CN109828070B - Method for determining fingerprint of traditional Chinese medicine shengqiang decoction - Google Patents
Method for determining fingerprint of traditional Chinese medicine shengqiang decoction Download PDFInfo
- Publication number
- CN109828070B CN109828070B CN201910196913.8A CN201910196913A CN109828070B CN 109828070 B CN109828070 B CN 109828070B CN 201910196913 A CN201910196913 A CN 201910196913A CN 109828070 B CN109828070 B CN 109828070B
- Authority
- CN
- China
- Prior art keywords
- mobile phase
- fingerprint
- decoction
- chinese medicine
- traditional chinese
- 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
Images
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method for determining traditional Chinese medicine shengqiang decoction fingerprint, which adopts high performance liquid chromatography, and the chromatographic conditions comprise: the chromatographic column is an octadecylsilane chemically bonded silica chromatographic column, acetonitrile or methanol is used as a mobile phase A, phosphate buffer aqueous solution is used as a mobile phase B, and a DAD detector is used as the detector, so that gradient elution is carried out. The method is rapid, simple, convenient, comprehensive, accurate and reliable, and is suitable for detecting the fingerprint of the shengqiang soup.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicines, in particular to a method for measuring a fingerprint of a traditional Chinese medicine shengqiang decoction.
Background
The prescription of Sheng Qiang Tang is from the 'xi Lu of Zhong Can' of Qing Fing Xi, the 'treatment of sinking of the atmosphere in the chest, short breath and no rest … …'.
The prescription of the decoction for promoting the secretion of qi comprises: six cents of raw astragalus, three cents of rhizoma anemarrhenae, five cents of radix bupleuri, five cents of platycodon grandiflorum and one cents of rhizoma cimicifugae.
The function of the shengxiao decoction is mainly indicated: when the chest is depressed, the breath is short enough to breathe, or the breath is hard to breathe, there appears to be asthma, or the breath stops, which is dangerous to be in the hectare. It is accompanied by alternating chills and fever, dry throat with thirst, fullness and oppression, severe palpitation, coma, amnesia, and deep, slow and weak pulse. The modern clinical application is mainly used for treating coronary heart disease, chronic heart failure and the like.
The traditional Chinese medicine fingerprint is developed by using a DNA fingerprint. The first developed is the chromatographic fingerprint of chemical components of Chinese medicine, especially the High Performance Liquid Chromatography (HPLC) fingerprint. HPLC has high resolution, different chemical components can be separated to form chromatographic peaks with different heights to form a chromatogram, and the heights and peak areas of the chromatographic peaks respectively represent various chemical components and the contents of the chemical components. The whole chromatogram represents the amount and quantity of chemical components contained in the sample.
The traditional Chinese medicine fingerprint has an important position in modern and future traditional Chinese medicine quality control, accords with the characteristics of integrity and fuzziness of traditional Chinese medicines, can analyze the information of types and content distribution of effective components and ineffective components in the traditional Chinese medicines, and has more important functions in various aspects such as traditional Chinese medicine quality control, traditional Chinese medicine pharmacodynamic component research, traditional Chinese medicine action mechanism research and the like along with the continuous application of more and more technologies to the traditional Chinese medicine fingerprint research.
