CN110398551B - Establishment method of ginseng fruit medicinal material fingerprint spectrum and standard fingerprint spectrum thereof - Google Patents
Establishment method of ginseng fruit medicinal material fingerprint spectrum and standard fingerprint spectrum thereof Download PDFInfo
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Abstract
The invention relates to the technical field of traditional Chinese medicine fingerprint spectrums, in particular to a ginseng fruit medicine fingerprint spectrum establishing method and a standard fingerprint spectrum thereof. The invention provides a method for establishing a ginseng fruit medicinal material fingerprint, which adopts methanol to extract a ginseng fruit medicinal material, then carries out high performance liquid chromatography analysis on the obtained extracting solution, establishes an HPLC fingerprint by selecting a proper mobile phase and controlling a gradient elution program, and combines with principal component analysis to better evaluate the quality of the ginseng fruit medicinal material to ensure the consistency of the quality of the ginseng fruit medicinal material; the method provided by the invention is simple and convenient to operate, accurate and reliable, can make up for the defects of the existing quality control technology, improves the quality control technology of the ginseng fruit medicinal material, avoids the singleness and limitation of quality control, provides scientific basis for the quality control of the ginseng fruit medicinal material, and lays a foundation for improving the quality control level of the ginseng fruit medicinal material.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine fingerprint spectrums, in particular to a ginseng fruit medicine fingerprint spectrum establishing method and a standard fingerprint spectrum thereof.
Background
Ginseng (Panax ginseng C.A. Meyer) is a perennial herb of Panax genus of Araliaceae, is mostly used as medicine with underground rhizome part, has sweet and slightly bitter taste and slightly warm nature, has the effects of invigorating primordial qi, recovering pulse, strengthening collapse, invigorating spleen, benefiting lung, promoting fluid production, nourishing blood, tranquilizing mind, and improving intelligence, and is mainly used for treating diseases such as weak body, desire to loose, cold limbs, little pulse, spleen deficiency, anorexia, lung deficiency, cough and asthma, body fluid deficiency, thirst, internal heat, diabetes, deficiency of both qi and blood, deficiency of qi due to chronic disease, palpitation, insomnia, impotence, cold womb and other diseases. The ginseng is one of important special products in China, is also a rare medicinal material running in China and abroad, is known as 'all grass king' and has the effective components of saponins and polysaccharides, and modern researches show that the saponins in the ginseng have obvious pharmacological activities of resisting tumors, resisting diabetes, resisting cardiovascular and cerebrovascular diseases, resisting inflammation, resisting epilepsy, resisting oxidation and the like.
Researches show that the effective components of the ginseng fruit are ginsenoside substances, the content of the ginseng fruit is about 4 times of that of underground rhizome parts, and meanwhile, the ginseng fruit is used as a raw material medicament to be prepared into various medicaments for clinical application based on the definite pharmacological activity of the ginsenoside substances, but the Chinese pharmacopoeia does not contain the related contents of ginseng fruit medicinal materials, and the medicinal materials do not have legal quality control standards at present. Therefore, a method for comprehensively, objectively and scientifically evaluating the quality of ginseng fruit medicinal materials is urgently needed.
Disclosure of Invention
The invention aims to provide a method for establishing a ginseng fruit medicinal material fingerprint and a standard fingerprint thereof.
