CN110568109A - Method for screening radix peucedani feeding materials in lung ventilating and regulating preparation by adopting HPLC (high performance liquid chromatography) - Google Patents
Method for screening radix peucedani feeding materials in lung ventilating and regulating preparation by adopting HPLC (high performance liquid chromatography) Download PDFInfo
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Abstract
The invention relates to a method for screening the feeding of radix peucedani in a lung-ventilating and regulating preparation by adopting an HPLC method, which adopts a High Performance Liquid Chromatography (HPLC) method and takes a mixed control solution as a control, and can simultaneously determine the content of characteristic components of the radix peucedani and the purple-flowered peucedanum, thereby not only providing the technical support for screening whether the feeding of the radix peucedani is replaced by the purple-flowered peucedanum in the lung-ventilating and regulating preparation, but also improving the quality standard of the lung-ventilating and regulating preparation. The method is simple, convenient and quick to operate, greatly reduces the detection cost and time, improves the working efficiency, can more effectively, comprehensively and accurately control the quality of the lung ventilating and regulating preparation, and ensures the stability and uniformity of the product quality, thereby achieving the aim of ensuring the safety and effectiveness of product taking.
Description
Technical Field
The invention relates to a method for screening the material feeding of peucedanum praeruptorum in a preparation for ventilating and regulating the lung, belonging to the technical field of natural product detection.
Background
The peucedanum root has the functions of depressing qi and reducing phlegm, dispelling wind and clearing heat, and is clinically used for treating wind-heat cough, excessive phlegm, asthma, cough with yellow and thick sputum and the like. Has wide application in Chinese patent medicines for clearing lung-heat, relieving cough and reducing sputum, treating cold and the like and has large market demand. The whiteflower peucedanum and the purple peucedanum are used as certified peucedanum in the version of 2000 and before in the version of 2005, only the whiteflower peucedanum is used as certified peucedanum in the version of 2005, the purple peucedanum is deleted, and the purple peucedanum in the version of 2010 is listed as an independent variety. The specification of the "Chinese pharmacopoeia" 2015 year edition: radix Peucedani is dried root of radix Peucedani of Umbelliferae. Radix Peucedani is the dried root of Umbelliferae plant. Therefore, the loading condition of the peucedanum root in the Chinese pharmacopoeia of the calendar version is greatly changed. Secondly, the peucedanum praeruptorum dunn has higher requirements on soil texture, has higher growth altitude, is mostly wild, is not easy to cultivate and has less and less resources. The peucedanum praeruptorum has the advantages of low growth altitude, easy survival, easy cultivation and more resources. The characteristics of the radix peucedani and the purple flower radix peucedani are very similar to those of decoction pieces, and the differentiation is difficult for pharmaceutical suppliers or medicinal material suppliers. Based on the above reasons, the peucedanum praeruptorum dunn is easy to be mixed or substituted in the use process of Chinese patent medicine, and modern researches find that the main chemical components and pharmacological actions of the peucedanum praeruptorum dunn and the peucedanum praeruptorum dunn are greatly different.
The preparation for promoting the dispersing function of the lung has the effects of relieving exterior syndrome, dispelling cold, dispersing lung qi, relieving cough and the like. The traditional Chinese medicine composition is clinically used for treating cold and cough caused by wind-cold restraining the exterior and lung qi obstruction, and the symptoms of fever, aversion to cold, cough, nasal obstruction, nasal discharge, headache, anhidrosis and limb ache. The preparation is a national medical and nail-protection medicament and a national basic medicament, and has a large market share. The existing standard of the lung-ventilating and regulating preparation does not relate to a detection method of radix peucedani, the radix peucedani is a ministerial drug of the lung-ventilating and regulating preparation, and the quality of the preparation is influenced by the feeding problem of the radix peucedani. Therefore, in order to ensure the safe and effective medication of people, the establishment of the method for screening the peucedanum praeruptorum feeding in the lung ventilating and regulating preparation has important significance.
Disclosure of Invention
The invention aims to provide the method for effectively and accurately screening the fed material of the peucedanum praeruptorum in the lung ventilating and regulating preparation and simultaneously measuring the content of the characteristic components of the peucedanum praeruptorum, which has the advantages of simple and convenient operation and strong practicability, saves the detection cost and time.
