CN107505418B - Construction method of HPLC fingerprint of lung-tonifying and blood-activating capsule and standard fingerprint - Google Patents
Construction method of HPLC fingerprint of lung-tonifying and blood-activating capsule and standard fingerprint Download PDFInfo
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- CN107505418B CN107505418B CN201710516710.3A CN201710516710A CN107505418B CN 107505418 B CN107505418 B CN 107505418B CN 201710516710 A CN201710516710 A CN 201710516710A CN 107505418 B CN107505418 B CN 107505418B
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention relates to a method for constructing a lung-tonifying and blood-activating capsule HPLC fingerprint and a standard fingerprint thereof. The method comprises precisely preparing 50% methanol solution of capsule content for invigorating lung and promoting blood circulation as test solution and mixed solution of calycosin glucoside, calycosin, paeoniflorin, isopsoralen and psoralen with concentration of 50 μ g/ml respectively as reference solution; obtaining the HPLC fingerprint of the lung-tonifying and blood-activating capsule under the specific chromatographic condition. The standard fingerprint spectrum containing 12 common chromatographic peaks is obtained by finding out common characteristic peaks of HPLC fingerprint spectra constructed by more than 10 batches of lung tonifying and blood circulation invigorating capsule samples and analyzing and comparing the fingerprint spectra. The method can monitor the quality of the finished product; provides scientific basis for the standardized research of the lung tonifying and blood circulation invigorating capsule.
Description
Technical Field
The invention relates to a method for constructing a lung-tonifying and blood-activating capsule HPLC fingerprint and a standard fingerprint thereof.
Background
The lung tonifying and blood circulation invigorating capsule is recorded in the first part of the 2015 edition of Chinese pharmacopoeia and is prepared from three medicaments of astragalus, red paeony root and fructus psoraleae. The theory of traditional Chinese medicine holds that astragalus mongholicus has the effects of tonifying qi, red paeony root has the effect of removing blood stasis, and fructus psoraleae has the effects of absorbing qi and relieving asthma. The three medicines have the effects of benefiting qi, activating blood circulation, tonifying lung and reinforcing kidney, and are used for treating pulmonary heart disease (in remission stage) belonging to qi deficiency and blood stasis syndrome with symptoms of cough and shortness of breath, or cough, asthma, chest distress, palpitation, short breath, cold limbs, hypodynamia, soreness and weakness of waist and knees, cyanosis of lips, pale tongue with white fur, dark purple tongue and the like. The invention provides a method for constructing an HPLC fingerprint of a lung-tonifying and blood-activating capsule, which can monitor the quality of the lung-tonifying and blood-activating capsule through a standard fingerprint of the lung-tonifying and blood-activating capsule so as to ensure the uniformity of a finished product.
Disclosure of Invention
The invention provides a method for constructing an HPLC fingerprint of a lung-tonifying and blood-activating capsule. The method can monitor the quality of the finished product; provides scientific basis for the standardized research of the lung tonifying and blood circulation invigorating capsule.
The invention relates to a method for constructing HPLC (high performance liquid chromatography) fingerprint spectrum of a lung tonifying and blood circulation activating capsule, which comprises the following steps:
(1) preparation of a test solution: taking the content of the product, grinding, taking about 1.2g, precisely weighing, placing in a conical flask with a plug, precisely adding 50ml of methanol, weighing, heating and refluxing for 1 hour, cooling, weighing again, supplementing the lost weight with methanol, shaking up, filtering, precisely weighing 25ml of subsequent filtrate, recovering solvent to dryness, dissolving the residue with 50% of methanol, quantitatively transferring to a 5ml measuring flask, adding 50% of methanol to scale, and shaking up to obtain the product.
(2) Preparation of control solutions: respectively weighing appropriate amount of calycosin glucoside, calycosin, penoniflorin, isopsoralen, and psoralen reference substances, and making into mixed solution with concentration of 50 μ g/ml each.