The invention provides a method for establishing a ginseng fruit medicinal material fingerprint spectrum, which comprises the following steps:
providing a mixed reference solution, wherein the mixed reference solution comprises 12 saponin components, namely ginsenoside Re, ginsenoside Rb1, ginsenoside F3, ginsenoside Rg2, ginsenoside Rc, ginsenoside Rb2, ginsenoside Rb3, ginsenoside F1, ginsenoside Rd, ginsenoside F2, ginsenoside Rg3 and pseudo-ginsenoside Rh 2;
extracting a ginseng fruit medicinal material by using methanol to obtain an extracting solution;
respectively carrying out high performance liquid chromatography analysis on the mixed reference substance solution and the extracting solution, and taking a chromatographic peak of the mixed reference substance solution as a reference to obtain a ginseng fruit medicinal material fingerprint containing 12 common peaks;
the chromatographic conditions of the high performance liquid chromatography are as follows:
mobile phase: the mobile phase comprises a mobile phase A and a mobile phase B, wherein the mobile phase A is acetonitrile; the mobile phase B is a phosphoric acid aqueous solution, and the volume percentage of phosphoric acid in the mobile phase B is 0.2%;
gradient elution procedure:
increasing the mobile phase A from 15% to 31% and reducing the mobile phase B from 85% to 69% in 0-15 min;
15-25 min, keeping the mobile phase A at 31% and the mobile phase B at 69%;
increasing the mobile phase A from 31% to 37% and reducing the mobile phase B from 69% to 63% in 25-35 min;
increasing the mobile phase A from 37% to 45% and reducing the mobile phase B from 63% to 55% in 35-45 min;
increasing the mobile phase A from 45% to 60% and reducing the mobile phase B from 55% to 40% in 45-60 min;
a detector: a diode array detector.
Preferably, the extraction is performed under ultrasonic conditions; the power of the ultrasonic wave is 200-300W, and the frequency is 35-45 kHz.
Preferably, the extraction time is 30-40 min.
Preferably, the dosage ratio of the methanol to the ginseng fruit medicinal materials is (15-25) mL: 0.1 g.
Preferably, the flow rate of the mobile phase is 0.8-1.2 mL/min.
Preferably, the detection wavelength when performing the high performance liquid chromatography is 203 nm.
Preferably, the high performance liquid chromatography is performed using a column
Omega Polar C18 chromatography column; the specification of the chromatographic column is as follows: the length was 250mm, the inner diameter was 4.6mm, and the filler particle size was 5 μm.
Preferably, the column temperature for the HPLC analysis is 30 to 35 ℃.
Preferably, the sample injection volume for performing the high performance liquid chromatography is 5-40 μ L.
The invention provides a ginseng fruit medicinal material standard fingerprint obtained by the establishment method of the ginseng fruit medicinal material fingerprint in the technical scheme, which comprises 12 common peaks, wherein the peak 1 is ginsenoside Re; peak 2 is ginsenoside Rb 1; peak 3 is ginsenoside F3; peak 4 is ginsenoside Rg 2; the No. 5 peak is ginsenoside Rc; peak No. 6 is ginsenoside Rb 2; peak 7 is ginsenoside Rb 3; peak 8 is ginsenoside F1; peak 9 is ginsenoside Rd; peak 10 is ginsenoside F2; peak 11 is ginsenoside Rg 3; the peak 12 is pseudoginsenoside Rh 2.
The invention provides a method for establishing a ginseng fruit medicinal material fingerprint, which adopts methanol to extract a ginseng fruit medicinal material, then carries out high performance liquid chromatography analysis on the obtained extracting solution, establishes an HPLC fingerprint by selecting a proper mobile phase and controlling a gradient elution program, and combines with principal component analysis to better evaluate the quality of the ginseng fruit medicinal material to ensure the consistency of the quality of the ginseng fruit medicinal material; the method provided by the invention is simple and convenient to operate, accurate and reliable, can make up for the defects of the existing quality control technology, improves the quality control technology of the ginseng fruit medicinal material, avoids the singleness and limitation of quality control, provides scientific basis for the quality control of the ginseng fruit medicinal material, and lays a foundation for improving the quality control level of the ginseng fruit medicinal material.
Drawings
FIG. 1 is a fingerprint of a ginseng fruit drug;
FIG. 2 shows fingerprints of 40 batches of ginseng fruit medicinal materials.
