CN103487528B - HPLC fingerprint determination method of cough relieving Bulbus fritillariae cirrhosae and loquat dripping pills - Google Patents
HPLC fingerprint determination method of cough relieving Bulbus fritillariae cirrhosae and loquat dripping pills Download PDFInfo
- Publication number
- CN103487528B CN103487528B CN201310472601.8A CN201310472601A CN103487528B CN 103487528 B CN103487528 B CN 103487528B CN 201310472601 A CN201310472601 A CN 201310472601A CN 103487528 B CN103487528 B CN 103487528B
- Authority
- CN
- China
- Prior art keywords
- tendril
- loquat
- peak
- fritillary bulb
- peaks
- 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.)
- Active
Links
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
An HPLC (high performance liquid chromatography) fingerprint determination method of cough relieving Bulbus fritillariae cirrhosae and loquat dripping pills comprises the following steps: 1, cough relieving Bulbus fritillariae cirrhosae and loquat dripping pill tested substance solution preparation: preciously weighing the cough relieving Bulbus fritillariae cirrhosae and loquat dripping pills, and carrying out ultrasonic extraction of the cough relieving Bulbus fritillariae cirrhosae and loquat dripping pills by using 30-100% ethanol as an extraction solvent to prepare a tested substance solution; and 2, injecting the solution obtained in step 1 into a high performance liquid chromatograph, and determining to obtain a cough relieving Bulbus fritillariae cirrhosae and loquat dripping pill fingerprint. An HPLC method is adopted to establish the fingerprint according to the self characteristics of the cough relieving Bulbus fritillariae cirrhosae and loquat dripping pills, and optimal chromatogram conditions are found, so the determination result is precious, and has a good reappearance and a good stability.
Description
Technical field
The invention belongs to medical art, especially relate to and a kind ofly control the HPLC finger print measuring method coughing tendril-leaved fritillary bulb loquat drop pills.
Background technology
Control and cough tendril-leaved fritillary bulb loquat drop pills and be made up of loguat leaf, fritillary bulb, balloonflower root, RHIZOMA TYPHONII FLAGELLIFORMIS, menthol, adopt modernization preparation process technology to refine to form, there is the effect of a surname's lung sending down abnormally ascending, clearing heat and eliminating phlegm, cough caused for the strongly fragrant lung of phlegm heat, disease is seen cough, is coughed up phlegm, dry throat, pharyngalgia, heating, general malaise; Flu and bronchitis are shown in above-mentioned disease person, are the herbal species by special-protection-by-the-State.
The quality of traditional Chinese medicine quality, the difference after all existed in contained chemical composition in the inner and content thereof.This species diversity can be reflected by the chromatographic fingerprinting of Chinese medicine.As effective control device of the whole evaluation traditional Chinese medicine quality of multi-component complex sample, traditional Chinese medicine fingerprint is at present can for a kind of method of thoroughly evaluating traditional Chinese medicine quality pattern accepted extensively both at home and abroad.
Have about controlling the research coughing in tendril-leaved fritillary bulb loquat drop pills finger-print that there is not been reported at present at home and abroad, in order to better control its quality, ensure security and the validity of clinical application, better Instructing manufacture, make technology controlling and process more rationally strict, be necessary that its fingerprint pattern quality control method is set up in research.
Summary of the invention
The invention provides and a kind ofly control the HPLC finger print measuring method coughing tendril-leaved fritillary bulb loquat drop pills, the method comprises the following steps:
(1) control the preparation coughing tendril-leaved fritillary bulb loquat drop pills need testing solution: accurately weighed controlling coughs tendril-leaved fritillary bulb loquat drop pills, with the ethanol of 30%-100% as Extraction solvent, ultrasonic extraction, as need testing solution;
(2) solution step (1) obtained injects high performance liquid chromatograph and measures, and obtains controlling the finger-print coughing tendril-leaved fritillary bulb loquat drop pills.
Preferably, in step (1), Extraction solvent is 30% ethanol or 80% ethanol.
Further, the liquid-phase chromatographic column in step (2) take octadecylsilane chemically bonded silica as filling agent.