The traditional Chinese medicine fingerprint has more advantages than the DNA fingerprint, not only has the characteristics of qualitative identification and use (the number and relative position of various chemical components-retention time), but also has the quantity concept, the height and the peak area of the peak represent the content of a certain chemical component, and the ratio of the peak height (or the peak area) of each peak represents the relative content among various chemical components. The combination of qualitative and quantitative endows the traditional Chinese medicine with greater effect of fingerprint spectrum. The traditional Chinese medicine fingerprint spectrum not only can identify the uniqueness of an individual and a certain species, but also can hook the quantity characteristics of the individual and the species with other systems, such as the drug effect research result. The fingerprint of the ginkgo biloba extract shows the 33 ginkgo biloba flavonoids (chemical components) and the respective contents. In germany, over 30 years of chemical composition and pharmacodynamic related studies, it is a typical example that ginkgo extract consisting of about 24% ginkgetin and about 6% ginkgolide (with corresponding fingerprint pattern to control its composition and relative content) has the best therapeutic effect. Therefore, the traditional Chinese medicine fingerprint is not only a traditional Chinese medicine quality control mode and technology, but also can be developed into a research system and a research mode for developing traditional Chinese medicine theories (complex systems) and new drugs by adopting various fingerprints[1]. (reference: [1 ]]) Roo Guan, Wang Yi Ming, Cao jin, multidimensional and multi-information characteristic spectrum and application thereof [ J]Chinese patent medicine 2000, 22(6): 395)
In order to control the quality of the traditional Chinese medicine compound shengqiang decoction and analyze the information of the variety and content distribution of each component in the traditional Chinese medicine shengqiang decoction, the effective components of the traditional Chinese medicine, the action mechanism of the traditional Chinese medicine and the like, a corresponding fingerprint map control method needs to be established, but in the prior art, no quick, simple, convenient and accurate analysis method is suitable for detecting the related information of the number, relative position and the like of each chemical component of the traditional Chinese medicine shengqiang decoction. Therefore, it is necessary to establish a fingerprint for determining the Chinese medicine shengqiang decoction by High Performance Liquid Chromatography (HPLC).
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a method for measuring the fingerprint of the traditional Chinese medicine shengqiang decoction, which is quick, simple, convenient, comprehensive, accurate and reliable and is suitable for detecting the fingerprint of the shengqiang decoction.
The invention provides a method for determining traditional Chinese medicine shengqiang decoction fingerprint, which adopts high performance liquid chromatography, and the chromatographic conditions comprise: performing gradient elution by using an octadecylsilane chemically bonded silica chromatographic column, acetonitrile or methanol as a mobile phase A, a phosphate buffer aqueous solution as a mobile phase B and a DAD (digital data acquisition) detector as the detector;
the gradient elution procedure was: the volume ratio of the mobile phase A to the mobile phase B is from 5: 95 is gradually changed to 8 at a constant speed: 92; the volume ratio of the mobile phase A to the mobile phase B is from 8: 92, gradually changing to 13 at a constant speed: 87; the volume ratio of the mobile phase A to the mobile phase B is from 13: 87 is gradually changed to 20: 80; the volume ratio of the mobile phase A to the mobile phase B is from 20: 80, gradually changing to 30: 70; and within 70-95min, the volume ratio of the mobile phase A to the mobile phase B is 30: 70; the volume ratio of the mobile phase A to the mobile phase B is from 30: 70, gradually changing to 5 at a constant speed: 95; within 100-: 95.
preferably, the chromatographic column is 250mm in length and 4.6mm in diameter.
Preferably, the octadecylsilane chemically bonded silica of the column has a particle size of 2-10 μm.
Preferably, the octadecylsilane chemically bonded silica particle size of the column may be 2, 3, 4, 5, 6, 7, 8, 9 or 10 μm.
Preferably, the octadecylsilane chemically bonded silica particle size of the column is 5 μm.
Octadecylsilane bonded silica chromatographic columns are commercially available in a variety of brands, such as: elet Supersil ODS2, Shim-pack VP-ODS, etc.
Preferably, the aqueous phosphate buffer solution is an aqueous potassium dihydrogen phosphate-phosphate buffer solution.
Preferably, the volume fraction of phosphoric acid in the aqueous phosphate buffer is 0.01-0.5%.
Preferably, the volume fraction of phosphoric acid in the aqueous phosphate buffer solution may be 0.01, 0.05, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.1, 1.2, 1.3, 1.4 or 1.5%.
Preferably, the volume fraction of phosphoric acid in the aqueous phosphate buffer is 0.1%.
Preferably, the concentration of the monopotassium phosphate in the phosphate buffer aqueous solution is 0.01-0.5 mol/L.
Preferably, the concentration of monopotassium phosphate in the aqueous phosphate buffer solution can be 0.01, 0.02, 0.03, 0.04, 0.05, 0.1, 0.2, 0.3, 0.4 or 0.5 mol/L.