Detailed Description
The invention provides a method for establishing a ginseng fruit medicinal material fingerprint spectrum, which comprises the following steps:
providing a mixed reference solution, wherein the mixed reference solution comprises 12 saponin components, namely ginsenoside Re, ginsenoside Rb1, ginsenoside F3, ginsenoside Rg2, ginsenoside Rc, ginsenoside Rb2, ginsenoside Rb3, ginsenoside F1, ginsenoside Rd, ginsenoside F2, ginsenoside Rg3 and pseudo-ginsenoside Rh 2;
extracting a ginseng fruit medicinal material by using methanol to obtain an extracting solution;
respectively carrying out high performance liquid chromatography analysis on the mixed reference substance solution and the extracting solution, and taking a chromatographic peak of the mixed reference substance solution as a reference to obtain a ginseng fruit medicinal material fingerprint containing 12 common peaks;
the chromatographic conditions of the high performance liquid chromatography are as follows:
mobile phase: the mobile phase comprises a mobile phase A and a mobile phase B, wherein the mobile phase A is acetonitrile; the mobile phase B is a phosphoric acid aqueous solution, and the volume percentage of phosphoric acid in the mobile phase B is 0.2%;
gradient elution procedure:
increasing the mobile phase A from 15% to 31% and reducing the mobile phase B from 85% to 69% in 0-15 min;
15-25 min, keeping the mobile phase A at 31% and the mobile phase B at 69%;
increasing the mobile phase A from 31% to 37% and reducing the mobile phase B from 69% to 63% in 25-35 min;
increasing the mobile phase A from 37% to 45% and reducing the mobile phase B from 63% to 55% in 35-45 min;
increasing the mobile phase A from 45% to 60% and reducing the mobile phase B from 55% to 40% in 45-60 min;
a detector: a diode array detector.
The invention provides a mixed reference substance solution, which comprises 12 saponin components, namely ginsenoside Re, ginsenoside Rb1, ginsenoside F3, ginsenoside Rg2, ginsenoside Rc, ginsenoside Rb2, ginsenoside Rb3, ginsenoside F1, ginsenoside Rd, ginsenoside F2, ginsenoside Rg3 and pseudo-ginsenoside Rh 2. The kind of the solvent in the mixed control solution is not particularly limited in the present invention, and a solvent for preparing the mixed control solution, which is well known to those skilled in the art, may be used. In the examples of the present invention, methanol is specifically used as a solvent.
The method for preparing the mixed reference solution is not particularly limited in the present invention, and the solution preparation method known to those skilled in the art may be adopted. In the embodiment of the invention, a proper amount of 12 saponin component reference substances are respectively taken, precisely weighed, prepared into a mixed reference substance solution by using methanol, filtered by a 0.22 mu m microporous filter membrane, and the subsequent filtrate is taken and stored at 4 ℃ in a sealed manner.
The invention adopts methanol to extract the ginseng fruit medicinal material to obtain the extracting solution. In the invention, the ginseng fruit medicinal material is preferably used in the form of ginseng fruit medicinal material powder, and specifically, the ginseng fruit medicinal material powder is sieved by a 40-mesh sieve, and the sieved part is taken for subsequent extraction. In the invention, the dosage ratio of the methanol to the ginseng fruit medicinal materials is preferably (15-25) mL: 0.1g, more preferably (20 to 25) mL: 0.1 g.
In the present invention, the extraction is preferably performed under ultrasonic conditions; the power of the ultrasonic wave is preferably 200-300W, and more preferably 250-300W; the frequency of the ultrasonic wave is preferably 35-45 kHz, and more preferably 40-45 kHz; the extraction time is preferably 30-40 min, and more preferably 30-35 min.
In the embodiment of the invention, about 0.1g of ginseng fruit medicinal material powder (sieved part after being sieved by a 40-mesh sieve) is precisely weighed and placed in a 50mL conical flask; precisely adding 15-25 mL of methanol, weighing, extracting for 30-40 min under the ultrasonic condition of 200-300W and 35-45 kHz, standing to room temperature, complementing the lost weight with methanol, uniformly mixing, filtering with a 0.22 mu m filter membrane, and taking the subsequent filtrate to obtain the extracting solution.