Preferably, the liquid chromatography in step (2) adopts 0.2% aqueous formic acid-acetonitrile to do mobile phase, and liquid phase chromatogram condition is:
Chromatographic column: ACQUITY UPLC HSS T3,1.8um, 2.1 × 100mm, Waters take acetonitrile as mobile phase A, with 0.2% aqueous formic acid for Mobile phase B, carry out gradient elution; Column temperature is 40 DEG C; Flow velocity is 0.2ml per minute, and determined wavelength is 320nm, and condition of gradient elution is:
Preferably, liquid chromatography in step (2) adopts 0.2% aqueous formic acid-methyl alcohol to do mobile phase, liquid phase chromatogram condition is: chromatographic column: ACQUITY UPLC HSS T3,1.8um, 2.1 × 100mm, Waters take methyl alcohol as mobile phase A, with 0.2% aqueous formic acid for Mobile phase B, carry out gradient elution; Column temperature is 40 DEG C; Flow velocity is 0.2ml per minute, and determined wavelength is 320nm, and condition of gradient elution is:
Object of reference solution of the present invention is chlorogenic acid reference substance: get chlorogenic acid accurately weighed in right amount, adds methyl alcohol and is mixed with every 1 milliliter of solution containing 0.1mg chlorogenic acid.
Accurate absorption object of reference solution and each 1 μ l of need testing solution, inject Ultra Performance Liquid Chromatography instrument respectively, measures, and record chromatogram, formulates to control and cough tendril-leaved fritillary bulb loquat drop pills liquid-phase fingerprint; Test sample liquid-phase fingerprint selects representative sample as standard finger-print, and should present 25 total peaks in test sample finger-print, the peak corresponding to object of reference peak is S peak, is designated as No. 6 peaks, calculates the relative retention time at each total peak and S peak.
Each total peak with the relative retention time at S peak be: No. 1 peak 0.347, No. 2 peaks 0.618, No. 3 peaks 0.715, No. 4 peaks 0.864, No. 5 peaks 0.932, No. 6 S peaks 1.000, No. 7 peaks 1.066, No. 8 peaks 1.133, No. 9 peaks 1.268, No. 10 peaks 1.284, No. 11 peaks 1.304, No. 12 peaks 1.332, No. 13 peaks 1.393, No. 14 peaks 1.453, No. 15 peaks 1.539, No. 16 peaks 1.628, No. 17 peaks 1.771, No. 18 peaks 1.798, No. 19 peaks 1.822, No. 20 peaks 1.941, No. 21 peaks 2.165, No. 22 peaks 2.290, No. 23 peaks 2.434, No. 24 peaks 2.466, No. 25 peaks 2.539.
Present invention also offers and a kind ofly control the method for quality control coughing tendril-leaved fritillary bulb loquat drop pills, comprise the following steps:
(1) get qualified have control and cough tendril-leaved fritillary bulb loquat drop pills product, control the standard finger-print coughing tendril-leaved fritillary bulb loquat drop pills according to said determination method establishment;
(2) get to be checked controlling and cough tendril-leaved fritillary bulb loquat drop pills, obtain finger-print according to said determination method;
(3) standard finger-print that finger-print step (2) obtained and step (1) obtain contrasts, and meets and is specification product, do not meet and be substandard product.
Wherein, the finger-print of specification product and the similarity of standard finger-print must not lower than 0.90; The non-shared peak total area must not be greater than 10% of total peak area.
The advantage that the present invention has and good effect are:
(1) the present invention controls in foundation and coughs in the finger-print process of tendril-leaved fritillary bulb loquat drop pills, confirms 25 common characteristic peaks, and is studied its relative retention time and relative peak area, ensure that chemical composition stability and the safety in utilization of preparation.
(2) control and cough complex chemical composition in tendril-leaved fritillary bulb loquat drop pills flavour of a drug, the separating difficulty realizing its characteristic fingerprint peak is large, the present invention, in the process setting up finger-print, have employed the method for gradient elution, solves fingerprint characteristic peak and is difficult to separately and the interference problem of impurity peaks.
(3) foundation is controlled and is coughed tendril-leaved fritillary bulb loquat drop pills standard finger-print, overcomes the defect that single component assay is difficult to reflect whole content, on the whole, macroscopically can control to control the inherent quality coughing tendril-leaved fritillary bulb loquat drop pills.