The first invention aims to provide a method for screening the feeding of peucedanum praeruptorum in the lung ventilating and regulating pill by using an HPLC method, which comprises the following steps:
(1) Preparing a honeyed pill sample: weighing the product with different weights, cutting into pieces, mixing, weighing large honeyed pill about 4g (water honeyed pill about 1g), precisely weighing, placing in a conical flask with a stopper, precisely adding 50mL of methanol, sealing the stopper, weighing, ultrasonically treating (power 500W, frequency 40kHz) for 45min, cooling, weighing again, supplementing the weight loss with methanol, shaking, and filtering with filter paper to obtain filtrate A;
(2) And (3) purification: taking 5mL of the filtrate A, adding the filtrate A to a 100-200 mesh neutral alumina column (the specification of the column is 1.5cm in inner diameter), eluting with 100mL of methanol, collecting an effluent liquid and an eluent, evaporating to dryness, dissolving residues in methanol, transferring to a 5mL measuring flask, adding methanol to a constant volume to scale, shaking up, and passing through a 0.45 mu m microporous membrane to obtain a filtrate B;
(3) Detection conditions are as follows: taking 5 mu L of filtrate B, adopting Agilent ZorbaxSB-C18Column, detection wavelength: 321 nm; mobile phase: a phase is methanol, B phase is water, gradient elution is adopted, and the volume ratio of methanol to mobile phase is as follows: 35-35% for 0-14 min; 14-15min, 35% -59%; 15-44min, 59% -59%; 44-45min, 59% -75%; 45-55min, 75-75%; 55-56min, 75-95%; 56-60min, 95-95%, flow rate: 0.5-1.0 mL/min; column temperature: and calculating the contents of praeruptorin A, praeruptorin B and decursin in the test solution at 20-40 deg.C by one-point method.
the chromatographic column in the step (3) is Agilent ZorbaxSB-C18(150mm×4.6mm，5μm)。
the flow rate in the step (3) is 1.0 mL/min.
The column temperature in the step (3) is 35 ℃.
(4) And (4) screening result judgment standard: if decursin is detected in the chromatogram of the test sample, adding decursin, which may be the single or non-single type of decursin, into the preparation; if none of the three components in the test sample is detected, radix Peucedani and their congeneric plants are not added into the preparation; if only nodakenin is detected in the sample, only nodakenin is added into the preparation.
The second invention aims to provide a method for screening the dosing of the peucedanum root in other dosage forms for ventilating and regulating the lung by using an HPLC method, which comprises the following steps:
Preparing samples of other dosage forms for ventilating and regulating lung: taking 0.75g of lung-ventilating and regulating capsule (about 0.75g of tablet, about 1g of concentrated pill and about 2g of granule), grinding, precisely weighing, placing in a conical flask with a plug, precisely adding 50mL of methanol, sealing, weighing, ultrasonically treating (power 500W, frequency 40kHz) for 45min, cooling, weighing, supplementing the weight loss with methanol, shaking, and filtering with 0.45 μm microporous membrane to obtain filtrate I;
Detection: taking 5 mu L of filtrate I, adopting Agilent ZorbaxSB-C18column, detection wavelength: 321 nm; mobile phase: a phase is methanol, B phase is water, gradient elution is adopted, and the volume ratio of methanol to mobile phase is as follows: 35-35% for 0-14 min; 14-15min, 35% -59%; 15-44min, 59% -59%; 44-45min, 59% -75%; 45-55min, 75-75%; 55-56min, 75-95%; 56-60min, 95-95%, flow rate: 0.5-1.0 mL/min; column temperature: 20-40 ℃; calculating the contents of praeruptorin A, praeruptorin B and decursin in the test solution by using an external standard point method.
Thirdly, screening result judgment standard: if decursin is detected in the chromatogram of the test sample, adding decursin, which may be the single or non-single type of decursin, into the preparation; if none of the three components in the test sample is detected, radix Peucedani and their congeneric plants are not added into the preparation; if only nodakenin is detected in the sample, only nodakenin is added into the preparation.
the chromatographic column in the step II is Agilent ZorbaxSB-C18(150mm×4.6mm，5μm)。
the flow rate in the step II is 1.0 mL/min.
The temperature of the middle column is 35 ℃.