Respectively carrying out high performance liquid chromatography analysis on the mixed reference substance solution and the extracting solution, and taking a chromatographic peak of the mixed reference substance solution as a reference to obtain a ginseng fruit medicinal material fingerprint containing 12 common peaks;
the chromatographic conditions of the high performance liquid chromatography are as follows:
mobile phase: the mobile phase comprises a mobile phase A and a mobile phase B, wherein the mobile phase A is acetonitrile; the mobile phase B is a phosphoric acid aqueous solution, and the volume percentage of phosphoric acid in the mobile phase B is 0.2%;
gradient elution procedure:
increasing the mobile phase A from 15% to 31% and reducing the mobile phase B from 85% to 69% in 0-15 min;
15-25 min, keeping the mobile phase A at 31% and the mobile phase B at 69%;
increasing the mobile phase A from 31% to 37% and reducing the mobile phase B from 69% to 63% in 25-35 min;
increasing the mobile phase A from 37% to 45% and reducing the mobile phase B from 63% to 55% in 35-45 min;
increasing the mobile phase A from 45% to 60% and reducing the mobile phase B from 55% to 40% in 45-60 min;
a detector: a diode array detector.
In the invention, the flow rate of the mobile phase is preferably 0.8-1.2 mL/min, and more preferably 1.0 mL/min.
In the present invention, the detection wavelength in the high performance liquid chromatography is preferably 203 nm.
In the present invention, the column used for the high performance liquid chromatography is preferably a column used for the high performance liquid chromatography
Omega polar C18 chromatography column; the specification of the chromatographic column is preferably: the length was 250mm, the inner diameter was 4.6mm, and the filler particle size was 5 μm.
In the present invention, the column temperature for performing the high performance liquid chromatography is preferably 30 to 35 ℃, and more preferably 35 ℃.
In the present invention, the volume of sample injection for the HPLC analysis is preferably 5 to 40. mu.L, and more preferably 10 to 20. mu.L.
The invention provides a ginseng fruit medicinal material standard fingerprint obtained by adopting the establishment method of the ginseng fruit medicinal material fingerprint in the technical scheme, which comprises 12 common peaks, wherein the peak 1 is ginsenoside Re; peak 2 is ginsenoside Rb 1; peak 3 is ginsenoside F3; peak 4 is ginsenoside Rg 2; the No. 5 peak is ginsenoside Rc; peak No. 6 is ginsenoside Rb 2; peak 7 is ginsenoside Rb 3; peak 8 is ginsenoside F1; peak 9 is ginsenoside Rd; peak 10 is ginsenoside F2; peak 11 is ginsenoside Rg 3; the peak 12 is pseudoginsenoside Rh 2.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Experimental materials:
40 batches of ginseng fruit medicinal materials are collected from different areas of white mountain city in Jilin province in 2017 and 8 months, and specific sample information is shown in table 1:
sample information for Table 140 batches of ginseng fruit medicinal materials
(2) Instruments and reagents:
high performance liquid chromatograph: waters 2695 high performance liquid chromatograph (Waters corporation, usa); waters2996PDA diode array Detector (Waters corporation, USA); empower chromatography workstation (Waters corporation, usa); mettler ab135-S (mettler-toledo instruments (shanghai) ltd); the assay was chromatographically pure (Sigma) with acetonitrile.
The rest reagents are analytically pure (Beijing chemical reagent factory); the water was double distilled, prepared by a Millipore pure water system (Millipore, Milford, MA, USA); ginsenoside Re (Ginsenoside Re, abbreviated as Re, lot: 110754-201626), Ginsenoside Rb1(Ginsenoside Rb1, abbreviated as Rb1, lot: 110704-201627), Ginsenoside Rg2(Ginsenoside Rg2, abbreviated as Rg2, lot: 111779-201601), Ginsenoside Rc (Ginsenoside Rc, abbreviated as Rc, lot: 11641-201602), Ginsenoside Rb2(Ginsenoside Rb2, abbreviated as Rb2, lot: 111715-201626), Ginsenoside Rb 8 (Ginsenoside Rb3, abbreviated as Rb3, lot: 1111111114), Ginsenoside F1(Ginsenoside F1, abbreviated as F1, abbreviated as F42, lot: 201603, lot: 20160762), lot: 20160110469-2016023, lot: 2016048, abbreviated as Ginsenoside F2, lot: 2016070-2016048, lot: 2016070-201604, 2016070-201609, 2016048, and lot: Ginsenoside Rg-2016048, ginsenoside F3(Ginsenoside F3, abbreviated as F3, batch number: MUST-18032311) and Pseudoginsenoside Rh2(Pseudoginsenoside Rh2, abbreviated as Rh2, batch number: MUST-18082801) controls were provided by Goodpasture Biotech limited, and the 12 saponin component controls were all more than 98% pure by HPLC analysis.