(4) cough each effective constituent fingerprint graph in tendril-leaved fritillary bulb loquat drop pills integrally treat to control, focus on tandem and the mutual relationship of each characteristic peak, both avoided and judged to control because only measuring one, two chemical composition the one-sidedness coughing tendril-leaved fritillary bulb loquat drop pills total quality, additionally reduced the possibility artificially processed for requisite quality.Control for complete, accurate evaluation the quality coughing tendril-leaved fritillary bulb loquat drop pills and provide new ways and means.
(5) high, the favorable reproducibility of the inventive method good stability, precision, convenient and be easy to grasp.
Accompanying drawing explanation
Fig. 1 be the present invention 10 crowdes control cough tendril-leaved fritillary bulb loquat drop pills liquid chromatogram superposition collection of illustrative plates
Fig. 2 controls the liquid chromatography reference fingerprint coughing tendril-leaved fritillary bulb loquat drop pills
Embodiment
Embodiment 1: control the HPLC finger print measuring method coughing tendril-leaved fritillary bulb loquat drop pills
1.1 instruments and reagent
Instrument: Waters ACQUITY TM UPLC Ultra Performance Liquid Chromatography instrument, Masslynx
tM4.0 workstation;
Chromatographic column: ACQUITY UPLC HSS T3,1.8um, 2.1 × 100mm, Waters
Reagent: methyl alcohol, acetonitrile, formic acid are chromatographically pure (Fisher), and water is ultrapure water, it is pure that all the other reagent are analysis.
The preparation of 1.2 object of reference solution
The retention time of chlorogenic acid (self-control, structure is through MS, UV, FIR, NMR confirmation) is 7.99min, responds comparatively strong, substantially can reach baseline separation, therefore, specify it to be object of reference with front and back impurity under this condition.Get chlorogenic acid appropriate, accurately weighed, add methyl alcohol and be mixed with the solution containing 0.1mg chlorogenic acid in every 1 milliliter, shake up, to obtain final product.
The preparation of 1.3 need testing solutions
Up-to-standard 10 batches of standard need testing solution are controlled and cough tendril-leaved fritillary bulb loquat drop pills as standard items (No.6 Chinese Medicine Factory, Tianjin Zhongxin Pharmaceutical Industry Group Co provides, and lot number is respectively 630120,631017,631021,631024,631026,631036,631039,631045,631048,632002 totally 10 batches).Accurately weighed 0.5g, is placed in erlenmeyer flask, and precision adds 80% ethanol water 10mL, and ultrasonic extraction 15min, leaves standstill to room temperature, filters, gets subsequent filtrate, to obtain final product.
1.3.1, the selection of Extraction solvent alcohol water ratio
Investigate 30% ethanol water, 50% ethanol water, 80% ethanol water, the need testing solution of the ultrasonic extraction of 100% ethanolic solution detects under the detection method determined, find that in the chromatogram of the need testing solution of the ultrasonic extraction of 100% ethanolic solution, indivedual chromatographic peak peak shape is poor, in the chromatogram of the need testing solution of the ultrasonic extraction of 50% ethanolic solution, chromatographic peak peak area is all on the low side, and the chromatogram of the need testing solution of the ultrasonic extraction of 30% ethanolic solution and the need testing solution of the ultrasonic extraction of 80% ethanolic solution is substantially without significant difference, consider the shelf stability of need testing solution, therefore select 80% ethanol water as Extraction solvent.
1.3.2, the selection of Extraction solvent volume
The need testing solution investigating the ultrasonic extraction of 5mL, 10mL, 25mL, 50mL80% ethanolic solution respectively detects under the detection method determined, find that the peak area at each peak in the chromatogram of the need testing solution that 5mL Extraction solvent extracts is all lower, in the chromatogram of the need testing solution that 10mL Extraction solvent extracts, chromatographic peak information is comparatively abundant and peak shape is better, in the chromatogram of the need testing solution that 25mL and 50mL Extraction solvent extracts, chromatographic peak peak shape is poor respectively, and therefore the volume of selective extraction solvent is 10mL.
