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Characterization method of secondary metabolite chromatogram and mass spectrum fingerprint spectrum of callicarpa nudiflora genuine medicinal materials

A technology of secondary metabolites, purple pearl authenticity, applied in the field of characterization of secondary metabolites chromatography and mass spectrometry fingerprints, can solve the confusion in the application of nude flower purple pearl base sources, the same thing with different names, the same name and different things, and authentic Problems such as inability to characterize medicinal materials, achieve good reproducibility and stability, large peak capacity, and good resolution

Active Publication Date: 2020-02-21
JIANGXI POZIN PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The technical problem to be solved by the present invention is to provide a kind of secondary metabolism of naked flower purple pearl authentic medicinal materials in view of the chaotic application of naked flower purple pearl base sources in the market, the same thing with different names, the same name and different substances, and the authentic medicinal materials that cannot be characterized. Characterization Method of Product Chromatography and Mass Spectrometry Fingerprint

Method used

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  • Characterization method of secondary metabolite chromatogram and mass spectrum fingerprint spectrum of callicarpa nudiflora genuine medicinal materials
  • Characterization method of secondary metabolite chromatogram and mass spectrum fingerprint spectrum of callicarpa nudiflora genuine medicinal materials
  • Characterization method of secondary metabolite chromatogram and mass spectrum fingerprint spectrum of callicarpa nudiflora genuine medicinal materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Take a sample of A. nudiflora (Baisha, harvested in February 2017), crush it, pass through a 40-mesh sieve, accurately weigh about 0.5g of the sample powder, put it in a stoppered Erlenmeyer flask, add 25mL of 50% methanol aqueous solution , weighed, sonicated for 30min, allowed to cool, supplemented with 50% methanol for weight loss, shaken, passed through a 0.22μm microporous membrane, and the filtrate was taken as the test solution.

[0039] Using Ultra Performance Liquid Chromatography (UPLC) Waters ACQUITY ARC in UPLC Method TM Ultra High Performance Liquid Chromatograph; EclipsePlusC 18 RRHD chromatographic column, its specification is outer diameter 2.1mm×column length 150mm, packing diameter 1.8μm. The mobile phase is (A) 0.1% phosphoric acid aqueous solution and (B) acetonitrile, gradient elution, change the gradient, optimize the conditions of the fingerprint spectrum of the nudibranch, and select the spectrum with better results, 1-6 different gradient elut...

Embodiment 2

[0054] Take a sample of the nude flower purple pearl (origin Baisha, harvested on October 15, 2016), crush it, pass through a 40-mesh sieve, accurately weigh about 0.5g of the sample powder, place it in a stoppered conical flask, and add 50% methanol Aqueous solution 25mL, weighing, ultrasonic 30min, let cool, make up for weight loss with 50% methanol, shake well, pass through 0.22μm microporous membrane, take the subsequent filtrate as the test solution.

[0055] Using Ultra Performance Liquid Chromatography (UPLC) Waters ACQUITY ARC in UPLC Method TM Ultra-high performance liquid chromatography; phenomenonex kintex XB-C 18 100A chromatographic column, its specification is outer diameter 2.1mm×column length 150mm, packing diameter 1.7μm. The mobile phase is (A) 0.1% phosphoric acid aqueous solution and (B) acetonitrile, and gradient elution is performed, and the gradient is changed to optimize the conditions of the fingerprint of Aurora nudiflora. 1-7 different gradient el...

Embodiment 3

[0073] Take a sample of the nude flower purple pearl (origin Baisha, harvested on October 15, 2016), crush it, pass through a 40-mesh sieve, accurately weigh about 0.5g of the sample powder, place it in a stoppered conical flask, and add 80% methanol Aqueous solution 25mL, weigh, ultrasonic 45min, let cool, make up for weight loss with 80% methanol, shake well, pass through 0.22μm microporous membrane, take the subsequent filtrate as the test solution.

[0074] Using Ultra Performance Liquid Chromatography (UPLC) Waters ACQUITY ARC TM Model ultra-high performance liquid chromatography; Phenomenex kintex XB-C 18 The chromatographic column has the specifications of outer diameter 2.1mm×column length 150mm, and packing diameter 1.7μm. The mobile phase is (A) 0.1% phosphoric acid aqueous solution and (B) acetonitrile, and the gradient elution is as follows:

[0075] time Mobile phase (v / v%) B time Mobile phase (v / v%) B 0min 8％ 5min 13％ 15min 13％ ...

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Abstract

The invention relates to the technical field of traditional Chinese medicine analysis, in particular to a characterization method of a secondary metabolite chromatogram and a mass spectrum fingerprintspectrum of callicarpa nudiflora genuine medicinal materials. According to the method, the UPLC is adopted to establish the full-component fingerprint spectrum of a callicarpa nudiflora genuine medicinal material, and the UPLC and DAD / QTOF-MS / MS combined technology is adopted to carry out on-line rapid component qualitative analysis and compound identification on the full-component fingerprint spectrum of the callicarpa nudiflora genuine medicinal material and the optimal chemical substance phenotype of the callicarpa nudiflora genuine medicinal material in the specific natural environment isformed. The callicarpa nudiflora genuine medicinal material full-component fingerprint spectrum method has the beneficial effects that the operation is simple, the peak capacity is large, the precision, the reproducibility and the stability are good, the chromatographic peak separation degree is good, the analysis time is short, and the analysis efficiency and the sensitivity are high; the formedoptimal phenotype of chemical substances of the callicarpa nudiflora genuine medicinal material in a specific natural environment solve the problems of disordered application of callicarpa nudiflorabase sources, incapability of representing genuine medicinal materials and the like in the market are solved.

Description

technical field [0001] The invention relates to the technical field of analysis of traditional Chinese medicines, in particular to a characterization method of secondary metabolite chromatographic and mass spectrometric fingerprints of authentic medicinal materials of Zizhu nudiflora. Background technique [0002] Authentic medicinal materials are the essence of traditional Chinese medicine, and they are synonymous with high-quality medicinal materials in traditional Chinese medicine. The formation of authentic medicinal materials is inseparable from the excellent germplasm of traditional Chinese medicine and the specific natural environment. For this reason, many authentic medicinal materials are often given place names before the name of the medicine to show their authentic production areas, such as Xining rhubarb, Ningxia wolfberry, and Chuan Fritillaria. [0003] Modern biology believes that the biological essence of authentic medicinal materials is phenotype variation ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G16H70/40
CPCG16H70/40
Inventor 杨扬李小锋杨义芳陈梁邓杰仁康兴东章弘扬夏淑英任昭洁肖绍川
Owner JIANGXI POZIN PHARMA
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