(3) Preparing a mixed reference substance solution:
respectively taking appropriate amount of 12 saponin components as reference substances, precisely weighing, preparing into mixed reference substance solution with methanol, filtering with 0.22 μm microporous membrane, collecting the filtrate, sealing, and storing at 4 deg.C.
(4) Preparation of extract (test solution):
taking about 0.1g of ginseng fruit medicinal material powder (sieved part after being sieved by a 40-mesh sieve), precisely weighing, and placing in a 50mL conical flask; precisely adding 20mL of methanol, weighing, extracting under ultrasonic condition of 250W and 30kHz for 30min, standing to room temperature, adding methanol to make up for the lost weight, mixing, filtering with 0.22 μm filter membrane, and collecting the filtrate to obtain extractive solution.
(5) Chromatographic conditions of high performance liquid chromatography:
mobile phase: the mobile phase comprises a mobile phase A and a mobile phase B, wherein the mobile phase A is acetonitrile; the mobile phase B is a phosphoric acid aqueous solution, and the volume percentage of phosphoric acid in the mobile phase B is 0.2%;
gradient elution procedure:
increasing the mobile phase A from 15% to 31% and reducing the mobile phase B from 85% to 69% in 0-15 min;
15-25 min, keeping the mobile phase A at 31% and the mobile phase B at 69%;
increasing the mobile phase A from 31% to 37% and reducing the mobile phase B from 69% to 63% in 25-35 min;
increasing the mobile phase A from 37% to 45% and reducing the mobile phase B from 63% to 55% in 35-45 min;
increasing the mobile phase A from 45% to 60% and reducing the mobile phase B from 55% to 40% in 45-60 min;
the flow rate of the mobile phase is 1.0 mL/min;
the detector is a diode array detector;
the detection wavelength is 203 nm;
the chromatographic column is
Omega Polar C18 chromatography column, specification: the length is 250mm, the inner diameter is 4.6mm, and the grain diameter of the filler is 5 mu m;
the column temperature was 35 ℃;
the injection volume was 10. mu.L.
(6) Precision investigation:
sampling herba Herminii sample solution continuously for 5 times according to the above chromatographic conditions, measuring peak area and retention time of each component, and calculating relative retention time and relative peak area. The results show that the relative retention time and RSD of the relative peak area are less than 3.0% for all chromatographic peaks, indicating good precision of the analytical method.
(7) Similarity analysis
The fingerprint of ginseng fruit is processed by software of a Chinese medicine chromatogram fingerprint similarity evaluation system (2004A version). Matching by using the spectrum of the sample of the number S1 as a comparison fingerprint (shown in figure 1), carrying out similarity evaluation analysis, and identifying and determining 12 chromatographic peaks shared by 40 samples by comparing with retention time in a chromatogram of a comparison product. In fig. 1, peak No. 1 is ginsenoside Re; peak 2 is ginsenoside Rb 1; peak 3 is ginsenoside F3; peak 4 is ginsenoside Rg 2; the No. 5 peak is ginsenoside Rc; peak No. 6 is ginsenoside Rb 2; peak 7 is ginsenoside Rb 3; peak 8 is ginsenoside F1; peak 9 is ginsenoside Rd; peak 10 is ginsenoside F2; peak 11 is ginsenoside Rg 3; the peak 12 is pseudoginsenoside Rh 2. Comparing 40 different batches of herba Herminii fingerprint (shown in figure 2) with the reference fingerprint to obtain similarity result.
And (4) analyzing similarity results, wherein the total peak area of each 40 batches of ginseng fruit medicinal materials accounts for more than 95% of the total peak area, and similarity evaluation results are relatively consistent and accord with the traditional Chinese medicine fingerprint standard.