1.3.3, the selection of extraction time
Investigate the ultrasonic need testing solution extracting 15min, 30min, 45min respectively of 80% ethanolic solution to detect under the detection method determined, find that the chromatogram of three is substantially without significant difference, therefore the selective extraction time is 15min.
1.4 chromatographic condition
Take octadecylsilane chemically bonded silica as filling agent, (column length is 10cm, and internal diameter is 2.1mm, and particle diameter is 1.8um), take acetonitrile as mobile phase A, with 0.2% aqueous formic acid for Mobile phase B, carries out gradient elution by table 1; Column temperature is 40 DEG C; Flow velocity is 0.2ml per minute, and determined wavelength is 320nm.Theoretical cam curve calculates should be not less than 80000 by object of reference peak.
Table 1 condition of gradient elution
1.4.1 the selection of mobile phase
Adopt 0.2% aqueous formic acid and acetonitrile and 0.2% aqueous formic acid and methyl alcohol as flow visualizing respectively, at ACQUITY UPLC HSS T3(1.8um, 2.1 × 100mm, Waters) chromatographic column is separated, optimization condition of gradient elution, gradient elution program is as follows.
Table 2 condition of gradient elution I
Table 3 condition of gradient elution II
Under the condition that eluotropic strength is close, for main chromatographic peak, 0.2% aqueous formic acid and methyl alcohol is adopted to carry out gradient elution (condition II) as mobile phase, with 0.2% aqueous formic acid and acetonitrile as compared with mobile phase (condition I), indivedual peaks degree of separation is slightly poor, so, select 0.2% formic acid water and acetonitrile as mobile phase, carry out wash-out by gradient condition I, control the main compound coughing opposed polarity in tendril-leaved fritillary bulb loquat drop pills and can reach good separation.
1.4.2, the selection of chromatographic column:
①ACQUITY UPLC HSS T3，1.8um，2.1×100mm，Waters
②ACQUITY UPLC Shield RP18，1.7um，2.1×100mm，Waters
③ACQUITY UPLC BEH HILIC，1.7um，2.1×100mm，Waters
With 0.2% aqueous formic acid and acetonitrile for mobile phase, adopt condition of gradient elution I, analyze at above-mentioned 3 root chromatogram columns.Result shows to adopt 1. number chromatographic column, controls the main chromatogram peak energy coughed in tendril-leaved fritillary bulb loquat drop pills and obtains desirable separating effect, and peak shape is symmetrical.Therefore 1. number chromatographic column is selected to carry out compartment analysis in this experiment.
1.4.3, the selection of wavelength
By carrying out UV scanning with photodiode array detector to each chromatographic peak, three-dimensional uv absorption chromatogram is shown in Fig. 2, the chromatogram extracted under 210nm, 254nm, 280nm and 320nm wavelength contrasts, when finding using 320nm as determined wavelength, the information of compound comparatively horn of plenty on chromatogram, baseline is steady.Therefore select 320nm as determined wavelength, carry out data statistics and similarity analysis.
1.5 measure
Accurate absorption object of reference solution and each 1 μ l of need testing solution, inject Ultra Performance Liquid Chromatography instrument respectively, measures, record chromatogram.; Test sample finger-print Content of Chlorogenic Acid object of reference peak is S peak (peak 6), calculates relative retention time; The peak area at S peak (No. 6 peaks) is 1, calculates other each common characteristic fingerprint peaks peak area ratio.
1.5.1 the determination at total peak
According to 10 batches of test sample liquid chromatography collection of illustrative plates, determine that total peak should have 25, each total peak successively label is 1,2 ..., N, wherein object of reference peak label is 6(S).
1.5.2 total peak relative retention time
With No. 6 total peaks for reference, calculate each total peak relative retention time in 10 batches of test samples, the results are shown in Table 4.Shown by table 4, relative retention time has good reappearance, meets " technical requirement of traditional Chinese medicine finger-print research " (provisional).The difference of each total peak relative retention time and its average is all less than 0.2%.Therefore, specify in this product finger-print, in test sample collection of illustrative plates each total peak relative retention time setting (average) ± 2% within.
