only those steps or modules listed, but may alternatively include other steps not listed or inherent to such process, method, article, or device.
The "plurality" referred to in the present invention means two or more. "and/or" describes the association relationship of the associated objects, meaning that there may be three relationships, e.g., a and/or B, which may mean: a exists alone, A and B exist simultaneously, and B exists alone. The character "/" generally indicates that the former and latter associated objects are in an "or" relationship.
The embodiment provides a quality control method of pinellia ternate syrup, which comprises the following steps:
preparation of a test solution: taking a pinellia ternate syrup sample, adding a sodium hydroxide aqueous solution, distilling, collecting distillate by using a hydrochloric acid aqueous solution, filtering, and taking a subsequent filtrate to prepare a sample solution;
preparation of control solutions: dissolving ephedrine hydrochloride and pseudoephedrine hydrochloride as reference substances in solvent to obtain reference substance solution;
injecting the test solution and the reference solution into a liquid chromatograph for determination;
the mobile phase of the liquid chromatograph is as follows: the volume ratio is 3.5-7: 93 to 96.5 acetonitrile-0.3 to 0.7 wt% phosphoric acid aqueous solution.
The herba ephedrae is a monarch drug in the prescription of the pinellia ternata syrup, and the ephedrine and the pseudoephedrine are one of the important effective components of the pinellia ternata syrup, so that the content measurement by selecting the ephedrine and the pseudoephedrine in the herba ephedrae as index components is beneficial to controlling the quality of the pinellia ternata syrup.
In the research process, the inventor finds that in order to obtain a chromatogram with good peak shape and high separation degree, the concentration of a mobile phase phosphoric acid aqueous solution is very critical, the concentration of the phosphoric acid aqueous solution is controlled to be 0.3-0.7 wt%, particularly 0.3-0.5 wt%, and the volume ratio of acetonitrile to the phosphoric acid aqueous solution is 5-6: 94-95, the interference of other substances in the pinellia ternate syrup can be well eliminated, and the ephedrine hydrochloride and the pseudoephedrine hydrochloride can be well separated.
Meanwhile, the inventor finds that the pinellia ternate syrup sample has more and complex components, and the content of the target substance in the test solution prepared by the conventional dilution method is too low, so that the effective content measurement cannot be realized; when the extraction method is adopted, the removal effect on interfering impurities is poor, and the obtained test solution is too thick and difficult to operate. Finally, the invention discovers that the content of the target substance of the test solution prepared by the distillation method is obviously improved, and the test solution is strong in operability and easy to control. Especially, the sodium hydroxide aqueous solution with the mass concentration of 25-40% is added before distillation, so that the content of ephedrine hydrochloride and pseudoephedrine hydrochloride in the test solution can be obviously improved, and the stability among batches is good.
Under the very preferable chromatographic conditions, the chromatographic column of the liquid chromatograph is selected to be a DIAMOND ODS C18 column, and the obtained chromatogram has good separation effect and high accuracy. The conventional Hypersil ODS chromatographic column for determining the content of ephedrine in other Chinese medicinal preparations (such as cough syrup) can cause serious deformation of chromatogram under the chromatographic condition of the invention, and cannot be determined.
The present invention will be described in further detail with reference to specific examples.
Example 1
Instrument and reagent
1. Instrument for measuring the position of a moving object
Agilent 1200 high performance liquid chromatograph; a VWD detector.
A chromatographic column: DIAMOND ODS C18 column (200X 4.6mm, 5 μm), column number: 99902.
2. reagents and materials
Pinellia ternata syrup (batch No. N07004S, J05001, J10002 and A08001), and herba Ephedrae negative control sample (both produced and prepared by Guangzhou Baiyunshan Panshou pharmaceutical industry Co., Ltd.);
the ephedrine hydrochloride reference (batch No. 171241-200506) and the pseudoephedrine hydrochloride reference (batch No. 171237-200304) are all from China pharmaceutical biological product institute.
Acetonitrile is chromatographically pure; the water was ultrapure water and the other reagents were analytical grade (both manufactured and prepared by Tiandi corporation, USA).
Second, investigation of the preparation method of the test sample
Three preliminary experimental protocols were designed for the preparation of test solutions: direct dilution, extraction and distillation. The content of the target substance of the test solution prepared by the direct dilution method is too low; the sample solution extracted by the extraction method is too thick and thick, the extraction operation cannot be continued, and the impurity removal effect of the extraction method is poor, so that the display of a chromatographic peak can be interfered; the impurity removal effect of the test solution prepared by the distillation method is ideal, and the experiment is easy to control and operate, so that the distillation method is selected to prepare the pinellia ternate syrup test solution. The concentration of NaOH and HCl solutions was examined experimentally below by adding NaOH and HCl to the distillate during distillation.