The embodiment shows that the method provided by the invention is simple and convenient to operate, accurate and reliable, can make up the defects of the existing quality control technology, improves the quality control technology of the ginseng fruit medicinal material, avoids the singleness and limitation of quality control, provides scientific basis for the quality control of the ginseng fruit medicinal material, and lays a foundation for improving the quality control level of the ginseng fruit medicinal material.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (6)
1. A method for establishing a fingerprint of a ginseng fruit medicinal material is characterized by comprising the following steps:
providing a mixed reference solution, wherein the mixed reference solution comprises 12 saponin components, namely ginsenoside Re, ginsenoside Rb1, ginsenoside F3, ginsenoside Rg2, ginsenoside Rc, ginsenoside Rb2, ginsenoside Rb3, ginsenoside F1, ginsenoside Rd, ginsenoside F2, ginsenoside Rg3 and pseudo-ginsenoside Rh 2;
extracting a ginseng fruit medicinal material by using methanol to obtain an extracting solution; the extraction is carried out under ultrasonic conditions; the power of the ultrasonic wave is 200-300W, and the frequency is 35-45 kHz; the extraction time is 30-40 min; the dosage ratio of the methanol to the ginseng fruit medicinal materials is (15-25) mL: 0.1 g;
respectively carrying out high performance liquid chromatography analysis on the mixed reference substance solution and the extracting solution, and taking a chromatographic peak of the mixed reference substance solution as a reference to obtain a ginseng fruit medicinal material fingerprint containing 12 common peaks;
the chromatographic conditions of the high performance liquid chromatography are as follows:
mobile phase: the mobile phase comprises a mobile phase A and a mobile phase B, wherein the mobile phase A is acetonitrile; the mobile phase B is a phosphoric acid aqueous solution, and the volume percentage of phosphoric acid in the mobile phase B is 0.2%;
gradient elution procedure:
increasing the mobile phase A from 15% to 31% and reducing the mobile phase B from 85% to 69% in 0-15 min;
15-25 min, keeping the mobile phase A at 31% and the mobile phase B at 69%;
increasing the mobile phase A from 31% to 37% and reducing the mobile phase B from 69% to 63% in 25-35 min;
increasing the mobile phase A from 37% to 45% and reducing the mobile phase B from 63% to 55% in 35-45 min;
increasing the mobile phase A from 45% to 60% and reducing the mobile phase B from 55% to 40% in 45-60 min;
a detector: a diode array detector;
the chromatographic column adopted for the high performance liquid chromatography is a Luna Omega C18 chromatographic column; the specification of the chromatographic column is as follows: the length is 250mm, the inner diameter is 4.6mm, and the grain size of the filler is 5 mu m.
2. The method for establishing the ginseng fruit medicinal material fingerprint spectrum according to claim 1, wherein the flow rate of the mobile phase is 0.8-1.2 mL/min.
3. The method for establishing the ginseng fruit medicinal material fingerprint spectrum according to claim 1, wherein the detection wavelength during the high performance liquid chromatography is 203 nm.
4. The method for establishing the ginseng fruit medicinal material fingerprint spectrum according to claim 1, wherein the column temperature during the high performance liquid chromatography is 30-35 ℃.
5. The method for establishing the ginseng fruit medicinal material fingerprint spectrum according to claim 1, wherein the sample injection volume during the high performance liquid chromatography is 5-40 μ L.
6. The standard fingerprint of the ginseng fruit medicinal material obtained by the establishing method of the fingerprint of the ginseng fruit medicinal material according to any one of claims 1 to 5 is characterized by comprising 12 common peaks, wherein the peak 1 is ginsenoside Re; peak 2 is ginsenoside Rb 1; peak 3 is ginsenoside F3; peak 4 is ginsenoside Rg 2; the No. 5 peak is ginsenoside Rc; peak No. 6 is ginsenoside Rb 2; peak 7 is ginsenoside Rb 3; peak 8 is ginsenoside F1; peak 9 is ginsenoside Rd; peak 10 is ginsenoside F2; peak 11 is ginsenoside Rg 3; the peak 12 is pseudoginsenoside Rh 2.
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