Table 4 has peak relative retention time
1.5.3 the ratio of total peak area
According to 10 batches of test sample liquid chromatography collection of illustrative plates, have selected and have distinctive 8 total fingerprint peakses, No. 3 peaks, No. 4 peaks, No. 5 peaks, No. 6 peaks, No. 7 peaks, No. 10 peaks, No. 11 peaks, No. 14 peaks carry out the odds ratio of peak area comparatively; It is No. 6 peaks (object of reference peak), No. 7 peaks, No. 10 peaks that unimodal area accounts for the total peak that total peak area is greater than 10%; Unimodal area accounts for total peak area and is greater than 5%, and the total peak being less than 10% is No. 3 peaks, No. 11 peaks, No. 14 peaks; Other unimodal area in each peak accounts for total peak area and is all less than 5%.
Select total coneincone area relatively large in this product finger-print, the peak area at more stable No. 6 total peaks (object of reference peak), as 1, calculates the ratio of other each common characteristic fingerprint peaks peak area, the results are shown in Table 5.Specify in this product finger-print, in test sample collection of illustrative plates, in the ratio of each total peak area and finger-print, the odds ratio of each total peak area is comparatively, except No. 6 peaks (object of reference peak), No. 3 total peaks, No. 7 total peaks, No. 11 its differences of total peak must not be greater than ± and 10%; No. 10 total peaks, No. 14 its differences of total peak must not be greater than ± and 20%; Other unimodal area in each peak accounts for total peak area and is all less than 5%, and peak area ratio does not do requirement.
Table 5 has the ratio of peak area
1.5.4, non-shared peak area
The non-shared peak total area accounts for the percent value of total peak area in table 6, and result shows, the non-shared peak total area accounts for total peak area number percent and is all less than 10%, meets " technical requirement of traditional Chinese medicine finger-print research " (provisional).
The table 6 non-shared peak total area accounts for total peak area number percent
1.5.5, fingerprint similarity
With common pattern (average vector) for reference, calculated by included angle cosine and related coefficient two kinds of algorithms.10 batches of test sample data and Similarity Measure the results are shown in Table 6, table 7.Result shows, each batch of similarity between test sample and common pattern all >=0.927.Therefore, specify that each batch of similarity between test sample and common pattern should be not less than 0.9.
Table 7 similar matrix (related coefficient)
Table 8 similar matrix (included angle cosine)
Table 9 sample number is corresponding with lot number to be shown
Test example 1: methodological study
Assay method of the present invention, its chromatographic condition is through Method validation, and result is good.
Precision test:
(lot number: 631021), injects Ultra Performance Liquid Chromatography instrument, continuous sample introduction 6 times, adds up respectively to the relative retention time at each common characteristic peak and peak area relative ratio to get same need testing solution.Result shows, controls the relative retention time coughing tendril-leaved fritillary bulb loquat drop pills each common characteristic peak basically identical, RSD < 3%; The peak area relative ratio at each total peak is basically identical, RSD < 3%, controls to cough tendril-leaved fritillary bulb loquat drop pills liquid-phase fingerprint precision test and meet the requirements.
Stability test:
(lot number: 631021) at room temperature preserve measures respectively at 0,2,4,6,8,24 hour sample introduction to get need testing solution.Respectively the relative retention time at each common characteristic peak and peak area relative ratio are added up.Result shows, controls the relative retention time coughing each total peak of tendril-leaved fritillary bulb loquat drop pills basically identical, RSD < 3%; The peak area relative ratio at each total peak is basically identical, RSD < 3%, controls to cough the stability test of tendril-leaved fritillary bulb loquat drop pills finger-print and meet the requirements.
Reappearance is tested
(lot number: 631021) make 6 parts of need testing solutions respectively, injects Ultra Performance Liquid Chromatography instrument and measures, and adds up respectively to the relative retention time at each total peak and peak area relative ratio to get need testing solution.Result shows, controls the relative retention time coughing each total peak of tendril-leaved fritillary bulb loquat drop pills basically identical, RSD < 3%; The peak area relative ratio at each total peak is basically identical, RSD < 3%, controls and coughs the requirement of tendril-leaved fritillary bulb loquat drop pills reproducibility of fingerprint agreement with experimental.