Preferably, the concentration of the monopotassium phosphate in the phosphate buffer aqueous solution is 0.02 mol/L.
Preferably, mobile phase a is acetonitrile.
Preferably, the flow rate is 0.5-1.5 ml/min.
Preferably, the flow rate may be 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.1, 1.2, 1.3, 1.4 or 1.5 ml/min.
Preferably, the flow rate is 1.0 ml/min.
Preferably, the column temperature is 20-40 ℃.
Preferably, the column temperature may be 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, or 40 ℃.
Preferably, the column temperature is 35 ℃.
Preferably, the detection wavelength is 200-220 nm.
Preferably, the detection wavelength may be 200, 201, 202, 203, 204, 205, 206, 207, 208, 209, 210, 211, 212, 213, 214, 215, 216, 217, 218, 219 or 220 nm.
Preferably, the detection wavelength is 210 nm.
Preferably, the sample size is 15-25. mu.L.
Preferably, the sample size may be 15, 16, 17, 18, 19, 20, 21, 22, 23, 24 or 25 μ L.
Preferably, the sample size is 20 μ L.
Preferably, the specific steps of the assay are: preparing a test solution and a reference medicinal solution, sequentially injecting samples, and recording a chromatogram.
Preferably, the control medicinal materials are radix astragali, rhizoma anemarrhenae, cimicifugae rhizoma, radix Platycodi and bupleuri radix.
The preparation method of the test solution comprises the following steps: collecting the dry extract powder of SHENGQIANG decoction, adding methanol, ultrasonic treating for 25-35min, shaking, cooling, and filtering to obtain filtrate to obtain sample solution.
Preferably, the preparation method of the reference medicinal material solution comprises the following steps: weighing dry extract powder of control medicinal material, adding methanol, ultrasonic treating for 25-35min, shaking, cooling, and filtering to obtain filtrate as control medicinal material solution.
The preparation method of the control medicinal material dry extract powder and the Shengxiao decoction dry extract powder is the same.
The dry paste powder is the conventional term in the field.
The inventors have performed gradient elution studies on a plurality of mobile phases, respectively, and each mobile phase is shown in table 1:
table 1 list of mobile phases
Remarking: the gradient elution procedure for the mobile phase was the same.
The inventor of the present invention, through performing gradient elution tests on the above-mentioned multiple mobile phases, finds that acetonitrile is used as mobile phase a and phosphate buffer aqueous solution is used as mobile phase B, wherein the volume fraction of phosphoric acid is 0.1%, and the concentration of potassium dihydrogen phosphate is 0.02mol/L, so that the characteristic chromatographic peaks of the trapping liquid can be well separated, and the peaks have symmetrical peak shapes, and the measurement results are shown in fig. 1 and table 2:
TABLE 2 measurement results of the fingerprint of Shengxiao decoction
From the above table, 14 chromatographic peaks were detected in the shengjun decoction, wherein peaks 6, 9 and 12 are exclusive peaks of raw astragalus, peaks 3, 4, 5 and 9 are exclusive peaks of rhizoma anemarrhenae, peaks 7, 10 and 11 are exclusive peaks of cimicifugae foetidae, peak 2 is exclusive peak of platycodon grandiflorum, and no exclusive peak of bupleurum chinense was detected.
Compared with the prior art, the invention has the following beneficial effects:
the method comprehensively considers the comprehensive influence of the chromatographic column, fluidity, flow rate, column temperature and gradient elution procedures on separation detection, optimizes the detection result, has the advantages of rapidness, simplicity, convenience, comprehensiveness, accuracy and reliability, and is suitable for detecting the fingerprint of the Shangqiang decoction; the method is characterized in that the method has more peaks and good peak shape when the method is measured at the wavelength of 200-220nm, can clearly present the exclusive characteristic peaks of the raw astragalus, the rhizoma anemarrhenae, the platycodon grandiflorum and the rhizoma cimicifugae, is easy to identify, has high technical content of the established fingerprint, completely reflects information, avoids the singleness and one-sidedness of the quality control of the Chinese medicinal Shengxian decoction, and can effectively reflect the quality of the Chinese medicinal Shengxian decoction; the quality of the Chinese medicine shengqiang decoction can be effectively evaluated by the existence of special peaks of raw astragalus, rhizoma anemarrhenae, platycodon grandiflorum and rhizoma cimicifugae in the fingerprint, and the stability of the quality of the medicinal materials and the effectiveness and safety of clinical medication are ensured.