The technical effects are as follows:
1. The method established by the HPLC method can simultaneously detect the characteristic components of the peucedanum praeruptorum and the peucedanum purpurascens, and provides technical support for screening whether the peucedanum praeruptorum is used for replacing the peucedanum praeruptorum in the preparation for promoting the dispersing and regulating the lung. The method is simple, convenient and quick to operate, greatly reduces the detection cost and time, improves the working efficiency, can more effectively, comprehensively and accurately control the quality of the lung ventilating and regulating preparation, and ensures the stability and uniformity of the product quality, thereby achieving the aim of ensuring the safety and effectiveness of product taking.
2. The method can accurately determine the content of praeruptorin A and praeruptorin B in the lung-ventilating and regulating preparation, and the current quality standard of the lung-ventilating and regulating preparation has no control item of the praeruptorin. The invention improves the quality standard of the lung-ventilating and regulating preparation, further ensures the clinical curative effect of the lung-ventilating and regulating preparation, ensures the safe and effective administration of people, and provides a reference basis for the standard revision of the lung-ventilating and regulating preparation.
3. The invention is simultaneously suitable for various dosage forms for ventilating and regulating lung, including big honeyed pills, water-honeyed pills, concentrated pills, tablets, granules, oral liquid and capsules.
4. the lung-ventilating and regulating preparation is a national medical and health-care medicament and a national basic medicament, the method established by the invention effectively solves the problem of screening and feeding the peucedanum root, can effectively control the quality of the peucedanum root, ensures the stability and consistency of the product quality, has good application prospect and use value, and has important significance for market expansion, clinical application and the international process of the lung-ventilating and regulating preparation.
Description of the drawings:
FIG. 1 is a superimposed HPLC chromatogram of lung ventilating and regulating pill sample, negative and mixed control solution;
FIG. 2 is a superimposed HPLC chromatogram of lung ventilating and regulating sample, negative and mixed control solution;
FIG. 3 is a superimposed HPLC chromatogram of lung ventilating and regulating particle sample, negative and mixed control solution;
FIG. 4 is a superimposed HPLC chromatogram of lung ventilating and regulating capsule sample, negative and mixed control solution;
FIG. 5 is a superimposed HPLC chromatogram of the lung ventilating and regulating concentrated pill sample, the negative and the mixed control solution;
In the above fig. 1 to 5, 1 is nodakenin, 2 is praeruptorin A, and 3 is praeruptorin B.
Detailed Description
The invention is further illustrated by the following specific examples, which are intended to be illustrative of the invention and are not intended to be a further limitation of the invention.
The first embodiment is as follows: establishment of detection method
1. Instruments, reagents and materials
The instrument comprises the following steps: waters2695e high performance liquid chromatograph, chromatography workstation data processing system; sartorius model BP 211D electronic analytical balance; ultra pure water system (MILLIPORE); ultrasonic cleaning instrument (power 500W, frequency 40 kHz).
Reagent: the methanol is chromatographically pure (Fisher Scientific company, USA); methanol is analytically pure (chemical reagents of national drug group, Inc.); the water is ultrapure water; neutral alumina was used for chromatography (Dow Corona Chemicals Co., Ltd.).
Materials: decursin control (batch No. 111821-201604, purity: 99.6%, for content determination), praeruptorin A (batch No. 111711-201703 for content determination), and praeruptorin B (batch No. 111904-201804, 98.9% for content determination), all of which were purchased from China food and drug testing institute.
2. Chromatographic conditions
A chromatographic column: agilent ZorbaxSB-C18(150 mm. times.4.6 mm, 5 μm); detection wavelength: 321 nm; mobile phase: a phase is methanol, B phase is water, gradient elution is adopted, and the volume ratio of methanol to mobile phase is as follows: 35-35% for 0-14 min; 14-15min, 35% -59%; 15-44min, 59% -59%; 44-45min, 59% -75%; 45-55min, 75-75%; 55-56min, 75-95%; 56-60min, 95-95%. Flow rate: 1.0 mL/min; column temperature: 35 ℃;
3. Preparation of solutions
3.1 preparation of mixed control solutions: accurately weighing appropriate amount of decursin, praeruptorin A and praeruptorin B reference substances, adding methanol solution to obtain mixed solution containing decursin 40 μ g, praeruptorin A10 μ g and praeruptorin B10 μ g per mL, and shaking up;
3.2 preparation of test solution:
The preparation method of the test solution of the lung-ventilating and regulating pill comprises the following steps: taking the product with different weights, shearing, mixing uniformly, taking about 4g of big honeyed pills (about 1g of water honeyed pills), precisely weighing, placing in a conical flask with a plug, precisely adding 50mL of methanol, sealing the plug, weighing, carrying out ultrasonic treatment (power 500W and frequency 40kHz) for 45min, cooling, weighing again, supplementing the lost weight with methanol, shaking up, filtering, precisely weighing 5mL of subsequent filtrate, adding on a neutral alumina column (100-200 meshes, 5g and inner diameter of 1.5cm), eluting with 100mL of methanol, collecting effluent and eluent, evaporating to dryness, dissolving the residue with methanol, transferring to a 5mL measuring flask, adding methanol to fix the volume to scale, and shaking up to obtain the product.