(3) Analyzing the test solution and the reference solution by adopting a high performance liquid chromatography to obtain the high performance liquid chromatography fingerprint of the lung tonifying and blood circulation invigorating capsule, wherein the chromatographic conditions are as follows: the sample amount is 10 mul; the chromatographic column is Hitachihigh-Tech C18 (4.6X 250mm, 5 μm); performing gradient elution by using acetonitrile as a mobile phase A and 0.2% formic acid solution as a mobile phase B for 0-25min, 16% of A, 84% of B, 25-65min, 16-42% of A and 84-58% of B; the column temperature is 25 ℃; the detection wavelength is 260 nm.
Mass spectrum working parameters: ion spray voltage 1500V; spray air pressure 50 psi; auxiliary heating air pressure 60 psi; the temperature is 550 ℃; air curtain pressure 15 psi; the collision air pressure is 8 psi; inlet voltage 10V; and an electrospray ion source and a positive ion mode are adopted for detection.
The standard fingerprint of the lung tonifying and blood circulation promoting capsule is obtained by analyzing and comparing the HPLC fingerprints constructed by 10 batches of the lung tonifying and blood circulation promoting capsules and finding out common characteristic peaks of the fingerprints.
12 common chromatographic peaks are detected by the standard fingerprint of the lung-tonifying and blood-activating capsule, the common peaks belonging to astragalus are No. 4 peak, No. 8 peak and No. 10 peak, the common peaks belonging to red peony root are No. 2 peak, No. 5 peak, No. 6 peak and No. 7 peak, and the common peaks belonging to fructus psoraleae are No. 1 peak, No. 3 peak, No. 9 peak, No. 11 peak and No. 12 peak. Performing chromatographic peak attribution and peak purity detection on a main peak by using a DAD detector and an ultrafast liquid chromatography-quadrupole tandem time-of-flight mass spectrometry (UFLC-TRIPLE TOF-DAD-MS/MS) technical means, and identifying molecular ion peaks and cracking fragment information of a mass spectrum by comparing UV absorption curves: the No. 1 peak is psoralen glycoside, the No. 2 peak is paeoniflorin, the No. 3 peak is isobavalin, the No. 4 peak is calycosin glucoside, the No. 5 peak is galloyl paeoniflorin, the No. 6 peak is 1,2,3,4, 6-pentagalloyl glucose, the No. 10 peak is calycosin, the No. 11 peak is psoralen essence, and the No. 12 peak is isobavalin. The graph of the map is the map shown in figure 1 in the attached drawings of the specification. The relative retention values of a common peak in the fingerprint chart of the capsule for tonifying lung and activating blood are listed as follows by taking No. 4 peak calycosin glucoside as a reference peak:
drawings
FIG. 1 is a standard fingerprint of the lung tonifying and blood circulation promoting capsule of the present invention.
FIG. 2 is a chromatogram corresponding to standard fingerprint of the capsule for tonifying lung and promoting blood circulation, wherein the peak numbers 2, 4, 10, 11, and 12 are paeoniflorin, calycosin glucoside, calycosin, psoralen, and isopsoralen.
FIG. 3 is a negative control chromatogram of BUFEIHUOXUE Capsule, radix astragali, and radix astragali deficiency, in which the arrow from left to right indicates the peak number of chromatographic peak belonging to radix astragali in standard fingerprint of BUFEIHUOXUE Capsule.
FIG. 4 is a negative control chromatogram of BUFEIHUOXUE Capsule, radix Paeoniae Rubra, and radix Paeoniae Rubra, in which the arrow from left to right indicates the peak number of the chromatographic peak belonging to radix Paeoniae Rubra in the standard fingerprint of BUFEIHUOXUE Capsule.
FIG. 5 is a chromatogram of comparison of Bufeihuxiaoxue capsule and Buguzhi medicinal material, wherein the arrow in the chromatogram indicates the peak number of the chromatographic peak belonging to Buguzhi in the standard fingerprint of Bufeihuxiaoxue capsule.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
Example 1
1 Instrument and reagent
1.1 Instrument: ultra-fast high performance liquid chromatography (LC-20AD-XR binary pump, SIL-20AD-XR autosampler, CTO-20A column oven, SPD-M10A-PDA detector) of SHIMADUD Dionexultimate 3000 DGLC high performance liquid chromatograph (DGP-3600SD double ternary pump, SRD-3600 degasser, WPS-3000SL autosampler, TCC3000-RS column oven, DAD detector); a chromatographic column: hitachi High-Tech C18 (4.6X 250mm, 5 μm).
