CN110398551A - A kind of method for building up and its standard finger-print of panax ginseng fruit medicinal materials fingerprint - Google Patents

A kind of method for building up and its standard finger-print of panax ginseng fruit medicinal materials fingerprint Download PDF

Info

Publication number
CN110398551A
CN110398551A CN201910654262.2A CN201910654262A CN110398551A CN 110398551 A CN110398551 A CN 110398551A CN 201910654262 A CN201910654262 A CN 201910654262A CN 110398551 A CN110398551 A CN 110398551A
Authority
CN
China
Prior art keywords
ginsenoside
mobile phase
panax ginseng
ginseng fruit
peaks
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201910654262.2A
Other languages
Chinese (zh)
Other versions
CN110398551B (en
Inventor
刘建明
许旭东
吴海峰
佟晓乐
刘红
董新
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
JILIN JI'AN YISHENG PHARMACEUTICAL CO Ltd
Original Assignee
JILIN JI'AN YISHENG PHARMACEUTICAL CO Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by JILIN JI'AN YISHENG PHARMACEUTICAL CO Ltd filed Critical JILIN JI'AN YISHENG PHARMACEUTICAL CO Ltd
Priority to CN201910654262.2A priority Critical patent/CN110398551B/en
Publication of CN110398551A publication Critical patent/CN110398551A/en
Application granted granted Critical
Publication of CN110398551B publication Critical patent/CN110398551B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/26Conditioning of the fluid carrier; Flow patterns
    • G01N30/28Control of physical parameters of the fluid carrier
    • G01N30/36Control of physical parameters of the fluid carrier in high pressure liquid systems

Landscapes

  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Steroid Compounds (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The present invention relates to Fingerprint of Chinese medicine materia technical fields, and in particular to a kind of method for building up and its standard finger-print of panax ginseng fruit medicinal materials fingerprint.The present invention provides a kind of method for building up of panax ginseng fruit medicinal materials fingerprint, the present invention extracts panax ginseng fruit medicinal material using methanol, efficient liquid phase chromatographic analysis is carried out to gained extracting solution later, by selecting suitable mobile phase and controlling gradient elution program, establish HPLC finger-print, the quality of panax ginseng fruit medicinal material is preferably evaluated in conjunction with principal component analysis, it is ensured that panax ginseng fruit quality of medicinal material consistency;Method provided by the invention is easy to operate, accurately and reliably, it can make up for it the shortcoming of existing Quality Control Technology, keep panax ginseng fruit quality of medicinal material control technology more perfect, avoid the unicity and limitation of quality control, scientific basis is provided for the quality control of panax ginseng fruit medicinal material, is laid a good foundation to improve the quality control level of panax ginseng fruit medicinal material.