The preparation method of the test solution with other preparation forms comprises the following steps: taking the product with different weights, grinding, taking about 0.75g of lung-ventilating and regulating capsule (about 0.75g of tablet, about 1g of concentrated pill and about 2g of granule), precisely weighing, placing into a conical flask with a plug, precisely adding 50mL of methanol, sealing, weighing, ultrasonically treating (power 500W, frequency 40kHz) for 45min, cooling, weighing again, supplementing the lost weight with methanol, and shaking uniformly to obtain the final product.
Preparation of negative sample solution: preparing into radix Peucedani-deficient negative sample according to the preparation process of the preparation for promoting the dispersing function of the lung, and preparing into radix Peucedani-deficient negative sample solution according to the preparation process of the test solution.
4. Experiment of system applicability
taking 5 μ l of the mixed control solution, the test solution and the radix Peucedani negative sample solution prepared in "3" respectively, performing sample injection measurement under the above chromatographic conditions, and recording HPLC chromatogram, as shown in FIGS. 1-5. The separation degree of each component chromatographic peak is more than 1.5, the negative effect is not interfered, and the theoretical plate number is not less than 4000 based on the praeruptorin A peak.
5. Methodology investigation
5.1 Linear relationship examination test 1, 5, 10, 18 and 20. mu.l of each of the mixed control solutions prepared in "3.1" were precisely aspirated, and the solutions were injected into a liquid chromatograph and measured under the chromatographic conditions described in "2" above. And recording corresponding peak areas, taking the peak area Y as a vertical coordinate, taking the sample injection amount (ng) as a horizontal coordinate, drawing a standard curve and performing linear regression. The regression equation and linear range for the 3 components are shown in table 1. The results show that the concentrations of decursin, praeruptorin A and praeruptorin B solutions all have good linear relation with peak areas.
TABLE 1 Linear regression equation and linear range of 3 index components in TONGXUANLIFEI pill
5.2 precision test the lung-ventilating and regulating pill is cut into pieces, precisely weighed, a test solution is prepared according to the 3.2, the determination is carried out according to the chromatographic condition in the 2, the sample introduction is carried out for 6 times, the chromatographic peak areas of 3 compounds of decursin, praeruptorin A and praeruptorin B are recorded, and the RSD (%) value is calculated, and the result is shown in the table 2. The results show that the chromatographic peak areas RSD of the 3 compounds are less than 2%, and the instrument precision is good.
TABLE 2 results of precision test
5.3 stability test the 5.2 test sample solution is placed in a closed container, the sample is sampled and detected according to the 2 chromatographic conditions at room temperature for 0, 1, 2, 4, 8 and 16h, the chromatographic peak areas of 3 compounds of decursin, praeruptorin A and praeruptorin B are recorded, and the RSD (%) value is calculated, and the result is shown in Table 3. The result shows that the chromatographic peak areas RSD of the 3 compounds are less than 2% after the test solution is placed for 16h, and the test solution is stable within 16h at room temperature.
TABLE 3 stability test results
5.4 repeatability test the same lot of lung-regulating pills are cut into pieces, 6 parts of lung-regulating pills are taken, 4g of each part is precisely weighed, a test solution is prepared according to 3.2, the determination is carried out according to the chromatographic conditions in 2, the chromatographic peak areas of 3 compounds of decursin, praeruptorin A and praeruptorin B are recorded, the content of 3 compounds is calculated, the RSD (%) value is calculated, and the result is shown in Table 4. The results show that the RSD content of the 3 compounds is less than 3 percent, and the method has good reproducibility.
