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

A technology of fingerprint spectrum and construction method, applied in the field of Panax notoginseng drug analysis, can solve the problem of not being able to distinguish the medicinal parts of Panax notoginseng well, and achieve the effect of good stability and reproducibility

Inactive Publication Date: 2018-11-23
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

Benefits of technology

This patented technology allows researchers to accurately analyze various chemical components from panax ginger root (PTL) without losing their effectiveness or being affected by other factors like temperature during storage. It also provides an accurate way to compare these extracted compounds with existing methods that were used previously.

Problems solved by technology

This patented describes a technical problem with making pure butter gears without harmful side effects like those caused by common vegetables called panasapogenin. Current extraction techniques involve cutting down roots from plants, grinding up berries, crushing bags containing these roots, separating out impurity compounds, and then adding water solubilizers and preservatives to improve shelf life stability. These processes can lead to contaminants being added during production process. There have been attempts at developing fast identification systems based on molecular markers derived from nontoxic pigments extracted from this crude mixture.

Method used

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

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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 and 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 4...

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Abstract

The invention relates to the field of radix notoginseng pharmaceutical analysis, in particular to a construction method for HPLC (High Performance Liquid Chromatography) fingerprints of a radix notoginseng medicinal material and panax notoginseng saponins. The construction method comprises the following steps: (1) weighing a proper amount of notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, ginsenoside Rb2, ginsenoside Rb3 and ginsenoside Rf control substances, and adding methanol for dissolving to obtain a mixed control substance solution of which the concentration is 30 to 70 mu g.mL; (2) weighing a radix notoginseng sample, placing the weighed radix notoginseng sample into a container, adding the methanol to prepare a solution of which the concentration is 30 to 50 mu g.mL, weighing, performing ultrasonic extraction for 30 to 60 minutes, cooling to room temperature, supplementing lost solvent by the methanol, and filtering an extraction solution with a microfiltration membrane to obtain a test solution; (3) performing high performance liquid chromatography analysis on the mixed control substance solution obtained in step (1) and the test solution obtained instep (2) respectively; (4) testifying chemical components in a fingerprint with a control substance control method by adopting LC-MS (Liquid Chromatograph-Mass Spectrometer) or an HPLC-MS to constructthe HPLC fingerprint of the radix notoginseng medicinal material. The method can be applied to and provides a basis for the quality analysis of the radix notoginseng medicinal material and total saponin extracts.

Description

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Claims

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Application Information

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Owner 亳州中药材商品交易中心有限公司
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