Description

A kind of method for building up and its standard finger-print of panax ginseng fruit medicinal materials fingerprint
Technical field
The present invention relates to Fingerprint of Chinese medicine materia technical fields, and in particular to a kind of foundation of panax ginseng fruit medicinal materials fingerprint Method and its standard finger-print.
Background technique
Ginseng (Panaxginseng C.A.Meyer) is Araliaceae Panax herbaceos perennial, mostly with underground rhizome Part is used as medicine, sweet in flavor, slight bitter, slightly warm in nature, have reinforce vital energy, veins takes off admittedly, reinforce the spleen to benefit the lung, shengjin nourishing, tranquilize the mind and promote the intelligence etc. Effect, be chiefly used in it is physically weak to be taken off, cold weak pulse of limb, spleen eating less, the deficiency syndrome of the lung are breathed with cough, injury thirst, Heat Diabetes, deficiency of qi and blood, long The treatment of the illnesss such as sick empty thin, insomnia of palpitating with fear, impotence palace cold.Ginseng is one of important specialty in China, and the treasure having won fame both at home and abroad Precious medicinal material is known as " King of Herbs ", and effective component is mainly saponins and polysaccharose substance, modern research shows that ginseng Middle saponin component has significant antitumor, anti-diabetic, resisting cardiovascular disease, anti-inflammatory, anti-epileptic and the medicines such as anti-oxidant Reason activity.
Panax ginseng fruit is the ripening fruits of ginseng, and some researches show that effective component is Ginsenosides substance, and content is about It is 4 times of underground rhizome part, meanwhile, it is based on the specific pharmacological activity of ginsenoside substance, panax ginseng fruit is by as raw material A variety of medicinal applications are made in clinic in medicine, but " Chinese Pharmacopoeia " not yet records the related content of panax ginseng fruit medicinal material, and the medicinal material is current There is no legal quality control standard.Therefore, be badly in need of it is a kind of can it is comprehensive, objective, scientifically evaluate panax ginseng fruit quality of medicinal material Method.
Summary of the invention
The purpose of the present invention is to provide the method for building up and its standard finger-print of a kind of panax ginseng fruit medicinal materials fingerprint, Method provided by the invention is easy to operate, accurately and reliably, can make up for it the shortcoming of existing Quality Control Technology, makes panax ginseng fruit Quality of medicinal material control technology is more perfect.
The present invention provides a kind of method for building up of panax ginseng fruit medicinal materials fingerprint, comprising the following steps:
Mixed reference substance solution is provided, includes 12 kinds of saponin components, respectively ginseng in the mixed reference substance solution Saponin(e Re, ginsenoside Rb1, ginseng saponin F 3, ginsenoside Rg2, Ginsenoside Rc, ginsenoside Rb2, ginsenoside Rb3, Ginsenoside F1, ginsenoside Rd, Ginsenoside F2, ginseng sapoglycoside Rg 3 and pseudo-ginsenoside Rh2;
Panax ginseng fruit medicinal material is extracted using methanol, obtains extracting solution;
The mixed reference substance solution and extracting solution are subjected to efficient liquid phase chromatographic analysis respectively, with mixed reference substance solution Chromatographic peak on the basis of, obtain the panax ginseng fruit medicinal materials fingerprint containing 12 shared peaks;
The chromatographic condition of the high performance liquid chromatography are as follows:
Mobile phase: mobile phase includes mobile phase A and Mobile phase B, wherein mobile phase A is acetonitrile;Mobile phase B is phosphoric acid water Solution, the volumn concentration of phosphoric acid is 0.2% in the Mobile phase B;
Gradient elution program:
0~15min, mobile phase A increase to 31%, Mobile phase B by 15% and are reduced by 85% to 69%;
15~25min, mobile phase A keep 31%, Mobile phase B to keep 69%;
25~35min, mobile phase A increase to 37%, Mobile phase B by 31% and are reduced by 69% to 63%;
35~45min, mobile phase A increase to 45%, Mobile phase B by 37% and are reduced by 63% to 55%;
45~60min, mobile phase A increase to 60%, Mobile phase B by 45% and are reduced by 55% to 40%;
Detector: diode array detector.
Preferably, the extraction carries out under ultrasound condition;The power of the ultrasound be 200~300W, frequency be 35~ 45kHz。
Preferably, the time of the extraction is 30~40min.
Preferably, the amount ratio of the methanol and panax ginseng fruit medicinal material is (15~25) mL:0.1g.
Preferably, the flow velocity of the mobile phase is 0.8~1.2mL/min.
Preferably, Detection wavelength when carrying out the efficient liquid phase chromatographic analysis is 203nm.
Preferably, the chromatographic column used when carrying out the efficient liquid phase chromatographic analysis for Omega Polar C18 chromatographic column;The specification of the chromatographic column are as follows: a length of 250mm, internal diameter 4.6mm, packing material size are 5 μm.
Preferably, column temperature when carrying out the efficient liquid phase chromatographic analysis is 30~35 DEG C.
Preferably, sampling volume when carrying out the efficient liquid phase chromatographic analysis is 5~40 μ L.
The present invention provides the panax ginseng fruits that the method for building up of panax ginseng fruit medicinal materials fingerprint described in above-mentioned technical proposal obtains Medicinal material standard finger-print, including 12 shared peaks, No. 1 peak are ginsenoside Re;No. 2 peaks are ginsenoside Rb1;No. 3 peaks are Ginseng saponin F 3;No. 4 peaks are ginsenoside Rg2;No. 5 peaks are Ginsenoside Rc;No. 6 peaks are ginsenoside Rb2;It behaves at No. 7 peaks Join saponin(e Rb3;No. 8 peaks are Ginsenoside F1;No. 9 peaks are ginsenoside Rd;No. 10 peaks are Ginsenoside F2;No. 11 peaks are ginseng Saponin(e Rg3;No. 12 peaks are pseudo-ginsenoside Rh2.
The present invention provides a kind of method for building up of panax ginseng fruit medicinal materials fingerprint, and the present invention is using methanol to panax ginseng fruit medicine Material extracts, and carries out efficient liquid phase chromatographic analysis to gained extracting solution later, by selecting suitable mobile phase and controlling ladder Elution program is spent, HPLC finger-print is established, the quality of panax ginseng fruit medicinal material is preferably evaluated in conjunction with principal component analysis, it is ensured that people Join fruit quality of medicinal material consistency;Method provided by the invention is easy to operate, accurately and reliably, can make up for it existing Quality Control Technology Shortcoming, keep panax ginseng fruit quality of medicinal material control technology more perfect, avoid quality control unicity and limitation, be people The quality control for joining fruit medicinal material provides scientific basis, lays a good foundation to improve the quality control level of panax ginseng fruit medicinal material.
Detailed description of the invention
Fig. 1 is panax ginseng fruit medicinal material reference fingerprint;
Fig. 2 is 40 batches of panax ginseng fruit medicinal materials fingerprints.
Specific embodiment
The present invention provides a kind of method for building up of panax ginseng fruit medicinal materials fingerprint, comprising the following steps:
Mixed reference substance solution is provided, includes 12 kinds of saponin components, respectively ginseng in the mixed reference substance solution Saponin(e Re, ginsenoside Rb1, ginseng saponin F 3, ginsenoside Rg2, Ginsenoside Rc, ginsenoside Rb2, ginsenoside Rb3, Ginsenoside F1, ginsenoside Rd, Ginsenoside F2, ginseng sapoglycoside Rg 3 and pseudo-ginsenoside Rh2;
Panax ginseng fruit medicinal material is extracted using methanol, obtains extracting solution;
The mixed reference substance solution and extracting solution are subjected to efficient liquid phase chromatographic analysis respectively, with mixed reference substance solution Chromatographic peak on the basis of, obtain the panax ginseng fruit medicinal materials fingerprint containing 12 shared peaks;
The chromatographic condition of the high performance liquid chromatography are as follows:
Mobile phase: mobile phase includes mobile phase A and Mobile phase B, wherein mobile phase A is acetonitrile;Mobile phase B is phosphoric acid water Solution, the volumn concentration of phosphoric acid is 0.2% in the Mobile phase B;