Drawings
FIG. 1 is the fingerprint of the Shengxiao decoction measured in example 1 of the present invention.
FIG. 2 is the fingerprint of the control Astragalus membranaceus drug measured in example 1 of the present invention.
FIG. 3 is a fingerprint of a rhizoma anemarrhenae reference drug measured in example 1 of the present invention.
FIG. 4 shows the fingerprint of the drug for reference drug of Cimicifuga foetida obtained in example 1 of the present invention.
FIG. 5 shows the measured fingerprint of the reference radix Platycodi drug in example 1 of the present invention.
FIG. 6 shows the measured fingerprint of the radix bupleuri reference drug in example 1 of the present invention.
FIG. 7 is the fingerprint of the shengxi decoction obtained in example 2 of the present invention.
FIG. 8 is the fingerprint of the shengxi decoction obtained in example 3 of the present invention.
FIG. 9 is the fingerprint of the shengxi decoction obtained in example 4 of the present invention.
FIG. 10 is the fingerprint of the shengxi decoction obtained in example 5 of the present invention.
FIG. 11 is the fingerprint of the shengxi decoction obtained in example 6 of the present invention.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A method for measuring fingerprint of Chinese medicinal SHENGQIAOTANG adopts high performance liquid chromatography, and its chromatographic conditions include: the chromatographic column is an octadecylsilane chemically bonded silica chromatographic column (250 multiplied by 4.6mm, 5 mu m), acetonitrile is taken as a mobile phase A, phosphate buffer aqueous solution is taken as a mobile phase B, wherein the volume fraction of phosphoric acid is 0.1%, the concentration of potassium dihydrogen phosphate is 0.02mol/L, the detector is a DAD detector, the detection wavelength is 210nm, the flow rate is 1.0ml/min, the column temperature is 35 ℃, and gradient elution is carried out;
the gradient elution procedure was: the volume ratio of the mobile phase A to the mobile phase B is from 5: 95 is gradually changed to 8 at a constant speed: 92; the volume ratio of the mobile phase A to the mobile phase B is from 8: 92, gradually changing to 13 at a constant speed: 87; the volume ratio of the mobile phase A to the mobile phase B is from 13: 87 is gradually changed to 20: 80; the volume ratio of the mobile phase A to the mobile phase B is from 20: 80, gradually changing to 30: 70; and within 70-95min, the volume ratio of the mobile phase A to the mobile phase B is 30: 70; the volume ratio of the mobile phase A to the mobile phase B is from 30: 70, gradually changing to 5 at a constant speed: 95; within 100-: 95.
solution preparation:
raw astragalus root control solution: weighing 1g of radix astragali control medicinal material, preparing into radix astragali control medicinal material dry extract powder according to the preparation process of the Shengxian decoction dry extract powder, adding 10mL of methanol, performing ultrasound for 30min, shaking up, cooling, and filtering to obtain a subsequent filtrate to obtain radix astragali control medicinal material solution.
Rhizoma anemarrhenae reference medicinal material solution: weighing 1g of rhizoma anemarrhenae reference medicinal material, preparing rhizoma anemarrhenae reference medicinal material dry extract powder according to the preparation process of the shengqiang decoction dry extract powder, adding 10mL of methanol, performing ultrasonic treatment for 45min, shaking up, cooling, and filtering to obtain a subsequent filtrate to obtain a rhizoma anemarrhenae reference medicinal material solution.
