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HPLC (High Performance Liquid Chromatography) fingerprint spectrum construction method and HPLC fingerprint spectrum

A fingerprint and construction method technology, applied in the field of Sanqi drug analysis, can solve the problem of not being able to identify the medicinal parts of Sanqi, and achieve good stability and reproducibility

Inactive Publication Date: 2018-08-03
亳州中药材商品交易中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above two documents were identified from the methods of infrared analysis and ultraviolet analysis, and they were only used as authenticity identification, and the medicinal parts of Panax notoginseng could not be well identified.

Method used

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  • HPLC (High Performance Liquid Chromatography) fingerprint spectrum construction method and HPLC fingerprint spectrum
  • HPLC (High Performance Liquid Chromatography) fingerprint spectrum construction method and HPLC fingerprint spectrum
  • HPLC (High Performance Liquid Chromatography) fingerprint spectrum construction method and HPLC fingerprint spectrum

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1. Chromatographic conditions

[0033] Column: Kromasil C 18 Chromatographic column (250×4.6mm, 5μm, ); mobile phase: acetonitrile (A): water (B) linear gradient elution (v / v), the ratio is shown in Table 1; flow rate: 1mL min -1 ; Column temperature: 30° C.; Detection wavelength: 203 nm. Injection volume: 20 μL.

[0034] Table 1: Acetonitrile (A): water (B) mobile phase gradient table (v / v)

[0035] time

0~5min

5~20min

20~45min

45~50min

50~60min

60~70min

Acetonitrile (%)

5→20

20→36

36→80

80→100

100

100→5

water(%)

95→80

80→64

64→20

20→0

0

0→95

[0036] 2. Preparation of reference substance and test solution

[0037]Preparation of reference solution: Accurately weigh appropriate amount of notoginseng saponin R 1 , Ginsenoside Rg 1 , Re, Rb 1 , Rb 2 , Rb 3 and Rf reference substance, dissolved in methanol to make a concentration of about 50μg·mL -1 mixed reference solution....

Embodiment 2

[0046] 1. Precision experiment

[0047] Accurately draw the notoginseng need testing solution in the embodiment one, measure by the chromatographic condition in the embodiment one, respectively continuous sampling 5 times, with notoginseng saponin R 1 The relative retention time and peak area ratio of the characteristic peaks in the obtained spectrum were analyzed for the reference peak (S peak), and the RSD was calculated. Among them, the RSD of the retention time of the S peak was 0.14%, the RSD of the peak area was 0.46%, the RSD of the relative retention time of other characteristic peaks was 0.013%-0.21%, and the RSD of the relative peak area was 0.29%-3.44%.

[0048] 2. Stability experiment

[0049] Accurately draw the notoginseng need testing solution in embodiment one, place respectively after 1,2,3,5,7 days, measure fingerprint by the chromatographic conditions in embodiment one, with notoginseng saponin R 1 The relative retention time and peak area ratio of the cha...

Embodiment 3

[0054] Accurately weigh 20, 40, 60, 80, 100 heads of Panax notoginseng main root, tendon (branch root), scissors (rhizome), leaf and flower coarse powder 2g respectively, a kind of need testing solution preparation method according to embodiment Prepared, measured by chromatographic conditions in Example 1, the results are shown in image 3 with 4 . Take notoginseng saponin R1 as the reference peak (S peak) to analyze the relative retention time and peak area ratio of the characteristic peaks in the spectra obtained. The results are shown in Table 3 and Table 4.

[0055] Table 3. The relative retention time of the main peaks in the HPLC fingerprints of Panax notoginseng with different specifications and different medicinal parts

[0056]

[0057] Table 4. The relative peak area ratio of the main peaks in the HPLC fingerprints of Panax notoginseng with different specifications and different medicinal parts

[0058]

[0059]

[0060] As can be seen from Tables 3 and ...

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Abstract

The invention relates to the field of analysis of pseudo-ginseng drugs, and particularly relates to an HPLC (High Performance Liquid Chromatography) fingerprint spectrum construction method for the pseudo-ginseng drugs and panax notoginseng saponins and an HPLC fingerprint spectrum. The HPLC fingerprint spectrum construction method comprises the following steps: (1) respectively weighing proper amount of notoginsenoside R1, ginsenosides Rg1, Re, Rb1, Rb2, Rb3 and a reference substance Rf, adding methyl alcohol to dissolve, preparing a mixed reference substance solution at the concentration of30-70 [mu]g.mL<-1>; (2) weighing a pseudo-ginseng sample, placing in a vessel, adding methyl alcohol, preparing a solution at the concentration of 30-50 mg / mL, weighing, ultrasonically extracting for30-60 minutes, cooling to the room temperature, supplementing a lost solvent with methyl alcohol, and filtering an extracting solution by using a microporous filter membrane, thereby obtaining a sample solution; (3) respectively taking the mixed reference substance solution prepared in the step (1) and the sample solution prepared in the step (2) to implement high performance liquid chromatograph;and (4) using a reference substance comparison method to establish the HPLC fingerprint spectrum for the pseudo-ginseng drugs by testifying the chemical ingredients in the fingerprint spectrum through the LC-MS or HPLC-MS. The HPLC fingerprint spectrum construction method and the HPLC fingerprint spectrum are used for the quality analysis of the pseudo-ginseng drugs and panax notoginseng saponinextracts, and provide the evidences.

Description

technical field [0001] The invention relates to the field of notoginseng drug analysis, and specifically relates to a method for constructing an HPLC fingerprint of a notoginseng medicinal material and a total saponin of notoginseng and an HPLC fingerprint. Background technique [0002] Panax notoginseng is Panax notoginsng (Burk) F.H.Chen, a plant of the genus Panax of the family Araliaceae. It was first recorded in "Compendium of Materia Medica", and it is mainly produced in Yunnan, Guangxi and other provinces of my country. It has the functions of dispelling blood stasis, stopping bleeding, reducing swelling and relieving pain, and is a commonly used traditional Chinese medicine in clinic. The main active ingredient of Panax notoginseng is total saponins of Panax notoginseng, which has pharmacological effects such as dilating blood vessels, reducing myocardial oxygen consumption, inhibiting platelet aggregation, prolonging coagulation time, lowering blood lipids, scavengi...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 怀化
Owner 亳州中药材商品交易中心有限公司
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