Gradient elution program:
0~15min, mobile phase A increase to 31%, Mobile phase B by 15% and are reduced by 85% to 69%;
15~25min, mobile phase A keep 31%, Mobile phase B to keep 69%;
25~35min, mobile phase A increase to 37%, Mobile phase B by 31% and are reduced by 69% to 63%;
35~45min, mobile phase A increase to 45%, Mobile phase B by 37% and are reduced by 63% to 55%;
45~60min, mobile phase A increase to 60%, Mobile phase B by 45% and are reduced by 55% to 40%;
Detector: diode array detector.
The present invention provides mixed reference substance solution, includes 12 kinds of saponin components in the mixed reference substance solution, respectively For ginsenoside Re, ginsenoside Rb1, ginseng saponin F 3, ginsenoside Rg2, Ginsenoside Rc, ginsenoside Rb2, ginseng soap Glycosides Rb3, Ginsenoside F1, ginsenoside Rd, Ginsenoside F2, ginseng sapoglycoside Rg 3 and pseudo-ginsenoside Rh2.The present invention for The type of solvent does not have special restriction in mixed reference substance solution, using well known to those skilled in the art described for preparing The solvent of mixed reference substance solution.In an embodiment of the present invention, specifically using methanol as solvent.
The present invention does not have special restriction for the method for preparing mixed reference substance solution, ripe using those skilled in the art The technical solution for the preparation solution known.In an embodiment of the present invention, 12 kinds of saponin component controls are specifically taken respectively Appropriate product, it is accurately weighed, it is configured to mixed reference substance solution with methanol, crosses 0.22 μm of miillpore filter, takes subsequent filtrate, seals 4 DEG C It saves.
The present invention extracts panax ginseng fruit medicinal material using methanol, obtains extracting solution.In the present invention, the panax ginseng fruit medicine Material uses preferably in the form of panax ginseng fruit medicinal powder, and panax ginseng fruit medicinal powder is specifically crossed 40 meshes, and lower part of screen point is taken to carry out Subsequent extracted.In the present invention, the amount ratio of the methanol and panax ginseng fruit medicinal material is preferably (15~25) mL:0.1g, more preferably For (20~25) mL:0.1g.
In the present invention, the extraction preferably carries out under ultrasound condition;The power of the ultrasound is preferably 200~ 300W, more preferably 250~300W;The frequency of the ultrasound is preferably 35~45kHz, more preferably 40~45kHz;It is described to mention The time taken is preferably 30~40min, more preferably 30~35min.
In an embodiment of the present invention, panax ginseng fruit medicinal powder (lower part of screen point after crossing 40 meshes) is specifically taken about 0.1g, it is accurately weighed, it is placed in 50mL conical flask;Precision be added 15~25mL of methanol, it is weighed, 200~300W, 35~ 30~40min is extracted under 45kHz ultrasound condition, stands to room temperature, the weight of less loss is supplied with methanol, is mixed, 0.22 μm of filter membrane Filtering, takes subsequent filtrate to get extracting solution.
The mixed reference substance solution and extracting solution are carried out efficient liquid phase chromatographic analysis by the present invention respectively, to mix control On the basis of the chromatographic peak of product solution, the panax ginseng fruit medicinal materials fingerprint containing 12 shared peaks is obtained;
The chromatographic condition of the high performance liquid chromatography are as follows:
Mobile phase: mobile phase includes mobile phase A and Mobile phase B, wherein mobile phase A is acetonitrile;Mobile phase B is phosphoric acid water Solution, the volumn concentration of phosphoric acid is 0.2% in the Mobile phase B;
Gradient elution program:
0~15min, mobile phase A increase to 31%, Mobile phase B by 15% and are reduced by 85% to 69%;
15~25min, mobile phase A keep 31%, Mobile phase B to keep 69%;
25~35min, mobile phase A increase to 37%, Mobile phase B by 31% and are reduced by 69% to 63%;
35~45min, mobile phase A increase to 45%, Mobile phase B by 37% and are reduced by 63% to 55%;
45~60min, mobile phase A increase to 60%, Mobile phase B by 45% and are reduced by 55% to 40%;