Above measurement result shows, with this liquid chromatography for measuring control cough tendril-leaved fritillary bulb loquat drop pills liquid-phase fingerprint stability, precision, reappearance test all meet the requirements, this liquid phase chromatography therefore can be selected as controlling the assay method coughing tendril-leaved fritillary bulb loquat drop pills liquid-phase fingerprint.
Above preferred embodiment of the present invention has been described in detail, but described content being only preferred embodiment of the present invention, can not being considered to for limiting practical range of the present invention.All equalizations done according to the present patent application scope change and improve, and all should still belong within patent covering scope of the present invention.
Claims (3)
1. control the HPLC finger print measuring method coughing tendril-leaved fritillary bulb loquat drop pills, it is characterized in that, comprise the following steps:
(1) control the preparation coughing tendril-leaved fritillary bulb loquat drop pills need testing solution: accurately weighed controlling coughs tendril-leaved fritillary bulb loquat drop pills, with the ethanol of 30%-100% as Extraction solvent, ultrasonic extraction, as need testing solution;
(2) solution step (1) obtained injects high performance liquid chromatograph and measures, and obtains controlling the finger-print coughing tendril-leaved fritillary bulb loquat drop pills;
Liquid phase chromatogram condition in described step (2) is:
Chromatographic column: ACQUITY UPLC HSS T3,1.8um, 2.1 × 100mm, Waters take acetonitrile as mobile phase A, with 0.2% aqueous formic acid for Mobile phase B, carry out gradient elution; Column temperature is 40 DEG C; Flow velocity is 0.2ml per minute, and determined wavelength is 320nm, and condition of gradient elution is:
。
2. assay method according to claim 1, is characterized in that: in described step (1), Extraction solvent is 30% ethanol or 80% ethanol.
3. assay method according to claim 2, is characterized in that: described liquid chromatography adopts 0.2% aqueous formic acid-methyl alcohol to do mobile phase;
Liquid phase chromatogram condition in described step (2) is: chromatographic column: ACQUITY UPLC HSS T3,1.8um, and 2.1 × 100mm, Waters take methyl alcohol as mobile phase A, with 0.2% aqueous formic acid for Mobile phase B, carry out gradient elution; Column temperature is 40 DEG C; Flow velocity is 0.2ml per minute, and determined wavelength is 320nm, and condition of gradient elution is:
。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310472601.8A CN103487528B (en) | 2013-10-11 | 2013-10-11 | HPLC fingerprint determination method of cough relieving Bulbus fritillariae cirrhosae and loquat dripping pills |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310472601.8A CN103487528B (en) | 2013-10-11 | 2013-10-11 | HPLC fingerprint determination method of cough relieving Bulbus fritillariae cirrhosae and loquat dripping pills |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103487528A CN103487528A (en) | 2014-01-01 |
| CN103487528B true CN103487528B (en) | 2015-04-22 |
Family
ID=49827914
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310472601.8A Active CN103487528B (en) | 2013-10-11 | 2013-10-11 | HPLC fingerprint determination method of cough relieving Bulbus fritillariae cirrhosae and loquat dripping pills |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103487528B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105606752A (en) * | 2016-01-22 | 2016-05-25 | 哈尔滨市康隆药业有限责任公司 | Detection method of fingerprint spectrums of sugar-free strong pipa syrup |
| CN108445124A (en) * | 2018-03-20 | 2018-08-24 | 浙江省食品药品检验研究院 | Method for building up, standard finger-print and the application of thoroughfare Fructus Aurantii HPLC finger-prints |
| CN110361459B (en) * | 2019-05-20 | 2022-04-05 | 国药集团德众（佛山）药业有限公司 | Method for establishing loquat leaf standard decoction fingerprint |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102370921A (en) * | 2010-08-26 | 2012-03-14 | 江西济民可信集团有限公司 | Detection method of strong loquat dew traditional Chinese preparation |
| CN102854281A (en) * | 2012-08-29 | 2013-01-02 | 哈尔滨市康隆药业有限责任公司 | Detection method of sugar-free strong loquat syrup |
