Chromatographic analysis method of dehydroevodiamine

A technique for dehydroevodiamine and chromatographic analysis, which is applied in the field of chromatographic analysis, can solve problems such as tailing, and achieves the effects of convenient operation, simple analysis conditions and simple preparation.

Pending Publication Date: 2022-07-22
JIANGXI UNIVERSITY OF TRADITIONAL CHINESE MEDICINE +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The two are transformed into each other and exist at the same time, resulting in their combined peaks in high performance liquid chromatography, resulting in severe tailing

Method used

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  • Chromatographic analysis method of dehydroevodiamine
  • Chromatographic analysis method of dehydroevodiamine
  • Chromatographic analysis method of dehydroevodiamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A chromatographic analysis method for dehydroevodiamine in Evodia, the concrete steps are:

[0030] (1) Preparation of the reference substance solution: Precisely weigh 3.12 mg of the reference substance, dehydroevodiamine, and place it in a 10 mL volumetric flask, add anhydrous methanol to dissolve and dilute to the mark, and shake well to obtain the reference substance stock solution, which is stored in Refrigerator, dilute as needed before use;

[0031] (2) Evodia test sample solution: Take about 0.5 g of Evodia root powder, accurately weigh it, put it in a conical flask with stopper, add 25 mL of 70% ethanol precisely, weigh it, soak it for 1 h, sonicate it for 40 min, and let it Make up the lost weight by cooling, shake well and filter, take the filtrate, pass through a 0.22 μm filter membrane, and set aside;

[0032] (3) Chromatographic conditions: DIKMA Platisil ODS column (4.6×250μm, 5μm); mobile phase: methanol (A)-water (B), both containing 0.1mol / L HCl; grad...

Embodiment 2

[0035] The chromatographic analysis method of dehydroevodiamine in compound berberine tablets, the concrete steps are:

[0036] (1) Preparation of the test product: Take 10 pieces of compound berberine tablets, remove the sugar coating, crush them in a mortar, mix evenly, weigh 0.5 g, accurately weigh, accurately add 25 ml of methanol, weigh the weight, ultrasonically Extraction for 30 min, let cool, make up the weight with methanol, take an appropriate amount of sample solution and pass through a 0.22 μm organic filter membrane to obtain;

[0037] (2) Chromatographic conditions: Shimadzu WondaCract ODS-2 (4.6×150mm, 5μm); mobile phase: acetonitrile (A)—0.1mol / L HCl (B); gradient elution: 0~6min, 43%~63% A; Flow rate: 1.0 mL / min; Injection volume: 5 μL; Column temperature: 30°C; Detection wavelength: 370 nm;

[0038] (3) Chromatographic separation efficiency: see the chromatogram image 3 , Dehydroevodiamine obtained a good chromatographic separation, and its chromatographic...

Embodiment 3

[0040] A chromatographic analysis method for dehydroevodiamine in rat plasma samples, the specific steps are:

[0041](1) Rats and methods of administration: SPF grade SD rats, male, body weight (200±20) g, 24 rats, provided by Hunan Slike Jingda Laboratory Animal Co., Ltd., license number SCXK (Xiang) 2016- 0002. The animals were reared at a temperature of 20-22°C, light / dark 12h / 12h, with free food and water, and the experiment was started after one week of adaptive rearing. Dehydroevodiamine was suspended in 0.5% CMC-Na and administered by gavage at a dose of 2.0 g / kg.

[0042] (2) Preparation of samples: Blank plasma sample: Take 50 μL of blank plasma sample, put it in a 1.5 mL centrifuge tube, add 1 mL of acetonitrile, vortex and mix for 2 min (deproteinized), and centrifuge at 4000 rpm for 10 min. The supernatant was taken, blown with nitrogen at 40°C, evaporated to dryness, reconstituted with 100 μL of 50% acetonitrile, vortexed for 2 min, and centrifuged at 14,000 ...

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Abstract

The invention discloses a chromatographic analysis method for thoroughly solving the peak shape of a dehydroevodiamine chromatographic peak, which adopts reversed-phase high performance liquid chromatography, takes hydrochloric acid as an additive for the first time, adjusts the pH value of a mobile phase to be 1-2, remarkably improves the problem of trailing of the dehydroevodiamine chromatographic peak, has simple analysis conditions, is convenient to operate, and is suitable for industrial production. The chromatographic mobile phase additive is economical and environment-friendly; symmetry factors of chromatographic peaks meet requirements of Chinese pharmacopoeia, and chromatographic analysis conditions can be used for measuring the content of dehydroevodiamine in medicinal materials, Chinese patent medicines and biological samples of fructus evodiae.

Description

technical field [0001] The invention relates to the technical field of chromatographic analysis methods, in particular to a chromatographic analysis method for dehydroevodiamine. Hydrochloric acid is added to a chromatographic mobile phase to make the pH of 1-2, so as to completely solve the chromatographic peak tailing of dehydroevodiamine. question. Background technique [0002] Dehydroevodiamine (DHED) is an indole alkaloid with high pharmacological activity isolated from the Rutaceae plant Evodia, mainly exists in Rutaceae ( Rutaceae ) in the fruit of the plant Evodia, is the characteristic component of the plant. Modern pharmacological studies have shown that dehydroevodiamine has various pharmacological activities such as anti-inflammatory, antiemetic, dilating blood vessels, slowing heart rate, lowering blood pressure, and neuroprotection. 2011, 29(11): 2415-2417; Hepatotoxicity comparison of crude andlicorice-processed euodiae fructus in rats with stomach excess-co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/34G01N30/06
CPCG01N30/34G01N30/06
Inventor 袁金斌张敏罗习珍钟民勇周立分杨林
Owner JIANGXI UNIVERSITY OF TRADITIONAL CHINESE MEDICINE
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