Detector: diode array detector.
In the present invention, the flow velocity of the mobile phase is preferably 0.8~1.2mL/min, more preferably 1.0mL/min.
In the present invention, Detection wavelength when carrying out the efficient liquid phase chromatographic analysis is preferably 203nm.
In the present invention, the chromatographic column used when carrying out the efficient liquid phase chromatographic analysis is preferably OmegaPolar C18 chromatographic column;The specification of the chromatographic column is preferred are as follows: a length of 250mm, internal diameter 4.6mm, packing material size 5 μm。
In the present invention, column temperature when carrying out the efficient liquid phase chromatographic analysis is preferably 30~35 DEG C, more preferably 35 ℃。
In the present invention, sampling volume when carrying out the efficient liquid phase chromatographic analysis is preferably 5~40 μ L, more preferably 10~20 μ L.
The present invention provides the people that the method for building up of the panax ginseng fruit medicinal materials fingerprint by adopting the above technical scheme obtains Join fruit medicinal material standard finger-print, including 12 shared peaks, No. 1 peak is ginsenoside Re;No. 2 peaks are ginsenoside Rb1;No. 3 Peak is ginsenoside F3;No. 4 peaks are ginsenoside Rg2;No. 5 peaks are Ginsenoside Rc;No. 6 peaks are ginsenoside Rb2;No. 7 peaks For ginsenoside Rb3;No. 8 peaks are Ginsenoside F1;No. 9 peaks are ginsenoside Rd;No. 10 peaks are Ginsenoside F2;No. 11 peaks are Ginseng sapoglycoside Rg 3;No. 12 peaks are pseudo-ginsenoside Rh2.
Below in conjunction with the embodiment in the present invention, the technical solution in the present invention is clearly and completely described.It is aobvious So, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the reality in the present invention Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to In the scope of protection of the invention.
Embodiment 1
(1) experimental material:
40 batches of panax ginseng fruit medicinal materials are that in August, 2017 picks up from Jilin Province Baishan different regions, and specific sample message is shown in Table 1:
The sample message of 1 40 batches of panax ginseng fruit medicinal materials of table
(2) instrument and reagent:
High performance liquid chromatograph: 2695 high performance liquid chromatograph of Waters (Waters, US);Waters 2996PDA diode array detector (Waters, US);Empower chromatographic work station (Waters, US); METTLERAB135-S (Mettler-Toledo Instrument (Shanghai) Co., Ltd.);Analysis is chromatographically pure (Sigma) with acetonitrile.
Remaining reagent is to analyze pure (Beijing chemical reagent factory);Water is distilled water, is prepared by Millipore pure water system (Millipore,Milford,MA,USA);(Ginsenoside Re is abbreviated as Re, lot number: 110754- to ginsenoside Re 201626), ginsenoside Rb1's (Ginsenoside Rb1 is abbreviated as Rb1, lot number: 110704-201627), ginsenoside Rg2 (Ginsenoside Rg2 is abbreviated as Rg2, lot number: 111779-201601), (Ginsenoside Rc, writes a Chinese character in simplified form Ginsenoside Rc For Rc, lot number: 11641-201602), (Ginsenoside Rb2 is abbreviated as Rb2, lot number: 111715- to ginsenoside Rb2 201626), ginsenoside Rb3 (Ginsenoside Rb3 is abbreviated as Rb3, lot number: 111686-201604), Ginsenoside F1 (Ginsenoside F1, is abbreviated as F1, is abbreviated as F1, lot number: 111763-201602), ginsenoside Rd (Ginsenoside Rd is abbreviated as Rd, lot number: 11818-201626), Ginsenoside F2 (Ginsenoside F2 is abbreviated as F2, lot number: 110804-201604), ginseng sapoglycoside Rg 3 (Ginsenoside Rg3 is abbreviated as Rg3, lot number: 110804-201604) compares Product are provided by Nat'l Pharmaceutical & Biological Products Control Institute, and (Ginsenoside F3 is abbreviated as F3, lot number: MUST- to ginseng saponin F 3 18032311), pseudo-ginsenoside Rh2 (Pseudoginsenoside Rh2 is abbreviated as Rh2, lot number: MUST-18082801) is right It is provided according to product by Chengdu Man Site Biotechnology Co., Ltd, and through HPLC to analyze its pure for above-mentioned 12 kinds of saponin component reference substances Degree is all larger than 98%.
(3) preparation of mixed reference substance solution:
Take 12 kinds of saponin component reference substances appropriate respectively, it is accurately weighed, mixed reference substance solution, mistake are configured to methanol 0.22 μm of miillpore filter, takes subsequent filtrate, seals 4 DEG C of preservations.
(4) preparation of extracting solution (test solution):
Panax ginseng fruit medicinal powder (lower part of screen point after crossing 40 meshes) about 0.1g is taken, it is accurately weighed, it is placed in 50mL conical flask In;Methanol 20mL is added in precision, weighed, and 30min is extracted under 250W, 30kHz ultrasound condition, stands to room temperature, is mended with methanol The weight of sufficient less loss, mixes, and 0.22 μm of membrane filtration takes subsequent filtrate to get extracting solution.
(5) chromatographic condition of high performance liquid chromatography:
Mobile phase: mobile phase includes mobile phase A and Mobile phase B, wherein mobile phase A is acetonitrile;Mobile phase B is phosphoric acid water Solution, the volumn concentration of phosphoric acid is 0.2% in the Mobile phase B;
Gradient elution program:
0~15min, mobile phase A increase to 31%, Mobile phase B by 15% and are reduced by 85% to 69%;
15~25min, mobile phase A keep 31%, Mobile phase B to keep 69%;
25~35min, mobile phase A increase to 37%, Mobile phase B by 31% and are reduced by 69% to 63%;
35~45min, mobile phase A increase to 45%, Mobile phase B by 37% and are reduced by 63% to 55%;
45~60min, mobile phase A increase to 60%, Mobile phase B by 45% and are reduced by 55% to 40%;
The flow velocity of mobile phase is 1.0mL/min;
Detector is diode array detector;
Detection wavelength is 203nm;
Chromatographic column isOmega Polar C18 chromatographic column, specification are as follows: a length of 250mm, internal diameter 4.6mm are filled out Expect that partial size is 5 μm;
Column temperature is 35 DEG C;
Sampling volume is 10 μ L.
(6) precision is investigated:
Take panax ginseng fruit medicinal material test solution, by above-mentioned chromatographic condition continuous sample introduction 5 times, measure each component peak area and Retention time calculates its relative retention time and relative peak area.The results show that the relative retention time and phase of all chromatographic peaks 3.0% is respectively less than to the RSD of peak area, shows that the precision of the analysis method is good.
(7) similarity analysis
Panax ginseng fruit finger-print is carried out using " similarity evaluation " (2004A editions) software Data processing.It is matched using the map of S1 sample as reference fingerprint (as shown in Figure 1), carries out similarity evaluation point It analyses and by being compared with retention time in reference substance chromatogram, pointing out and being determined that 12 chromatographic peaks are common to 40 batches of samples. In Fig. 1, No. 1 peak is ginsenoside Re;No. 2 peaks are ginsenoside Rb1;No. 3 peaks are ginsenoside F3;No. 4 peaks are ginsenoside Rg2;No. 5 peaks are Ginsenoside Rc;No. 6 peaks are ginsenoside Rb2;No. 7 peaks are ginsenoside Rb3;No. 8 peaks are ginsenoside F1;No. 9 peaks are ginsenoside Rd;No. 10 peaks are Ginsenoside F2;No. 11 peaks are ginseng sapoglycoside Rg 3;No. 12 peaks are anthropomorphic ginseng soap Glycosides Rh2.The panax ginseng fruit medicinal materials fingerprint (as shown in Figure 2) of 40 different batches and reference fingerprint are compared, phase is obtained Like degree result.
Similarity result analysis, each shared peak area of 40 batches of panax ginseng fruit medicinal materials account for total peak area and are all larger than 95%, similarity Evaluation result is more consistent, meets traditional Chinese medicine fingerprint standard.
As can be seen from the above embodiments, method provided by the invention is easy to operate, accurately and reliably, can make up for it existing matter Measure control technology shortcoming, keep panax ginseng fruit quality of medicinal material control technology more perfect, avoid quality control unicity and Limitation provides scientific basis for the quality control of panax ginseng fruit medicinal material, establishes to improve the quality control level of panax ginseng fruit medicinal material Basis.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered It is considered as protection scope of the present invention.