Taking pinellia ternate syrup (batch number: N07004S), precisely measuring 50mL, placing into a 500mL Kjeldahl flask with a frosted opening, respectively adding 150mL of 10 wt%, 20 wt%, 30 wt% and 35 wt% sodium hydroxide aqueous solution, connecting with a distilling device, heating and distilling, collecting distillate to near scale with 100mL measuring bottles containing 5mL of 0.05, 0.1 and 0.5moL/L hydrochloric acid aqueous solution in advance, adding water to a constant volume to scale, shaking up, filtering, taking subsequent filtrate, and performing content measurement, wherein the result is shown in Table 1.
Table 1 pretreatment methods comparison
The results show that: when 30-35 wt% of sodium hydroxide solution is added for distillation, the content measurement values of ephedrine hydrochloride and pseudoephedrine reach stability. The contents of ephedrine hydrochloride and pseudoephedrine are not obviously different when the receiving solution of hydrochloric acid of 0.05mol/L, 0.1mol/L and 0.5mol/L is used for testing. According to the combined measurement result of the solution and the receiving solution used in the distillation in the pretreatment experiment, and considering that the chromatographic column is damaged greatly due to overlarge acidity, a 30 wt% sodium hydroxide solution and a 0.1mol/L hydrochloric acid solution are selected as the receiving solution in the distillation.
Thirdly, investigation of chromatographic conditions
1. Examination of mobile phase:
the research team of the invention carries out the research experiment of chromatographic conditions, repeatedly debugs, preliminarily selects a mobile phase of acetonitrile-0.4 wt% phosphoric acid solution (5:95) and acetonitrile-0.4 wt% phosphoric acid solution (4:96), and has great damage to the chromatographic column because the volume percentage of acetonitrile is found to be less than 5%. Acetonitrile-0.1% wt phosphoric acid solution (5:95) and acetonitrile-0.2% wt phosphoric acid solution (5:95) were tried as mobile phases, and it was found that the separation degree between ephedrine hydrochloride and pseudoephedrine hydrochloride and the impurity peak and the main peak were inferior to that of acetonitrile-0.4% wt phosphoric acid solution (5:95), so that it was finally determined that C18 column was used as the stationary phase and acetonitrile-0.4% wt phosphoric acid solution (5:95) was used as the mobile phase.
2. Investigation of the column:
durability tests have selected different chromatographic columns for detecting ephedrine hydrochloride and pseudoephedrine hydrochloride, and the C18 chromatographic column of Hypersil ODS filler is commonly used for measuring the content of ephedrine in other Chinese medicinal preparations (such as cough syrup), but we find that under the chromatographic conditions of the embodiment of the invention, the C18 chromatographic column of Hypersil ODS filler can not be used for measuring, and the filler can cause serious deformation of a chromatogram. Finally, the DIAMOND ODS C18 column is selected as the chromatographic column, the detection effect is good, the chromatographic conditions are matched, the separation effect of the chromatogram obtained by determination is good, and the accuracy is high.
Fourthly, verification of methodology
1. Chromatographic conditions and System suitability test
The column is a DIAMOND ODS C18 column; the mobile phase is acetonitrile-0.4 wt% phosphoric acid water solution (5: 95); the flow rate is 1 ml/min-1(ii) a Column temperature: 25 ℃; the detection wavelength is 207 nm; the amount of the sample was 20. mu.L. The theoretical plate number is not less than 4000 calculated according to ephedrine hydrochloride peak.
2. Preparation of control solutions
Taking appropriate amount of ephedrine hydrochloride reference substance and pseudoephedrine hydrochloride reference substance, precisely weighing, and adding water to obtain solutions each containing 10 μ g per 1mL to obtain mixed reference solution of ephedrine hydrochloride and pseudoephedrine hydrochloride.
3. Preparation of test solution
Precisely measuring 50mL of a pinellia ternate syrup sample to be tested (batch number: N07004S), putting the sample into a 500mL Kjeldahl flask with a frosted opening, adding 100mL of 30 wt% sodium hydroxide solution, connecting a distillation device, heating and distilling, collecting distillate to a near scale by using a 100mL measuring flask which is previously filled with 5mL of 0.1moL/L hydrochloric acid solution, cooling, adding water to the scale, shaking up, filtering, and taking a continuous filtrate to obtain a sample solution.