-
2013
- 2013-10-11 CN CN201310472601.8A patent/CN103487528B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102370921A (en) * | 2010-08-26 | 2012-03-14 | 江西济民可信集团有限公司 | Detection method of strong loquat dew traditional Chinese preparation |
| CN102854281A (en) * | 2012-08-29 | 2013-01-02 | 哈尔滨市康隆药业有限责任公司 | Detection method of sugar-free strong loquat syrup |
Non-Patent Citations (5)
| Title |
|---|
| Rapid and Global Identification of Potentially Bioactive Crude Extracts from Chinese Medicinal Formula Chuanbeipipa Dropping Pills;Lin-Yi DONG等;《Latin American Journal of Pharmacy》;20120228;第31卷(第1期);第18-26页 * |
| UPLC-Q-TOF-MS测定治咳川贝枇杷滴丸中6种有效成分的含量;董林毅等;《中国药学杂志》;20120531;第47卷(第10期);第830-833页 * |
| 川贝枇杷糖浆含量测定的研究;黄玮;《现代中药研究与实践》;20111130;第25卷(第6期);第75-77页 * |
| 治咳川贝枇杷滴丸UPLC-Q-TOF-MSE指纹图谱研究;罗艺等;《药物分析杂志》;20121130;第32卷(第11期);第1941页第1-3节 * |
| 治咳川贝枇杷滴丸的质量控制及其挥发性成分的测定;殷玮等;《中国医药工业杂志》;20130930;第44卷(第9期);第879页第1-2节 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103487528A (en) | 2014-01-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104502518B (en) | A kind of detection method for the treatment of the Chinese medicine preparation of baby anorexia | |
| CN104458993B (en) | The method for building up of strong medicinal material blumea riparia HPLC finger-print | |
| CN110031570A (en) | The fingerprint atlas detection method of Kangganmao Granule | |
| CN107356691A (en) | Build the detection method of bent finger-print | |
| CN101966223A (en) | Fingerprint detection method for compound wintercreeper preparation | |
| CN107402265B (en) | Detection method of Kangyun granule fingerprint | |
| CN103487528B (en) | HPLC fingerprint determination method of cough relieving Bulbus fritillariae cirrhosae and loquat dripping pills | |
| CN103424498B (en) | Establishing method and application of fingerprint of detoxifying and kidney harmonizing capsule | |
| CN104316613B (en) | A kind of method for building up of dispelling wind detoxicating capsule finger printing | |
| CN110031564B (en) | Quality detection method of natural plant anticoccidial feed additive based on HPLC fingerprint | |
| CN102944625A (en) | Method for establishing carthamus tinctorius fingerprint by using high performance liquid chromatography and standard fingerprint of method | |
| CN102133333A (en) | Quality control method for shenmai injection mass spectrum finger prints | |
| CN108663440A (en) | Callicarpa nudiflora medicinal material UPLC fingerprint map constructions method and standard finger-print | |
| CN104849384B (en) | Set up method and its application of strong diisopropyl amine dichloro acetate preparation finger | |
| CN105699581B (en) | The construction method and its standard finger-print of the UPLC finger-print of sweet clover medicinal material | |
| CN110274970A (en) | The method for building up for melting poor finger-print and its application in Yixiesheng capsule Quality Control | |
| CN103293261A (en) | Content determination method of rhizoma bletillae | |
| CN102048906A (en) | Content measurement method of abrus herb capsules | |
| CN113759010B (en) | Method for constructing Chinese rose flower characteristic map | |
| CN102335333A (en) | Method for detecting traditional Chinese medicine preparation of compound nutritions paste | |
| CN115524424A (en) | Capsella bursa-pastoris sample quality control method | |
| CN109061024B (en) | Construction method and application of standard fingerprint spectrum of infant spleen-supporting granules | |
| CN109781884B (en) | Establishing method of Qianliexin capsule fingerprint and fingerprint thereof | |
| CN103575823A (en) | Detection method of 8 chemical components in Tangminling preparation | |
| CN108956835A (en) | A kind of fingerprint atlas detection method of the antipyretic oral drugs of clearing |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 300401 Tianjin city Beichen District North Light Patentee after: Jinyao Darentang Group Co.,Ltd. No 6 Chinese Medicine Factory Address before: 300401 Tianjin city Beichen District North Light Patentee before: No. 6 Traditional Chinese Medicine Factory of Tianjin Zhongxin Pharmaceutical Group Co.,Ltd. |
|
| CP01 | Change in the name or title of a patent holder |