Claims (10)

1. a kind of method for building up of panax ginseng fruit medicinal materials fingerprint, which comprises the following steps:
Mixed reference substance solution is provided, includes 12 kinds of saponin components, respectively ginsenoside in the mixed reference substance solution Re, ginsenoside Rb1, ginseng saponin F 3, ginsenoside Rg2, Ginsenoside Rc, ginsenoside Rb2, ginsenoside Rb3, ginseng Saponin(e F1, ginsenoside Rd, Ginsenoside F2, ginseng sapoglycoside Rg 3 and pseudo-ginsenoside Rh2;
Panax ginseng fruit medicinal material is extracted using methanol, obtains extracting solution;
The mixed reference substance solution and extracting solution are subjected to efficient liquid phase chromatographic analysis respectively, with the color of mixed reference substance solution On the basis of spectral peak, the panax ginseng fruit medicinal materials fingerprint containing 12 shared peaks is obtained;
The chromatographic condition of the high performance liquid chromatography are as follows:
Mobile phase: mobile phase includes mobile phase A and Mobile phase B, wherein mobile phase A is acetonitrile;Mobile phase B is phosphate aqueous solution, The volumn concentration of phosphoric acid is 0.2% in the Mobile phase B;
Gradient elution program:
0~15min, mobile phase A increase to 31%, Mobile phase B by 15% and are reduced by 85% to 69%;
15~25min, mobile phase A keep 31%, Mobile phase B to keep 69%;
25~35min, mobile phase A increase to 37%, Mobile phase B by 31% and are reduced by 69% to 63%;
35~45min, mobile phase A increase to 45%, Mobile phase B by 37% and are reduced by 63% to 55%;
45~60min, mobile phase A increase to 60%, Mobile phase B by 45% and are reduced by 55% to 40%;
Detector: diode array detector.
2. the method for building up of panax ginseng fruit medicinal materials fingerprint according to claim 1, which is characterized in that described to extract super It is carried out under the conditions of sound;The power of the ultrasound is 200~300W, and frequency is 35~45kHz.
3. the method for building up of panax ginseng fruit medicinal materials fingerprint according to claim 2, which is characterized in that the extraction when Between be 30~40min.
4. the method for building up of described in any item panax ginseng fruit medicinal materials fingerprints according to claim 1~3, which is characterized in that institute The amount ratio for stating methanol and panax ginseng fruit medicinal material is (15~25) mL:0.1g.
5. the method for building up of panax ginseng fruit medicinal materials fingerprint according to claim 1, which is characterized in that the mobile phase Flow velocity is 0.8~1.2mL/min.
6. the method for building up of panax ginseng fruit medicinal materials fingerprint according to claim 1, which is characterized in that carry out described efficient Detection wavelength when liquid-phase chromatographic analysis is 203nm.
7. the method for building up of panax ginseng fruit medicinal materials fingerprint according to claim 1, which is characterized in that carry out described efficient The chromatographic column used when liquid-phase chromatographic analysis forOmega Polar C18 chromatographic column;The specification of the chromatographic column are as follows: A length of 250mm, internal diameter 4.6mm, packing material size are 5 μm.
8. the method for building up of panax ginseng fruit medicinal materials fingerprint according to claim 1 or claim 7, which is characterized in that described in progress Column temperature when efficient liquid phase chromatographic analysis is 30~35 DEG C.
9. the method for building up of panax ginseng fruit medicinal materials fingerprint according to claim 1, which is characterized in that carry out described efficient Sampling volume when liquid-phase chromatographic analysis is 5~40 μ L.
10. the panax ginseng fruit medicinal material obtained using the method for building up of any one of the claim 1~9 panax ginseng fruit medicinal materials fingerprint Standard finger-print, which is characterized in that including 12 shared peaks, No. 1 peak is ginsenoside Re;No. 2 peaks are ginsenoside Rb1;3 Number peak is ginsenoside F3;No. 4 peaks are ginsenoside Rg2;No. 5 peaks are Ginsenoside Rc;No. 6 peaks are ginsenoside Rb2;No. 7 Peak is ginsenoside Rb3;No. 8 peaks are Ginsenoside F1;No. 9 peaks are ginsenoside Rd;No. 10 peaks are Ginsenoside F2;No. 11 peaks For ginseng sapoglycoside Rg 3;No. 12 peaks are pseudo-ginsenoside Rh2.
CN201910654262.2A 2019-09-11 2019-09-11 Establishment method of ginseng fruit medicinal material fingerprint spectrum and standard fingerprint spectrum thereof Active CN110398551B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910654262.2A CN110398551B (en) 2019-09-11 2019-09-11 Establishment method of ginseng fruit medicinal material fingerprint spectrum and standard fingerprint spectrum thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910654262.2A CN110398551B (en) 2019-09-11 2019-09-11 Establishment method of ginseng fruit medicinal material fingerprint spectrum and standard fingerprint spectrum thereof

