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Determination method of benzoic acid ester compounds in traditional Chinese medicine gentianae radix et rhizoma

A technology of ester compounds and benzoic acid, which is applied in the field of chemical analysis to achieve the effects of good stability, improved analysis efficiency and high sensitivity

Inactive Publication Date: 2014-04-23
INST OF MEDICINAL PLANTS YUNNAN ACAD OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, most of the literatures focus on the determination of gentiopicroside and swertiamarin in gentian by high performance liquid chromatography (HPLC), but there are no active ingredients of 2,3-dihydroxybenzoate in gentian to report

Method used

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  • Determination method of benzoic acid ester compounds in traditional Chinese medicine gentianae radix et rhizoma
  • Determination method of benzoic acid ester compounds in traditional Chinese medicine gentianae radix et rhizoma
  • Determination method of benzoic acid ester compounds in traditional Chinese medicine gentianae radix et rhizoma

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take dried samples of gentian (including roots, stems, leaves, seeds), crush them and pass through a 100-mesh sieve; weigh 1.5g and place them in a 50mL conical flask with stopper, add 10mL of 95% ethanol, and ultrasonically extract at room temperature for 40min , filtered, and the filtrate was passed through a 0.22 μm microporous membrane to prepare a sample solution.

Embodiment 2

[0023] The sample prepared in Example 1 was determined by liquid chromatography-mass spectrometry to determine the content of benzoate compounds, as follows.

[0024] instrument:

[0025] LC-MS / MS 8030 UHPLC triple quadrupole tandem mass spectrometer (Shimadzu, Japan).

[0026] Liquid chromatography conditions:

[0027] Chromatographic column: Shim-pack XR-ODS Ⅲ (75×2.0mm, 1.6μm); mobile phase: methanol-0.1% formic acid, isocratic elution (95% methanol), equilibration time is 6min; column temperature: 40°C; Flow rate: 0.45mL / min; injection volume: 20 μL.

[0028] Mass Spectrometry Conditions:

[0029] Electrospray ionization source (ESI), negative ionization mode; capillary voltage is 4.5KV; drying gas and atomizing gas are nitrogen, flow rates are 3.0 and 15mL / min respectively; collision gas (CID) argon; DL tube temperature 250°C, The heating block temperature is 300°C; the product ion scan is m / z 135 , the collision voltage is 35V; the quantitative analysis adop...

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Abstract

The invention provides a determination method of anti-senile dementia effective component benzoic acid ester compounds in a traditional Chinese medicine gentianae radix et rhizoma, and belongs to the field of chemical analysis. The method is characterized by comprising the steps: with gentianae radix et rhizoma as raw material, crushing, screening, then carrying out ultrasonic extraction by adopting a 95% ethanol solution, filtering, extracting the benzoic acid ester compounds, and detecting the main benzoic acid ester compounds in gentianae radix et rhizoma by adopting a liquid chromatography-tandem mass spectrometry. With the adopting of the LC-MS / MS method, the method is high in sensitivity and good in stability, is convenient and fast, and is suitable for batch quantity analysis of an ultra-low-content target object in a complex matrix.

Description

technical field [0001] The invention belongs to the field of chemical analysis, and in particular relates to a method for determining benzoic acid ester compounds, the effective anti-senile dementia components in the traditional Chinese medicine gentian. Background technique [0002] The traditional Chinese medicine Gentianae (Gentianae Radix et Rhizoma) is a Gentianae plant: Gentianae Radix et Rhizoma Gentiana manshurica Kitag., gentian Gentiana scabra Bge., three flower gentian Gentiana triflora Pall. or Yunnan gentian Gentiana rigescens The dried roots and rhizomes of Franch. Gentiana yunnanensis, aliases: Gentiana yunnanensis (Diannan herbal medicine), Gentiana gentiana (Illustrated Handbook of Higher Plants in China), bitter grass, herring gall, Gentiana chinensis (Yunnan), blue flower root, and firecracker flower. It is "Chinese Pharmacopoeia" One of the gentian varieties included is also a famous authentic medicinal material in Yunnan, and it is included in ...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 潘俊肖丹李晚谊沈锐
Owner INST OF MEDICINAL PLANTS YUNNAN ACAD OF AGRI SCI