1.2 reagent: 10 batches of finished product, all provided by Guangdong Leyun pharmaceutical Co. In the experiment, acetonitrile and formic acid used as reagents for liquid chromatography are chromatographically pure, the rest of the reagents are analytically pure, and water is ultrapure water.
Comparison products: psoralen (manufacturer: China institute for testing biological products of drugs, lot number: 110739-201416); isopsoralen (manufacturer: China institute for testing biological products of drugs, batch No. 110738-2013); paeoniflorin (manufacturer: China pharmaceutical biological products institute, batch No. 110736-201539); calycosin glucoside (manufacturer: China pharmaceutical biologicals institute, lot number: 111920-201505); calycosin (manufacturer: Dopperphy Biotechnology Co., Ltd., batch No. 151208).
2. Method and results
2.1 construction method of HPLC fingerprint of lung-tonifying and blood-activating capsule
2.1.1 preparation of the solution
Preparation of a test solution: taking the content of the product, grinding, taking about 1.2g, precisely weighing, placing in a conical flask with a plug, precisely adding 50ml of methanol, weighing, heating and refluxing for 1 hour, cooling, weighing again, supplementing the lost weight with methanol, shaking up, filtering, precisely weighing 25ml of subsequent filtrate, recovering solvent to dryness, dissolving the residue with 50% of methanol, quantitatively transferring to a 5ml measuring flask, adding 50% of methanol to scale, and shaking up to obtain the product.
Preparation of mixed control solution: respectively weighing appropriate amount of calycosin glucoside, calycosin, penoniflorin, isopsoralen, and psoralen reference substances, and making into mixed solution with concentration of 50 μ g/ml each.
Preparing a medicinal material test solution: taking decoction pieces of each medicinal material, and preparing the decoction pieces according to the method under the item of preparation of the test solution.
2.1.2 high performance liquid chromatography analysis: precisely sucking 10 mul of test solution, and injecting; chromatographic conditions are as follows: the chromatographic column is Hitachi High-Tech C18 (4.6X 250mm, 5 μm); the mobile phase is acetonitrile as a mobile phase A, 0.2% formic acid solution as a mobile phase B, and the following gradient elution mode is adopted:
the detection wavelength is 260 nm; flow rate: 0.8 ml/min; column temperature: 25 ℃; obtaining the high performance liquid chromatography standard fingerprint of the lung tonifying and blood circulation invigorating capsule.
2.1.3 consensus peak determination: comparing the obtained high performance liquid chromatography fingerprints of 10 batches of lung tonifying and blood circulation invigorating capsules by a traditional Chinese medicine chromatography fingerprint similarity evaluation system (2012 edition), determining 12 common characteristic peaks and obtaining a common mode (referring to fingerprints). The obtained chromatogram shows that the common peaks ascribed to radix astragali are No. 4, No. 8 and No. 10, the common peaks ascribed to radix Paeoniae Rubra are No. 2, No. 5, No. 6 and No. 7, and the common peaks ascribed to fructus Psoraleae are No. 1, No. 3, No. 9, No. 11 and No. 12. Performing chromatographic peak attribution and peak purity detection on a main peak by using a DAD detector and an ultrafast liquid chromatography-quadrupole tandem time-of-flight mass spectrometry (UFLC-TRIPLE TOF-DAD-MS/MS) technical means, and identifying molecular ion peaks and cracking fragment information of a mass spectrum by comparing UV absorption curves: the No. 1 peak is psoralen glycoside, the No. 2 peak is paeoniflorin, the No. 3 peak is isobavalin, the No. 4 peak is calycosin glucoside, the No. 5 peak is galloyl paeoniflorin, the No. 6 peak is 1,2,3,4, 6-pentagalloyl glucose, the No. 10 peak is hairy ruidaidzein, the No. 11 peak is psoralen, and the No. 12 peak is isobavalin. The chromatographic peaks form the fingerprint characteristics of the lung-tonifying and blood circulation-activating capsule.