Publications (2)

Publication Number Publication Date
CN110398551A true CN110398551A (en) 2019-11-01
CN110398551B CN110398551B (en) 2020-05-12

Family

ID=68324652

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910654262.2A Active CN110398551B (en) 2019-09-11 2019-09-11 Establishment method of ginseng fruit medicinal material fingerprint spectrum and standard fingerprint spectrum thereof

Country Status (1)

Country Link
CN (1) CN110398551B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111220719A (en) * 2019-11-11 2020-06-02 云南生物谷药业股份有限公司 Method for evaluating quality of ginseng medicinal material by using fingerprint spectrum

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111220719A (en) * 2019-11-11 2020-06-02 云南生物谷药业股份有限公司 Method for evaluating quality of ginseng medicinal material by using fingerprint spectrum

Also Published As

Publication number Publication date
CN110398551B (en) 2020-05-12

Similar Documents

Publication Publication Date Title
Cai et al. A capsule review of recent studies on the application of mass spectrometry in the analysis of Chinese medicinal herbs
Lau et al. Analysis of saponins in raw and steamed Panax notoginseng using high-performance liquid chromatography with diode array detection
Ong Extraction methods and chemical standardization of botanicals and herbal preparations
CN107271577B (en) Method for analyzing effective components of Qiling kidney-warming and bursa-eliminating preparation
Sarker et al. Applications of high performance liquid chromatography in the analysis of herbal products
CN102621264A (en) Method for constructing finger-print chromatogram for ginsenosides-containing crude drugs and preparations
CN104713953B (en) A kind of assay method of medicine finger-print
CN107340348A (en) A kind of method for building up of Bletilla striata medicinal materials HPLC finger-prints
CN110672747A (en) Method for detecting epimedium component, method for identifying variety of epimedium and application
CN106706786A (en) Method for determining content of six ginsenoside ingredients of folium ginseng
CN102353735B (en) Quality detection method for Tongmai Tangyanming capsule
CN105486762B (en) A kind of high-efficiency liquid-phase fingerprint detection method of female clever ball
CN107648369A (en) A kind of clarification process and method of quality control of the pharmaceutical composition that there is treatment acne to act on
CN110398551A (en) A kind of method for building up and its standard finger-print of panax ginseng fruit medicinal materials fingerprint
CN108226325A (en) Roripa montana gives birth to the method for building up of arteries and veins oral liquid composition finger-print
CN112798724A (en) Method for establishing saponin component chromatographic fingerprint suitable for ginseng traditional Chinese medicinal materials and medicinal material extracts
CN108732266A (en) A kind of construction method of the HPLC characteristic spectrums of capsule for radix astragalis and red-rooted salvia root
CN109239250B (en) Method for measuring fingerprint of brain-benefiting heart tablet and standard fingerprint thereof
CN109115904B (en) Construction method and application of UPLC fingerprint of Dingkundan
CN109212121A (en) Red ginseng medicinal materials fingerprint and its construction method with formulation ingredients relevance
CN104297360B (en) A kind of detection method of Compound Xueshuantong preparation finger-print
Ibrahem et al. Isolation of catchin and epigallocatchin from Iraqi Rhus coriaria by preparative high-performance liquid chromatography (PHPLC)
CN101953978B (en) Heart-soothing and lipid-lowering tablet medicine quality detecting method
CN107607653A (en) The method for determining Radix Scrophulariae extract finger-print
Yan et al. Simultaneous quantification of a herbal combination of Pueraria lobata, Salvia miltiorrhiza and Panax notoginseng by rapid resolution liquid chromatography

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