Cimicifugae foetidae reference medicinal material solution: weighing 1g of rhizoma cimicifugae control medicinal material, preparing into rhizoma cimicifugae control medicinal material dry extract powder according to the preparation process of the above decoction, adding 10mL of methanol, performing ultrasound for 45min, shaking, cooling, and filtering to obtain filtrate to obtain rhizoma cimicifugae control medicinal material solution.
And (3) reference platycodon root medicinal material solution: weighing 1g of radix Platycodi reference material, preparing into radix Platycodi reference material dry extract powder according to the preparation process of Shengxiao decoction dry extract powder, adding 10mL of methanol, ultrasonic treating for 45min, shaking, cooling, and filtering to obtain the filtrate to obtain radix Platycodi reference material solution.
Bupleurum root reference medicinal solution: weighing 1g of radix bupleuri control medicinal material, preparing into radix bupleuri control medicinal material dry extract powder according to the preparation process of the shengwang decoction dry extract powder, adding 10mL of methanol, performing ultrasonic treatment for 45min, shaking up, cooling, and filtering to obtain a subsequent filtrate to obtain radix bupleuri control medicinal material solution.
Test solution: collecting 1.5g of the Shengxian decoction dry extract powder, adding 20mL of methanol, performing ultrasonic treatment for 45min, shaking up, cooling, and filtering to obtain a subsequent filtrate to obtain a test solution.
The ultrasonic power is 500W and 40 KHz.
And (3) test operation: and sequentially sampling 20 mu L of each control solution and sample solution, and recording chromatograms.
Typical patterns are shown in figures 1-6, and figure 1 is the fingerprint of the shengxi decoction measured in example 1 of the invention; FIG. 2 is a fingerprint of a reference radix astragali obtained in example 1 of the present invention; FIG. 3 is a fingerprint of a rhizoma anemarrhenae reference drug measured in example 1 of the present invention; FIG. 4 shows the measured fingerprint of Cimicifuga foetida reference drug in example 1; FIG. 5 shows the measured fingerprint of the reference radix Platycodi drug in example 1 of the present invention; FIG. 6 is the measured fingerprint of the bupleurum root reference drug in example 1 of the present invention;
by comparing the fingerprint spectrums of the whole formula of the shengqiang decoction and a single medicinal material, the special peak numbers of the raw astragalus, the rhizoma anemarrhenae, the rhizoma cimicifugae and the platycodon grandiflorum and the retention time of the special peak numbers are as follows:
specific peak of raw astragalus: peak No. 6 (42.037min), peak No. 9 (59.587min), peak No. 12 (65.967 min);
dedicated peak of rhizoma anemarrhenae: peak 3 (23.943min), Peak 4 (30.435min), Peak 5 (31.793min), Peak 9 (59.947min)
The special peak of cimicifuga foetida: peak 7 (43.000min), peak 10 (57.493min), and peak 11 (63.207 min);
the special peak of platycodon grandiflorum: peak 2 (19.060 min);
no specific peak was detected in Bupleurum.
By adopting the detection method in the embodiment 1 of the invention and combining the figure 1, the detection of the Chinese medicinal Shengxiao decoction at the wavelength of 210nm has the advantages of more peaks, good peak shape, clear presentation of exclusive characteristic peaks of astragalus, rhizoma anemarrhenae, rhizoma cimicifugae and platycodon grandiflorum, easy identification, high technical content of the established fingerprint, complete reflected information, avoidance of the singleness and one-sidedness of the quality control of the Chinese medicinal Shengxiao decoction, and effective reflection of the quality of the Chinese medicinal Shengxiao decoction, thereby ensuring the stability of the quality of medicinal materials and the effectiveness and safety of clinical medication.
Example 2
A method for measuring fingerprint of Chinese medicinal SHENGQIAOTANG adopts high performance liquid chromatography, and its chromatographic conditions include: the chromatographic column is an octadecylsilane chemically bonded silica chromatographic column (250 multiplied by 4.6mm, 5 mu m), acetonitrile is taken as a mobile phase A, phosphoric acid aqueous solution with volume fractions of 0.2% is taken as a mobile phase B, the detector is a DAD detector, the detection wavelength is 210nm, the flow rate is 1.0ml/min, the column temperature is 35 ℃, and gradient elution is carried out; the gradient elution procedure was the same as in example 1.