2.1.4 precision test: the same lung tonifying and blood circulation promoting capsule sample solution is continuously injected for 6 times, the fingerprint is detected, evaluation is carried out by a traditional Chinese medicine chromatogram fingerprint similarity evaluation system (2012 edition), the similarity is more than 0.99, and the result shows that the precision of the instrument is good.
The similarity results are as follows:
2.1.5 stability study: sampling a test solution of the same lung-tonifying and blood-activating capsule respectively at 0 hour, 2 hours, 4 hours, 8 hours, 10 hours, 24 hours and 48 hours, detecting a fingerprint, evaluating by adopting a traditional Chinese medicine chromatogram fingerprint similarity evaluation system (2012 edition), wherein the similarity is more than 0.99, and the result shows that the test solution is stable in 48 hours. The similarity results are as follows:
2.1.6 repeatability tests: 6 parts of the same batch of capsules for tonifying lung and activating blood are taken, the operation is carried out according to the method under the preparation item of the test solution, the samples are respectively injected, the fingerprints are detected, the evaluation is carried out by adopting a traditional Chinese medicine chromatogram fingerprint similarity evaluation system (2012 edition), the similarity is more than 0.99, and the result shows that the method has good repeatability.
The similarity results are as follows:
| S1 | S2 | S3 | S4 | S5 | S6 | comparison fingerprint | |
| S1 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 0.999 | 1.000 |
| S2 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
| S3 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 0.999 | 1.000 |
| S4 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 0.999 | 1.000 |
| S5 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
| S6 | 0.999 | 1.000 | 0.999 | 0.999 | 1.000 | 1.000 | 1.000 |
| Comparison fingerprint | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
2.1.7 intermediate precision: the lung-tonifying and blood-activating capsules of the same batch are taken, are measured according to the law under the condition of variable factors such as different dates, different analysts, different instruments and the like, the fingerprint is detected, and a traditional Chinese medicine chromatogram fingerprint similarity evaluation system (2012 edition) is adopted for evaluation. The result shows that the method has good intermediate precision, and the HPLC fingerprint quality control method of the capsule for tonifying lung and activating blood is feasible.
(1) Different analysis times: the lung tonifying and blood circulation invigorating capsules of the same batch are taken, operated according to the method under the item of preparation of test solution on different dates, and evaluated by a traditional Chinese medicine chromatographic fingerprint similarity evaluation system (2012 edition), wherein the similarity is more than 0.99. The similarity results are as follows:
| analysis time 1 | Analysis time 2 | Comparison fingerprint | |
| Analysis time 1 | 1.000 | 0.994 | 0.999 |
| Analysis time 2 | 0.994 | 1.000 | 0.998 |
| Comparison fingerprint | 0.999 | 0.998 | 1.000 |
(2) Different analysts: the lung tonifying and blood circulation invigorating capsules of the same batch are taken, different people respectively operate according to the method under the item of preparation of test solution, and a traditional Chinese medicine chromatographic fingerprint similarity evaluation system (2012 edition) is adopted for evaluation, wherein the similarity is more than 0.99. The similarity results are as follows:
| analysts 1 | Analysts 2 | Comparison fingerprint | |
| Analysts 1 | 1.000 | 1.000 | 1.000 |
| Analysts 2 | 1.000 | 1.000 | 1.000 |
| Comparison fingerprint | 1.000 | 1.000 | 1.000 |
(3) Different instruments: taking one part of the lung tonifying and blood circulation promoting capsules of the same batch, operating according to the method under the item of preparation of test solution, respectively measuring in different instruments according to the method, and evaluating by adopting a traditional Chinese medicine chromatographic fingerprint similarity evaluation system (2012 edition), wherein the similarity is more than 0.99. The similarity results are as follows:
| analytical instrument 1 | Analytical instrument 2 | Comparison fingerprint | |
| Analytical instrument 1 | 1.000 | 1.000 | 1.000 |
| Analytical instrument 2 | 1.000 | 1.000 | 1.000 |
| Comparison fingerprint | 1.000 | 1.000 | 1.000 |
Claims (3)
1. A method for constructing an HPLC fingerprint of a lung-tonifying and blood-activating capsule is characterized by comprising the following steps:
(1) preparation of a test solution: precisely weighing 1.2g of capsule contents for tonifying lung and activating blood, precisely adding 50ml of methanol, heating and refluxing for 1 hour, cooling, complementing weight loss reduction amount with methanol, filtering, precisely taking 25ml of subsequent filtrate, recovering solvent until the solvent is dry, dissolving residues with 50% of methanol, quantitatively transferring to a 5ml measuring flask, and adding 50% of methanol to scale to obtain a sample solution;
(2) preparation of control solutions: respectively weighing appropriate amount of calycosin glucoside, calycosin, penoniflorin, isopsoralen, and psoralen reference substances, and making into mixed solution with concentration of 50 μ g/ml;
(3) analyzing the test solution and the reference solution by adopting a high performance liquid chromatography to obtain the high performance liquid chromatography fingerprint of the lung tonifying and blood circulation invigorating capsule, wherein the chromatographic conditions are as follows: the chromatographic column is Hitachi high and new technology C18; acetonitrile is taken as a mobile phase A, and 0.2% formic acid solution is taken as a mobile phase B; gradient elution, 0-25min, 16% A, 84% B; 25-65min, 16-42% of A and 84-58% of B; the column temperature is 25 ℃; the detection wavelength is 260nm, and the sample injection amount is 10 mu l;
mass spectrum working parameters: ion spray voltage 1500V; spray air pressure 50 psi; auxiliary heating air pressure 60 psi; the temperature is 550 ℃; air curtain pressure 15 psi; the collision air pressure is 8 psi; inlet voltage 10V; and an electrospray ion source and a positive ion mode are adopted for detection.
2. An HPLC standard fingerprint of a capsule for tonifying lung and activating blood is characterized in that: the method of claim 1, wherein the common characteristic peaks of 10 or more samples of the lung-tonifying and blood-activating capsules are determined by analyzing and comparing HPLC fingerprints, and 12 common chromatographic peaks are determined, wherein the common peaks include peaks 4, 8 and 10 derived from Astragalus membranaceus, peaks 2, 5, 6 and 7 derived from radix Paeoniae Rubra, and the common peaks include peaks 1, 3, 9, 11 and 12 derived from Psoralea corylifolia.
3. An HPLC standard fingerprint of a capsule for tonifying lung and activating blood is characterized in that: the construction method of claim 1, wherein HPLC finger prints constructed by more than 10 batches of lung-tonifying and blood-activating capsules are analyzed and compared, chromatographic peak attribution and peak purity detection are carried out on main peaks by using a DAD detector and an ultrafast liquid chromatography-quadrupole tandem time-of-flight mass spectrometry combined technical means, and molecular ion peaks and cracking fragment information identification of mass spectra are combined by UV absorption curve comparison: the No. 1 peak is psoralen glycoside, the No. 2 peak is paeoniflorin, the No. 3 peak is isobavalin, the No. 4 peak is calycosin glucoside, the No. 5 peak is galloyl paeoniflorin, the No. 6 peak is 1,2,3,4, 6-pentagalloyl glucose, the No. 10 peak is calycosin, the No. 11 peak is psoralen essence, and the No. 12 peak is isobavalin.
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| CN113917031B (en) * | 2021-10-12 | 2022-06-07 | 广东雷允上药业有限公司 | Method for determining blood concentration of lung-tonifying and blood-activating capsule in vivo by UHPLC-MS/MS method |
| CN114965732B (en) * | 2022-04-07 | 2023-12-22 | 陕西医药控股集团山海丹药业股份有限公司 | Construction method and application of HPLC fingerprint of Qitianfu body resistance strengthening capsule |
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| CN106581193B (en) * | 2017-02-24 | 2017-11-10 | 广东雷允上药业有限公司 | A kind of nourishing lung and activating blood capsule for treating COPD |
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