4. Preparation of negative control solution
Taking the medicinal materials except herba Ephedrae in the prescription composition, preparing herba Ephedrae negative control sample according to rhizoma Pinelliae syrup preparation process, and preparing according to the method under item "3" above to obtain negative control solution.
5. Selection of measurement wavelength and specificity test
Selection of measurement wavelength: the ultraviolet spectrum scanning is carried out on the ephedrine hydrochloride and pseudoephedrine hydrochloride reference solution, the result shows that the ephedrine hydrochloride and the pseudoephedrine hydrochloride have the maximum absorption at 205nm, the wavelength scanning of an ultraviolet spectrophotometer has an error range of +/-2 nm, meanwhile, the detection wavelength under the determination item of the content of the ephedra medicinal material of the Chinese pharmacopoeia 2005 edition is referred, and the Chinese pharmacopoeia rechecks the wavelengths of the ephedrine hydrochloride and the pseudoephedrine hydrochloride, so 207nm consistent with the Chinese pharmacopoeia is selected as the detection wavelength.
Precisely sucking 20 μ L of ephedrine hydrochloride reference solution, ephedrine hydrochloride and pseudoephedrine hydrochloride mixed reference solution, rhizoma Pinelliae syrup sample solution and herba Ephedrae negative reference solution respectively, and injecting into chromatograph, wherein the number of theoretical plates is 8366 calculated by ephedrine hydrochloride peak, and the number of theoretical plates is not less than 4000 according to the chromatographic condition of '1' considering different chromatographic columns. As shown in FIGS. 1-4, HPLC chromatogram results show that retention time of ephedrine hydrochloride reference and pseudoephedrine hydrochloride reference are substantially identical to corresponding peak of sample, separation degree is good, and herba Ephedrae negative control solution has no interference.
6. Investigation of linear relationships
Taking appropriate amount of ephedrine hydrochloride reference substance and pseudoephedrine hydrochloride reference substance, respectively, precisely weighing, and adding water to obtain ephedrine hydrochloride and pseudoephedrine hydrochloride mixed reference substance solution (ephedrine hydrochloride concentration: 41.84 μ g/mL; pseudoephedrine hydrochloride concentration: 43.08 μ g/mL). Absorbing the ephedrine hydrochloride and the hydrochloric acidThe pseudoephedrine mixed control solution was injected with 1. mu.L, 2. mu.L, 4. mu.L, 10. mu.L, 20. mu.L, 40. mu.L, respectively. Respectively taking the sample amount (mug) as an abscissa (x) and the peak area integral value as an ordinate (y), drawing a standard curve to obtain a linear equation of ephedrine hydrochloride: y 2.545 × 103x-0.3664, γ ═ 1.000; linear equation for pseudoephedrine hydrochloride: y is 2.561 × 103x-2.752, γ ═ 1.000; the result shows that the linear relation of ephedrine hydrochloride is good when the sample injection amount is 0.04184-1.674 mug, and the linear relation of pseudoephedrine hydrochloride is good when the sample injection amount is 0.04308-1.723 mug. The results are shown in Table 2.
TABLE 2 Linear and Linear Range
7. Stability test
The test solutions were prepared from pinellia ternate syrup (lot No. N07004S) by the method of item "3", and the peak area integrated values of the samples were measured by the method at 0, 2, 4, 8, 12, and 24 hours, respectively, and the measurement results are shown in table 3, where the average peak area of ephedrine hydrochloride is 753.469, RSD is 0.34% (N ═ 6), the average peak area of pseudoephedrine hydrochloride is 453.414, and RSD is 0.24% (N ═ 6). The test result shows that the test solution has stable measurement result within 24 hours.
TABLE 3 stability test results
8. Precision test
The sample solution prepared by the method of item "3" was subjected to sample injection for 6 times under the chromatographic conditions of the method of item "3", and the results are shown in table 4, where the average peak area of ephedrine hydrochloride is 753.809, RSD is 0.25%, the average peak area of pseudoephedrine hydrochloride is 452.661, and RSD is 0.36%, indicating that the accuracy is good.
TABLE 4 results of precision test
9. Repeatability test
The same batch of pinellia ternate syrup (batch number: N07004S) was taken, and the test solutions were prepared in parallel according to the preparation method of the test solution of item "3", and 6 parts in total were measured according to the method, and the results are shown in Table 5, showing that the method had good reproducibility.
TABLE 5 results of the repeatability tests
10. Accuracy (in sample recovery test recovery rate)
Taking pinellia ternate syrup (batch number: N07004S), precisely sucking 2.5mL of the product, weighing 6 parts in total, respectively placing the pinellia ternate syrup into a 500mL Kjeldahl flask with a frosted opening, precisely adding 3.6mL of ephedrine hydrochloride reference solution (C-0.2092 mg/mL) and 2.0mL of pseudoephedrine hydrochloride reference solution (C-0.2154 mg/mL), preparing test solution according to the preparation method of the test solution of item "3", respectively measuring the contents of ephedrine hydrochloride and pseudoephedrine hydrochloride, and calculating the sample recovery rate, wherein the average recovery rate is 100.8% of ephedrine hydrochloride (RSD-2.9%, N-6), and 99.09% of pseudoephedrine hydrochloride (RSD-1.5%, N-6), and the accuracy is good as shown in tables 6 and 7.
TABLE 6 ephedrine hydrochloride accuracy test results
TABLE 7 accuracy test results for pseudoephedrine hydrochloride
Fifthly, measuring the content of the sample
Taking 3 collected samples, preparing test solution according to the preparation method of the test solution of item 3 in parallel, and determining the content of ephedrine hydrochloride and pseudoephedrine hydrochloride according to the method. The results are shown in Table 8.
TABLE 8 measurement results of pinellia ternata syrup content
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A quality control method of pinellia ternate syrup is characterized by comprising the following steps:
preparation of a test solution: adding a pinellia ternate syrup sample to be tested into an aqueous solution of sodium hydroxide, distilling, collecting distillate by using an aqueous solution of hydrochloric acid, filtering, and taking a subsequent filtrate to prepare a sample solution;
preparation of control solutions: dissolving ephedrine hydrochloride and pseudoephedrine hydrochloride as reference substances in solvent to obtain reference substance solution;
injecting the test solution and the reference solution into a liquid chromatograph for determination;
the mobile phase of the liquid chromatograph is as follows: the volume ratio is 3.5-7: 93 to 96.5 acetonitrile-0.3 to 0.7 wt% phosphoric acid aqueous solution.
2. The quality control method according to claim 1, wherein the mobile phase is: the volume ratio is 5-6: 94 to 95 parts of acetonitrile-0.3 to 0.5 wt% of phosphoric acid aqueous solution.
3. The quality control method according to claim 1, wherein the aqueous sodium hydroxide solution has a mass concentration of 10% to 40%.
4. The quality control method according to claim 3, wherein the aqueous sodium hydroxide solution has a mass concentration of 25 to 40%.
5. The quality control method according to claim 1, wherein the chromatographic column of the liquid chromatograph is a DIAMOND ODS C18 column; the detector of the liquid chromatograph is a VWD detector.
6. The quality control method according to any one of claims 1 to 5, wherein the concentration of the aqueous hydrochloric acid solution is 0.05 to 0.5 mol/L; preferably, the concentration of the hydrochloric acid aqueous solution is 0.05-0.15 mol/L.
7. The quality control method according to any one of claims 1 to 5, wherein the size of the chromatographic column is: the length is 200 plus or minus 10mm multiplied by the diameter is 4.6 plus or minus 0.2mm, and the grain diameter is 5 plus or minus 0.2 mu m.
8. The quality control method according to any one of claims 1 to 5, wherein the chromatographic conditions of the liquid chromatograph include:
the detection wavelength is 207 +/-5 nm;
the sample volume is 20 +/-2 mu L;
the column temperature is 25 +/-2 ℃;
the flow rate is 1 plus or minus 0.2 ml/min;
the solvent is water.
9. The quality control method according to any one of claims 1 to 5, wherein in the preparation process of the sample solution, 1 to 3ml of sodium hydroxide aqueous solution is added to 1ml of the sample to be tested of the pinellia ternata syrup, and 1 to 3ml of distillate is collected by using 0.05 to 0.15ml of hydrochloric acid aqueous solution.
10. The quality control method according to any one of claims 1 to 5, wherein the effective components of the pinellia ternate syrup are prepared from raw materials comprising raw pinellia ternate, ephedra, aster, platycodon grandiflorum, polygala tenuifolia, loquat leaves, dried orange peel, licorice and peppermint oil.
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| CN114047272A (en) * | 2021-04-27 | 2022-02-15 | 合肥师范学院 | Method for evaluating quality of pinellia ternate and sparrow lawn pinellia ternate by using alkaloids |
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