Solution preparation and experimental procedures were the same as in example 1.
The typical spectrum is shown in FIG. 7, and FIG. 7 is the fingerprint of the shengxi decoction measured in example 2 of the present invention.
Example 3
A method for measuring fingerprint of Chinese medicinal SHENGQIAOTANG adopts high performance liquid chromatography, and its chromatographic conditions include: the chromatographic column is an octadecylsilane chemically bonded silica chromatographic column (250 multiplied by 4.6mm, 5 mu m), acetonitrile is taken as a mobile phase A, a mixed aqueous solution of phosphoric acid with volume fraction of 0.1% and tetrahydrofuran with volume fraction of 1% is taken as a mobile phase B, the detector is a DAD detector, the detection wavelength is 210nm, the flow rate is 1.0ml/min, the column temperature is 35 ℃, and gradient elution is carried out; the gradient elution procedure was the same as in example 1.
Solution preparation and experimental procedures were the same as in example 1.
The typical spectrum is shown in FIG. 8, and FIG. 8 is the fingerprint of the shengxi decoction measured in example 3 of the present invention.
Example 4
A method for measuring fingerprint of Chinese medicinal SHENGQIAOTANG adopts high performance liquid chromatography, and its chromatographic conditions include: the chromatographic column is an octadecylsilane chemically bonded silica chromatographic column (250 multiplied by 4.6mm, 5 mu m), methanol is taken as a mobile phase A, a phosphoric acid aqueous solution with the volume fraction of 0.5% is taken as a mobile phase B, the detector is a DAD detector, the detection wavelength is 210nm, the flow rate is 1.0ml/min, the column temperature is 35 ℃, and gradient elution is carried out; the gradient elution procedure was the same as in example 1.
Solution preparation and experimental procedures were the same as in example 1.
The typical spectrum is shown in FIG. 9, and FIG. 9 is the fingerprint of the shengxi decoction measured in example 4 of the present invention.
Example 5
A method for measuring fingerprint of Chinese medicinal SHENGQIAOTANG adopts high performance liquid chromatography, and its chromatographic conditions include: the chromatographic column was Shim-pack VP-ODS (250X 4.6mm, 5 μm), acetonitrile was used as mobile phase A, a phosphoric acid aqueous solution of 0.1% volume fraction was used as mobile phase B, the detector was a DAD detector, the detection wavelength was 210nm, the flow rate was 1.0ml/min, the column temperature was 35 ℃ and gradient elution was carried out; the gradient elution procedure was the same as in example 1.
Solution preparation and experimental procedures were the same as in example 1.
The typical pattern is shown in figure 10, and figure 10 is the fingerprint of the shengxi decoction measured in example 5 of the present invention.
Example 6
A method for measuring fingerprint of Chinese medicinal SHENGQIAOTANG adopts high performance liquid chromatography, and its chromatographic conditions include: the chromatographic column was Supersil ODS2 (250X 4.6mm, 5 μm), acetonitrile was used as mobile phase A, 0.1% phosphoric acid aqueous solution by volume fraction was used as mobile phase B, the detector was a DAD detector, the detection wavelength was 210nm, the flow rate was 1.0ml/min, the column temperature was 35 ℃ and gradient elution was carried out; the gradient elution procedure was the same as in example 1.
Solution preparation and experimental procedures were the same as in example 1.
The typical pattern is shown in figure 11, and figure 11 is the fingerprint of the shengxi decoction measured in example 6 of the present invention.
