CN113759007B - Quality control method of curcuma kwangsiensis - Google Patents
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Abstract
The invention provides a quality control method of curcuma kwangsiensis, which solves the problem that the quality control method disclosed in the prior art can not comprehensively and effectively control the quality of curcuma kwangsiensis formula particles. The invention comprises obtaining a characteristic map of a sample solution, taking a chromatographic peak of curcumenol as a reference peak S in the characteristic map, and calculating the relative retention time of each characteristic peak and the reference peak S, wherein the relative retention time of at least five characteristic peaks and the reference peak S is within +/-10% of a specified value, and the specified value is as follows: 0.32, 0.55, 0.78, 1.09 and 1.17. The invention realizes the overall quality control of the Guangxi zedoary formula particles by the common control of curzeol and other quality evaluation index components; has the advantages of more accurate and objective judgment and accordance with the clinical medication requirement.
Description
Technical Field
The invention relates to the field of quality control of traditional Chinese medicines, in particular to a quality control method of curcuma kwangsiensis.
Background
The curcuma kwangsiensis is the dried rhizome of curcuma kwangsiensis of Zingiberaceae, and is used as a medicament together with zedoary and curcuma wenyujin, and recently, the curcuma kwangsiensis gradually becomes the mainstream variety of commercial curcuma zedoary. It is pungent, bitter and warm in flavor. It enters liver and spleen meridians. Has effects of activating qi-flowing, removing blood stasis, resolving food stagnation and relieving pain. Can be used for treating abdominal mass, amenorrhea due to blood stasis, thoracic obstruction, cardialgia, and pain due to food stagnation. The Curcuma kwangsiensis mainly contains volatile oil, curcumin, polysaccharides, phenolic acids, sterols, alkaloids, trace elements and other chemical components.
The traditional Chinese medicine decoction is a main form of clinical medication, and the basis for exerting the curative effect is the components in the standard decoction, so the types and the amounts of the components in the standard decoction are controlled, the clinical requirements are better met, and the effectiveness of the medication can be ensured. The traditional Chinese medicine prescription granule is a novel prescription medication with uniform specification, uniform dosage and uniform quality standard, which is processed by taking traditional Chinese medicine decoction pieces as raw materials through the production processes of extraction, concentration, drying, granulation and the like. The traditional Chinese medicine decoction is based on a traditional Chinese medicine standard decoction, is used under the guidance of the traditional Chinese medicine theory, and has the characteristics of convenience in taking, easiness in storage, portability, controllable quality and the like compared with the traditional Chinese medicine decoction.
In the prior art, the quality control of the curcuma kwangsiensis is mainly performed on the small polar components such as curdione, germacrone, curcumenol and the like in medicinal materials and decoction pieces. Although a student establishes a fingerprint method for vinegar curcuma zedoary formula particles by HPLC, selects curcumenol and other components for characterization, and evaluates similarity, the components corresponding to each peak in the spectrum are not specified, and the measured components are mainly small molecular components in volatile oil, and the determined components are both obtained by water extraction of decoction pieces, wherein the small molecular content of the volatile oil is low and mainly contain some water-soluble large-polarity components, so that when the fingerprint method disclosed in the prior art is applied to the vinegar curcuma zedoary formula particles, the large-polarity components are not subjected to quality control, and the quality control method disclosed in the prior art cannot effectively and comprehensively and effectively control the quality of the vinegar curcuma zedoary formula particles.
In addition, the vinegar curcuma zedoary is a processed product of the curcuma zedoary, the Guangxi curcuma zedoary is a basic source of the curcuma zedoary specified in pharmacopoeia, the material basis of the vinegar curcuma zedoary and the Guangxi curcuma zedoary is consistent, and under the condition that the quality of the vinegar curcuma zedoary formula particles cannot be controlled comprehensively in the prior quality control method, the purpose of controlling the quality of the Guangxi curcuma zedoary formula particles cannot be controlled comprehensively in the prior quality control method.
Disclosure of Invention
Therefore, the invention solves the problem that the quality control method disclosed in the prior art can not comprehensively and effectively control the quality of the Guangxi zedoary formula particles, and provides the quality control method which can comprehensively control and effectively aim at the Guangxi zedoary formula particles.
A quality control method of Curcuma kwangsiensis comprises obtaining a characteristic spectrum of a test solution, calculating the relative retention time of each characteristic peak and a reference peak S by taking a chromatographic peak of curcumenol as the reference peak S in the characteristic spectrum, wherein the relative retention time of at least five characteristic peaks is within +/-10% of a specified value, and the specified value is as follows: 0.32, 0.55, 0.78, 1.09 and 1.17.
Obtaining a characteristic spectrum of a test solution by using UPLC (ultra performance liquid chromatography), wherein the chromatographic conditions of the UPLC are as follows:
a chromatographic column: a chromatographic column using octadecylsilane chemically bonded silica as a filler; taking acetonitrile as a mobile phase A, taking a phosphoric acid solution with the mass concentration of 0.01-0.15% as a mobile phase B, and eluting according to the following gradient elution procedure:
| time (minutes) | Mobile phase A (%) | Mobile phase B (%) |
| 0～14 | 5→33 | 95→67 |
| 14～18 | 33 | 67 |
| 18～23 | 33→55 | 67→45 |
| 23～25 | 55→63 | 45→37 |
The preparation process of the test solution comprises the following steps: taking a test sample, adding a solvent, uniformly mixing, weighing, pretreating, weighing again, supplementing the lost weight with the solvent, uniformly shaking, and filtering to obtain a filtrate, wherein the filtrate is the test sample solution.
The pretreatment is ultrasonic treatment, reflux treatment or shaking treatment.
When the pretreatment is ultrasonic treatment, the treatment time is 20min-40min; the frequency and the power of ultrasonic treatment are parameters of the ultrasonic instrument, the ultrasonic instruments with different frequencies and powers can be selected to treat the solution, the power selection range of the ultrasonic instrument is 120W-300W, and the frequency selection range of the ultrasonic instrument is 40kHz-100kHz.
When the pretreatment is reflux treatment, the treatment time is 20min-40min; when a test sample is treated, the purpose of reflux is achieved, the reflux temperature needs to be selected according to different extraction solvents, and the conventional reflux temperature is 70-95 ℃.
When the pretreatment is shaking treatment, the shaking treatment time is 30min-120min.
The concentration of the test solution is 10mg/ml-60mg/ml, and the solvent is methanol with the mass concentration of 30% -100% or ethanol with the mass concentration of 30% -100%.
The detection wavelength of the UPLC is as follows: 230nm-245nm.
The chromatographic column has a column length of 5-15cm, an inner diameter of 2.1mm, and a particle diameter of 1.6-1.8 μm. Tests show that the type of the chromatographic column does not influence, and the chromatographic column is only filled with octadecylsilane bonded silica gel, so that a specific type of chromatographic column is not required, such as: ACQUITY UPLC ^ Shield RP 18/AgIlent ZORBAX SB C18/ACQUITY UPLC HSST3 or other ultra-high performance liquid chromatography columns can be selected.
The flow rate of the UPLC is 0.38ml/min-0.42ml/min, and the number of theoretical plates is not less than 5000 calculated according to curzeol. The sampling amount in the invention is selected to be 2ml-5ml under the condition of not exceeding the bearing range of the instrument and has little influence on the spectrum.
The temperature of the chromatographic column is 38-42 ℃.
The technical scheme of the invention has the following advantages:
1. the Guangxi zedoary is a basic source of zedoary prescribed by pharmacopeia, the efficacy of the Guangxi zedoary is mainly related to contained sesquiterpene components, the contained sesquiterpene components mainly comprise curcumenol, and the components are dissolved out more in standard decoction, have higher transfer rate and more stable properties, so that the characteristic map of the Guangxi zedoary formula particle is represented by a class of components represented by the curcumenol with better transfer rate in the Guangxi zedoary standard decoction; in addition, by deeply researching the components of the Guangxi rhizoma zedoariae formula particle, the characteristic peaks of other quality evaluation index components which can be better transferred into the Guangxi rhizoma zedoariae standard decoction are adopted to jointly control the overall quality of the Guangxi rhizoma zedoariae formula particle. The method specifically comprises the following steps: the characteristic peak represented by curcumenol is used as a reference peak S, and then the relative retention time of the characteristic peaks of other quality evaluation index components in the characteristic map and the reference peak S is controlled within +/-10% of a specified value, and the specified value of the relative retention time of the other quality evaluation index components is set at the same time, so that the overall quality control of the Guangxi curcuma zedoary formula particle can be realized through the common control of the curcumenol and the other quality evaluation index components, and the quality judgment of the Guangxi curcuma zedoary formula particle is more accurate and objective and meets the clinical medication requirement;
in addition, the method can also effectively realize the quality control of the substance transfer process, and specifically comprises the following steps: can effectively realize the quality control of intermediate products (extract, concentrated solution and spray powder) in the preparation process of the formula granules, and effectively ensure that the finally prepared Guangxi zedoary formula granules have the components basically consistent with standard decoction.
2. The invention further optimizes the chromatographic conditions for obtaining the characteristic spectrum, including the optimization of the mobile phase and the optimization of the gradient elution program, combines the detection wavelength, can effectively improve the peak shape, improve the chromatographic peak separation degree, embody more characteristic peak information, achieve the effect of more efficient, sensitive and accurate detection, and save the detection time and the detection cost.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a standard characteristic spectrum obtained according to Guangxi rhizoma Curcumae standard decoction lyophilized powder at a detection wavelength of 240nm in the present invention.
FIG. 2 is a characteristic diagram of Guangxi rhizoma Curcumae formulation granules obtained by the reference group failure process of the present invention.
FIG. 3 is a standard characteristic spectrum obtained according to the standard decoction lyophilized powder of Curcumae rhizoma in Guangxi of the present invention when the detection wavelength is 258 nm.
Fig. 4 is a comparison graph of characteristic spectra of intermediate products obtained in each step of the preparation process of the curcuma kwangsiensis formula particles of the present invention.
FIG. 5 is a feature map of the first embodiment of the present invention in example 3.
FIG. 6 is a feature map of a second embodiment of the present invention in example 3.
Detailed Description
Example 1
A quality control method of Curcuma kwangsiensis comprises obtaining a characteristic map of a sample solution, wherein as shown in figure 1, the characteristic map takes a chromatographic peak of curcumenol as a reference peak S, and calculates relative retention time of each characteristic peak and the reference peak S, wherein the relative retention time of at least five characteristic peaks and the reference peak S is within +/-10% of a specified value, and the specified value is: 0.32 (Peak 1), 0.55 (Peak 2), 0.78 (Peak 3), 1.00 (Peak 4), 1.09 (Peak 5), and 1.17 (Peak 6).
The chromatographic conditions of the high performance liquid chromatography in this example are as follows:
octadecyl silane bonded silica gel is used as a filler, ACQUITY UPLC Shield RP18 (the length of a column is 10cm, the inner diameter of the column is 2.1mm, and the particle size is 1.7 mu m) chromatographic columns are arranged; acetonitrile is taken as a mobile phase A, 0.1 percent phosphoric acid is taken as a mobile phase B, and gradient elution is carried out according to the specification in the following table; the detection wavelength is 240nm; the column temperature is 40 ℃; the flow rate was 0.4ml/min. The number of theoretical plates is not less than 5000 calculated according to curcumenol peak.
TABLE 1
| Time (min) | Mobile phase A (%) | Mobile phase B (%) |
| 0～14 | 5→33 | 95→67 |
| 14～18 | 33 | 67 |
| 18～23 | 33→55 | 67→45 |
| 23～25 | 55→63 | 45→37 |
Preparation of reference solutions: taking a proper amount of curcumenol reference substance, precisely weighing, and adding 70% methanol to obtain 0.1mg/ml solution as reference substance solution.
Preparation of a test solution: taking a proper amount of a test sample, grinding, taking about 0.3g, precisely weighing, placing in a conical flask with a plug, precisely adding 25ml of 70% methanol, sealing the plug, weighing, carrying out ultrasonic treatment (power 250W, frequency 40 kHz) for 20 minutes, taking out, cooling, weighing again, complementing the weight loss by 70% methanol, shaking up, filtering, and taking a subsequent filtrate to obtain the product.
The preparation process of the standard decoction freeze-dried powder of zedoary turmeric in the invention is as follows: placing a proper amount of Guangxi rhizoma zedoariae decoction pieces in a casserole, adding water with the amount 6 times of that of the decoction pieces in one decoction, soaking for 30 minutes, boiling with strong fire (500 w), decocting with slow fire (200 w) for 30 minutes, filtering while hot, and rapidly cooling for later use; adding water with the amount 5 times of that of the decoction pieces into the second decoction, boiling the second decoction with strong fire, decocting the second decoction for 20 minutes with slow fire, filtering the second decoction while the second decoction is hot, and quickly cooling the second decoction for later use; mixing filtrates, concentrating (50 deg.C) at 50 deg.C until the ratio of material to liquid is about 1 (relative density is 1.05-1.10), and freeze drying to obtain the final product.
In this embodiment, 23 batches of standard decoction lyophilized powder of curcuma kwangsiensis prepared from decoction pieces of curcuma kwangsiensis are used as a sample to be tested to obtain a characteristic spectrum of the standard decoction lyophilized powder of curcuma kwangsiensis. According to the obtained characteristic spectrum of 23 batches of standard decoction freeze-dried powder of curcuma kwangsiensis, a standard characteristic spectrum is obtained by using a traditional Chinese medicine chromatography fingerprint spectrum similarity evaluation system (2012.1 version), and identification of common peaks is carried out, wherein 6 common peaks are identified in total, as shown in figure 1. Wherein, the peak 4 is the reference peak S corresponding to the curcumenol, and the detection results of the relative retention time of 6 common peaks and the reference peak S of 23 batches of the standard decoction of Guangxi zedoary are shown in Table 2.
TABLE 2
As can be seen from table 2: the relative retention time difference of each characteristic peak is small and is within the range of +/-10 percent, thereby meeting the quality control requirement.
The same test method was used to test the Guangxi rhizoma Zedoariae granules prepared from 3 batches of obtained Guangxi rhizoma Zedoariae decoction pieces, and the results are shown in Table 3 below. The specific process of preparing Guangxi zedoary formula granules from 3 batches of Guangxi zedoary decoction pieces is as follows:
taking three batches of Guangxi rhizoma zedoariae decoction pieces with the batch numbers of 190117-535400-10, 190318-530022-19 and 190814-537600-48 respectively, crushing the decoction pieces and feeding, extracting for 3 times, adding 12 times of water for the first decoction, adding 10 times of water for the second decoction and the third decoction respectively, extracting for 1 hour each time, and extracting volatile oil for later use; filtering the extractive solution with 150 mesh filter cloth, concentrating at 80 deg.C below to density of 1.10 (60 deg.C), and clathrating the volatile oil with cyclodextrin to obtain volatile oil: cyclodextrin: water =1, grinding for 60 minutes by a colloid mill, spray drying, air inlet temperature 180 ℃, adding a proper amount of auxiliary materials, mixing uniformly, and granulating. Finally obtaining Guangxi zedoary standard granules with the batch numbers of KL190117-535400-10, KL190318-530022-19 and KL 190814-537600-48.
TABLE 3
As can be seen from table 3: the relative retention time difference of each characteristic peak of 3 batches of Guangxi zedoary formula granules is small and is within the range of +/-10 percent, thereby meeting the quality control requirement.
Meanwhile, the comparison of the characteristic spectra obtained by detecting the intermediate products (extract, concentrated solution and spray powder) obtained in each step in the preparation process of the Guangxi zedoary formula particle with the batch number of KL190814-537600-48 is shown in FIG. 4.
As can be seen from FIG. 4, the peak No. 6 in the spectrum is that after extraction, a part of the peak No. 6 is in the extracted volatile oil, and a part of the peak No. 6 is remained in the extraction, while a part of the peak in the extract causes component loss in the concentration process, so that the peak No. 6 in the spectrum of the concentrated solution is absent, and after the volatile oil inclusion compound is added, the peak No. 6 is reappeared in the spray powder. Therefore, the quality control method can effectively realize the quality control of the Guangxi zedoary formula granules, and the components of the Guangxi zedoary formula granules can be basically consistent with standard decoction.
Reference group: a batch of Guangxi rhizoma zedoariae formula granules are prepared by adopting the following unqualified process.
The Guangxi rhizoma zedoariae decoction pieces are prepared with the batch number of 190117-535400-10, the decoction pieces are crushed and fed, extracted for 3 times, 12 times of water is added in the first decoction, 10 times of water is added in the second decoction and the third decoction respectively, and the extraction is carried out for 1 hour each time; filtering the extractive solution with 150 mesh filter cloth, concentrating at 80 deg.C or below to density of 1.10 (60 deg.C), spray drying at air inlet temperature of 180 deg.C, adding appropriate amount of adjuvants, mixing, and granulating. And finally obtaining standard Guangxi zedoary particles with the batch number of KL190117-535400-10, determining the Guangxi zedoary formula particles obtained by the unqualified process by adopting the same detection method, and obtaining characteristic maps by detection, wherein the results of the characteristic maps are shown in the following table 4 and figure 2.
TABLE 4
As can be seen from Table 4 and FIG. 2, the characteristic peak 6 of the formula granule prepared by adding the non-inclusion volatile oil is absent.
Therefore, the quality control method not only can effectively realize the overall control of the quality of the Guangxi zedoary formula particle, but also can effectively realize the quality control of intermediate products (extract, concentrated solution and spray powder) in the preparation process of the formula particle, and effectively ensures that the finally prepared Guangxi zedoary formula particle has the components basically consistent with standard decoction.
Example 2
In this embodiment, the precision, repeatability and stability of the characteristic spectrum are verified by a conventional method, which specifically includes:
according to the preparation method of the test sample, 6 parts of test sample solution is prepared in parallel, the characteristic spectrum is obtained by measuring according to the method, the No. 4 peak is taken as a reference peak, the relative peak area and the relative retention time are calculated, and the RSD of each characteristic peak is in the range of 0.0-0.1% and the RSD of the relative peak area is in the range of 0.1-1.3%, which shows that the repeatability of the characteristic spectrum is better.
According to the preparation method of the test sample, 6 parts of test sample solution are prepared in parallel, different instruments are adopted to obtain characteristic maps, the No. 4 peak is taken as a reference peak, the relative peak area and the relative retention time are calculated, and as a result, the relative retention time RSD of each characteristic peak is in the range of 0.0-0.2%, and the RSD of the relative peak area is in the range of 1.0-6.8%. The relative retention time RSD range between different instruments is 0.1% -0.3%, the relative peak area RSD range is 1.1% -12.1%, and the result shows that the relative retention time of the characteristic spectrum between different instruments meets the analysis requirement.
And taking the same test sample solution, respectively injecting samples after 0, 2, 4, 6, 8, 10, 12 and 24 hours to obtain a characteristic map, taking the No. 4 peak as a reference peak, and calculating the relative peak area and the relative retention time of the reference peak, so that the relative retention time RSD of each characteristic peak is in the range of 0.0-0.2%, and the RSD of the relative peak area is in the range of 0.4-2.2%, which indicates that the chemical components in the solution have better stability within 24 hours.
Example 3
The difference between this example and example 1 is that the chromatographic conditions are different, and the specific settings are as follows:
scheme one, in the scheme, a mobile phase B is a 0.01% phosphoric acid solution, and the detection wavelength of UPLC is as follows: 230nm, a flow rate of UPLC of 0.38ml/min, and a column temperature of 38 deg.C.
Scheme II, in the scheme, the mobile phase B is 0.15% phosphoric acid solution, and the detection wavelength of UPLC is as follows: 2458n, a flow rate of UPLC of 0.42ml/min, and a column temperature of 42 ℃.
Detecting the standard Guangxi rhizoma Curcumae particles with lot numbers of KL190117-535400-10 by using the above chromatographic conditions, and obtaining chromatograms shown in FIG. 5 and FIG. 6.
Comparative example 1
The difference between this example and example 1 is that in this example, only the standard decoction lyophilized powder of curcuma kwangsiensis corresponding to the decoction pieces of curcuma kwangsiensis with lot numbers 190117-535400-10 is used as a sample, and the detection is performed with the detection wavelength of 258nm, and the obtained characteristic spectrum is shown in fig. 3.
The S peak in fig. 3 corresponds to the curcumenol chromatographic peak. As can be seen from fig. 3: although the curcumenol has maximum absorption at 258nm, the chromatographic peak behind the curcumenol cannot be detected at the wavelength, so that the characteristic map information is not rich enough.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (7)
1. A quality control method of Curcuma kwangsiensis is characterized by comprising the steps of obtaining a characteristic map of a sample solution, calculating the relative retention time of each characteristic peak and a reference peak S by taking a chromatographic peak of curzeol as the reference peak S in the characteristic map, wherein the relative retention time of at least five characteristic peaks is within +/-10% of a specified value, and the specified value is as follows: 0.32, 0.55, 0.78, 1.09, 1.17;
obtaining a characteristic spectrum of a test solution by using UPLC, wherein the chromatographic conditions of the UPLC are as follows:
and (3) chromatographic column: a chromatographic column using octadecylsilane chemically bonded silica as a filler; the length of the chromatographic column is 5-15cm, the inner diameter of the chromatographic column is 2.1mm, and the particle size is 1.6-1.8 μm; taking acetonitrile as a mobile phase A, taking a phosphoric acid solution with the mass concentration of 0.01-0.15% as a mobile phase B, and eluting according to the following gradient elution procedure:
The solvent of the test solution is methanol with the mass concentration of 30-100% or ethanol with the mass concentration of 30-100%;
the detection wavelength of the UPLC is as follows: 230nm-245nm.
2. The method for controlling the quality of curcuma kwangsiensis as claimed in claim 1, wherein the preparation process of the test solution is as follows: taking a test sample, adding a solvent, uniformly mixing, weighing, pretreating, weighing again, supplementing the lost weight with the solvent, uniformly shaking, and filtering to obtain a filtrate, wherein the filtrate is the test sample solution.
3. The method for controlling the quality of curcuma kwangsiensis according to claim 2, wherein the pretreatment is ultrasonic treatment, reflux treatment or shaking treatment.
4. The method for controlling the quality of Curcuma kwangsiensis Koch as claimed in claim 3, wherein,
when the pretreatment is ultrasonic treatment, the treatment time is 20min-40min;
when the pretreatment is reflux treatment, the treatment time is 20min-40min;
when the pretreatment is shaking treatment, the shaking treatment time is 30min-120min.
5. The method for controlling the quality of zedoary turmeric according to any one of claims 2 to 4, wherein the concentration of said sample solution is 10mg/ml to 60mg/ml.
6. The method for controlling the quality of curcuma kwangsiensis according to any one of claims 2 to 4, wherein the flow rate of UPLC is 0.38ml/min to 0.42ml/min, and the number of theoretical plates is not less than 5000 calculated according to curcumenol.
7. The method for controlling the quality of curcuma kwangsiensis according to any one of claims 2-4, wherein the column temperature of said chromatographic column is 38-42 ℃.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101144802A (en) * | 2006-08-01 | 2008-03-19 | 烟台大学 | Zedoary turmeric oil analysis method |
| CN105738546A (en) * | 2014-12-12 | 2016-07-06 | 桂林八加一药物研究股份有限公司 | Establishment method of curcuma aromatica medicine fingerprint map and the fingerprint map thereof |
| CN110082446A (en) * | 2019-05-08 | 2019-08-02 | 陕西中医药大学 | A kind of turmeric quality determining method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101144802A (en) * | 2006-08-01 | 2008-03-19 | 烟台大学 | Zedoary turmeric oil analysis method |
| CN105738546A (en) * | 2014-12-12 | 2016-07-06 | 桂林八加一药物研究股份有限公司 | Establishment method of curcuma aromatica medicine fingerprint map and the fingerprint map thereof |
| CN110082446A (en) * | 2019-05-08 | 2019-08-02 | 陕西中医药大学 | A kind of turmeric quality determining method |
Non-Patent Citations (4)
| Title |
|---|
| Meiqiong Liu 等.Spectrum–effect relationship between HPLC fingerprints and hypolipidemic effect of Curcuma aromatica.2018,第32卷1-7. * |
| 周欣 等.蓬莪术药材醇提取物LC-MS指纹图谱的研究.2008,第33卷(第19期),2218-2221. * |
| 杨丰庆.中药莪术高效液相色谱指纹图谱分析.2009,第28卷294-296. * |
| 郝敏 等.3种温郁金根茎炮制品的UPLC指纹图谱与多成分含量测定研究.2018,第43卷(第11期),2288-2294. * |
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