TABLE 4 results of the repeatability tests
5.5 sample adding recovery test A lot of lung regulating pills are cut into pieces, 6 parts of lung regulating pills are taken, 2g of each part is precisely weighed, a decursin reference substance, a whiteflower peucedanum element A reference substance and a whiteflower peucedanum element B reference substance are precisely added, a sample solution is prepared according to the condition of 3.2, and the determination is carried out according to the chromatographic condition in 2. The chromatographic peak areas of 3 compounds of decursin, praeruptorin A and praeruptorin B are recorded, and the sample recovery rate and RSD (%) of each compound are calculated, and the results are shown in Table 5. The result shows that the recovery rate of the 3 compounds is between 95 and 105 percent, the RSD is less than 3 percent, and the accuracy of the invention is good.
TABLE 5 sample recovery test results
EXAMPLE two detection of Lung ventilating and regulating pill sample
1. The preparation and chromatographic conditions of the mixed reference solution are the same as above.
2. The preparation of the sample is the same as above, taking the lung ventilating and regulating pill with the batch number of 20180512.
3. And (3) HPLC determination: respectively and precisely sucking 5 μ l of the mixed reference solution and the test solution, injecting into a high performance liquid chromatograph, measuring, and calculating the content by an external standard method according to the peak areas of decursin, praeruptorin A and praeruptorin B, wherein the content of decursin, praeruptorin A and praeruptorin B is 0.133mg/g, 0.324mg/g and 0.128mg/g respectively. The HPLC chromatogram map detects three characteristic components at the same time, which indicates that the batch of the pill for ventilating and regulating lung is added with the purple peucedanum root, which can be a single material or a non-single material.
EXAMPLE III Lung-ventilating-regulating tablet sample testing
1. The preparation and chromatographic conditions of the mixed reference solution are the same as above.
2. The preparation of the lung-ventilating and regulating tablet with the batch number of 181001 is the same as above.
3. And (3) HPLC determination: respectively and precisely sucking 5 μ l of the mixed reference solution and the test solution, injecting into a high performance liquid chromatograph, measuring, detecting, and calculating the content by external standard method according to the peak areas of decursin and praeruptorin A, wherein the content of decursin and praeruptorin A is 0.321mg/g and 0.108mg/g respectively. Because the HPLC chromatogram detects the decursin and the praeruptorin A, the batch of the tablets for ventilating and regulating lung is added with the decursin, which can be a single feed or a non-single feed.
EXAMPLE four detection of Lung-ventilating-regulating granule sample
1. the preparation and chromatographic conditions of the mixed reference solution are the same as above.
2. the lung ventilating and regulating particles with the batch number of 190311 are taken, and the sample preparation is the same as the above.
3. and (3) HPLC determination: precisely sucking 5 μ l of the mixed reference solution and the test solution respectively, injecting into a high performance liquid chromatograph, and determining that decursin, praeruptorin A and praeruptorin B are not detected, which indicates that no peucedanum root, decursium japonicum and congeneric plant are added in the granules for ventilating and regulating lung.
Example five detection of Lung-ventilating and regulating Capsule sample
1. The preparation and chromatographic conditions of the mixed reference solution are the same as above.
2. the preparation of the sample is the same as above, taking the lung ventilating and regulating capsule with the batch number of 19310011.
3. And (3) HPLC determination: respectively and precisely sucking 5 μ l of the mixed reference solution and the test solution, injecting into a high performance liquid chromatograph, measuring, and calculating the content of decursin to be 0.583mg/g by adopting an external standard method according to the peak area of decursin without detecting decursin A and decursin B. Only decursin is detected by HPLC chromatogram, which indicates that the batch of capsules for ventilating, ventilating and regulating lung uses decursin instead of decursin.
EXAMPLE VI, lung ventilating and regulating concentrated pill sample testing
1. The preparation and chromatographic conditions of the mixed reference solution are the same as above.
2. The preparation method of the lung-ventilating and regulating concentrated pill with the batch number of 1903004 is the same as that of the sample preparation.
3. And (3) HPLC determination: respectively and precisely sucking 5 μ l of the mixed reference solution and the test solution, injecting into a high performance liquid chromatograph, measuring, detecting, and calculating the content by external standard method according to the peak areas of decursin and praeruptorin A, wherein the content of decursin and praeruptorin A is 0.13mg/g and 0.175mg/g respectively. Because the HPLC chromatogram detects the decursin and the praeruptorin A, the batch of the praeruptorin concentrated pills for ventilating and regulating the lung is added with the decursin, which can be a single feed or a non-single feed.
Claims (8)
1. A method for screening the material of peucedanum praeruptorum in the lung ventilating and regulating pill by adopting an HPLC method comprises the following steps:
(1) Preparing a honeyed pill sample: weighing the product with different weights, cutting into pieces, mixing, weighing large honeyed pill about 4g (water honeyed pill about 1g), precisely weighing, placing in a conical flask with a stopper, precisely adding 50mL of methanol, sealing the stopper, weighing, ultrasonically treating (power 500W, frequency 40kHz) for 45min, cooling, weighing again, supplementing the weight loss with methanol, shaking, and filtering with filter paper to obtain filtrate A;
(2) And (3) purification: taking 5mL of filtrate A, adding the filtrate A to a 100-200 mesh neutral alumina column, eluting with 100mL of methanol, collecting effluent liquid and eluent, evaporating to dryness, dissolving residues with methanol, transferring to a 5mL measuring flask, adding methanol to a constant volume to a scale, shaking up, and passing through a 0.45-micrometer microporous filter membrane to obtain filtrate B;
(3) Detection conditions are as follows: taking 5 mu L of filtrate B, adopting Agilent ZorbaxSB-C18Column, detection wavelength: 321 nm; mobile phase: a phase is methanol, B phase is water, gradient elution is adopted, and the volume ratio of methanol to mobile phase is as follows: 35-35% for 0-14 min; 14-15min, 35% -59%; 15-44min, 59% -59%; 44-45min, 59% -75%; 45-55min, 75-75%; 55-56min, 75-95%; 56-60min, 95-95%, flow rate: 0.5-1.0 mL/min; column temperature: and calculating the contents of praeruptorin A, praeruptorin B and decursin in the test solution at 20-40 deg.C by one-point method.
(4) And (4) screening result judgment standard: if decursin is detected in the chromatogram of the test sample, adding decursin, which may be the single or non-single type of decursin, into the preparation; if none of the three components in the test sample is detected, radix Peucedani and their congeneric plants are not added into the preparation; if only nodakenin is detected in the sample, only nodakenin is added into the preparation.
2. the method according to claim 1, wherein the chromatographic column in step (3) is Agilent ZorbaxSB-C18(150mm×4.6mm，5μm)。
3. The method according to claim 1, wherein the flow rate in the step (3) is 1.0 mL/min.
4. The method according to claim 1, wherein the column temperature in said step (3) is 35 ℃.
5. The method of claim 1, wherein the method of screening for a dosage of peucedanum praeruptorum in other lung ventilating dosage forms comprises the steps of:
preparing samples of other dosage forms for ventilating and regulating lung: taking 0.75g of lung-ventilating and regulating capsule (about 0.75g of tablet, about 1g of concentrated pill and about 2g of granule), grinding, precisely weighing, placing in a conical flask with a plug, precisely adding 50mL of methanol, sealing, weighing, ultrasonically treating (power 500W, frequency 40kHz) for 45min, cooling, weighing, supplementing the weight loss with methanol, shaking, and filtering with 0.45 μm microporous membrane to obtain filtrate I;
detection: taking 5 mu L of filtrate I, adopting Agilent ZorbaxSB-C18Column, detection wavelength: 321 nm; mobile phase: a phase is methanol, B phase is water, gradient elution is adopted, and the volume ratio of methanol to mobile phase is as follows: 35-35% for 0-14 min; 14-15min, 35% -59%; 15-44min, 59% -59%; 44-45min, 59% -75%; 45-55min, 75-75%; 55-56min, 75-95%; 56-60min, 95-95%, flow rate: 0.5-1.0 mL/min; column temperature: 20-40 ℃; calculating the contents of praeruptorin A, praeruptorin B and decursin in the test solution by using an external standard point method.
thirdly, screening result judgment standard: if decursin is detected in the chromatogram of the test sample, adding decursin, which may be the single or non-single type of decursin, into the preparation; if none of the three components in the test sample is detected, radix Peucedani and their congeneric plants are not added into the preparation; if only nodakenin is detected in the sample, only nodakenin is added into the preparation.
6. The method of claim 5, wherein the chromatographic column is Agilent ZorbaxSB-C18(150mm×4.6mm，5μm)。
7. The method of claim 5, wherein the flow rate in step (c) is 1.0 mL/min.
8. The process of claim 5 wherein the column temperature is 35 ℃.
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| CN114689730A (en) * | 2020-12-31 | 2022-07-01 | 鲁南制药集团股份有限公司 | Method for detecting coumarin components in Jingfang granules |
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Application publication date: 20191213 |