From fig. 7 to 11, it can be seen that none of the chromatographic conditions of examples 2 to 6 can separate the characteristic peaks of the liter-trapper well, and the chromatographic conditions of examples 2 to 6 are not suitable for detecting the fingerprint of the liter-trapper.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. A method for measuring fingerprint of traditional Chinese medicine shengqiang decoction is characterized in that high performance liquid chromatography is adopted, and the chromatographic conditions comprise: the chromatographic column is an octadecylsilane chemically bonded silica chromatographic column, acetonitrile is used as a mobile phase A, phosphate buffer aqueous solution is used as a mobile phase B, and a detector is a DAD detector for gradient elution;
wherein the phosphate buffer aqueous solution is a phosphoric acid-monopotassium phosphate buffer aqueous solution; in phosphate buffer aqueous solution, the volume fraction of phosphoric acid is 0.01-0.5%; in the phosphate buffer aqueous solution, the concentration of the monopotassium phosphate is 0.01-0.5 mol/L;
the gradient elution procedure was: the volume ratio of the mobile phase A to the mobile phase B is from 5: 95 is gradually changed to 8 at a constant speed: 92; the volume ratio of the mobile phase A to the mobile phase B is from 8: 92, gradually changing to 13 at a constant speed: 87; the volume ratio of the mobile phase A to the mobile phase B is from 13: 87 is gradually changed to 20: 80; the volume ratio of the mobile phase A to the mobile phase B is from 20: 80, gradually changing to 30: 70; and within 70-95min, the volume ratio of the mobile phase A to the mobile phase B is 30: 70; the volume ratio of the mobile phase A to the mobile phase B is from 30: 70, gradually changing to 5 at a constant speed: 95; within 100-: 95;
wherein the flow rate is 0.5-1.5 ml/min; the column temperature is 20-40 ℃; the detection wavelength is 200-220 nm.
2. The method for determining the fingerprint of shengtrapa decoction of traditional Chinese medicine according to claim 1, wherein the length of a chromatographic column is 250mm, and the diameter of the chromatographic column is 4.6 mm; the particle size of octadecylsilane chemically bonded silica of the chromatographic column is 2-10 μm.
3. The method for determining the fingerprint of the traditional Chinese medicine shengqiang decoction according to claim 1 or 2, wherein the volume fraction of phosphoric acid in the phosphate buffer aqueous solution is 0.1%; in the phosphate buffer aqueous solution, the concentration of potassium dihydrogen phosphate was 0.02 mol/L.
4. The method for determining the fingerprint of the traditional Chinese medicine shengtrapa decoction according to claim 1 or 2, wherein the flow rate is 1.0 ml/min.
5. The method for determining the fingerprint of the traditional Chinese medicine shengqiang decoction according to claim 1 or 2, wherein the column temperature is 35 ℃.
6. The method for determining the fingerprint of the shengqiang decoction according to claim 1 or 2, wherein the detection wavelength is 210 nm.
7. The method for determining the fingerprint of the traditional Chinese medicine shengtrapa decoction according to claim 1 or 2, wherein the sample size is 15-25 μ L.
8. The method for determining the fingerprint of the traditional Chinese medicine shengqiang decoction according to claim 1 or 2, which is characterized by comprising the following specific steps: preparing a test solution and a reference medicinal solution, sequentially injecting samples, and recording a chromatogram; the reference medicinal materials include radix astragali, rhizoma anemarrhenae, cimicifugae rhizoma, radix Platycodi and bupleuri radix.
9. The method for determining the fingerprint of the traditional Chinese medicine shengqiang decoction according to claim 8, wherein the preparation method of the test solution comprises the following steps: collecting the dry extract powder of SHENGQIANG decoction, adding methanol, ultrasonic treating for 25-35min, shaking, cooling, and filtering to obtain filtrate to obtain sample solution; the preparation method of the reference medicinal material solution comprises the following steps: weighing dry extract powder of control medicinal material, adding methanol, ultrasonic treating for 25-35min, shaking, cooling, and filtering to obtain filtrate as control medicinal material solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910196913.8A CN109828070B (en) | 2019-03-15 | 2019-03-15 | Method for determining fingerprint of traditional Chinese medicine shengqiang decoction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910196913.8A CN109828070B (en) | 2019-03-15 | 2019-03-15 | Method for determining fingerprint of traditional Chinese medicine shengqiang decoction |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109828070A CN109828070A (en) | 2019-05-31 |
| CN109828070B true CN109828070B (en) | 2021-05-04 |
Family
ID=66870148
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910196913.8A Active CN109828070B (en) | 2019-03-15 | 2019-03-15 | Method for determining fingerprint of traditional Chinese medicine shengqiang decoction |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109828070B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117969727A (en) * | 2024-01-27 | 2024-05-03 | 湖南易能生物医药有限公司 | Fingerprint construction method for flavonoid component in traditional Chinese medicine composition containing astragalus membranaceus and application of fingerprint construction method |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI285262B (en) * | 2005-06-20 | 2007-08-11 | Dev Center Biotechnology | Characteristic mass spectrum fingerprinting setting method and rapid identification method of Chinese herb medicine and prescription |
| CN108310190A (en) * | 2018-03-13 | 2018-07-24 | 华北理工大学 | A kind of Chinese medicine preparation and preparation method thereof for treating slow arrhythmia |
| CN108918696B (en) * | 2018-05-14 | 2021-07-27 | 广东省中医院 | Establishment method and quality control method of spleen-tonifying and lung-benefiting prescription fingerprint |
-
2019
- 2019-03-15 CN CN201910196913.8A patent/CN109828070B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN109828070A (en) | 2019-05-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111337589B (en) | Method for establishing orange-shell mixture HPLC fingerprint spectrum | |
| CN102138985B (en) | Quality control method of total glycosides single preparation of white paeony roots | |
| CN105806975B (en) | A kind of method for building up of Yinqiao San UPLC finger-print | |
| CN101991661B (en) | Method for detecting Chinese patent drug containing at least two of white paeony root, ginseng, salvia miltiorrhiza, sweet wormwood, liquorice and angelica sinensis | |
| CN107589191B (en) | Method for establishing and detecting HPLC (high Performance liquid chromatography) fingerprint spectrum of golden scallop oral liquid | |
| CN106353430A (en) | Qianliexin capsule quality evaluation method based on multi-index active ingredient measurement | |
| CN108872410A (en) | A kind of method for building up and its finger-print of lung-nourishing semifluid extract finger-print | |
| CN109828070B (en) | Method for determining fingerprint of traditional Chinese medicine shengqiang decoction | |
| CN104316613A (en) | Method for establishing fingerprint spectrum of wind-dispelling and detoxifying capsules | |
| CN107782811B (en) | Detection method of fingerprint of Qiling kidney-invigorating tablet | |
| CN111948330B (en) | Detection method of finger-print of Renzhu stomach-invigorating granules | |
| CN102133333A (en) | Quality control method for shenmai injection mass spectrum finger prints | |
| CN107576739A (en) | A kind of HPLC fingerprint atlas detection methods of LONGMU ZHUANGGU KELI | |
| CN111879884A (en) | Quality control method of Chinese medicinal preparation | |
| CN106290643A (en) | A kind of method of quality control of Chinese medicine Herba Schizonepetae anti-lung cancer activity composition | |
| CN114166958B (en) | Detection method of fingerprint of traditional Chinese medicine compound herba xanthil stomach-calming particles and application thereof | |
| CN106770785B (en) | A method of establishing the finger-print of madder rattan medicinal material | |
| CN105588888A (en) | Traditional Chinese medicine fingerprint spectrum quality control and measuring method | |
| CN108445125A (en) | The HPLC fingerprint atlas detection methods of pain-relieving and illness-eliminating capsule | |
| CN109142563A (en) | A kind of construction method of guilingji capsules UPLC finger-print and its application | |
| CN113189248B (en) | HPLC fingerprint construction and detection method of Yinhua Miyanling tablets | |
| CN103969353A (en) | Identification method for fingerprint spectrum of rhubarb-salvia miltiorrhiza extract | |
| CN102114094A (en) | Chromatographic fingerprint of cassia twig and Tuckahoe pharmaceutical composition and detection method and application thereof | |
| CN114113356A (en) | Fingerprint spectrum detection method of Xiaoyao pills | |
| CN101435801A (en) | Fingerprint pattern identifying method of ganoderma lucidum spore oil |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |