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Chinese medicine prepared aconite root and method for establishing fingerprint of alkaloid in extract thereof

A technique for fingerprinting and establishing methods, which is applied in the field of analysis of traditional Chinese medicine and its extracts, can solve problems such as the analysis method of undescribed Chinese medicine varieties, and achieve the effects of stable retention time, good separation and good peak shape

Inactive Publication Date: 2009-05-20
JIANGSU WANBANG BIOPHARMLS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the HPLC method and the "Technical Requirements" of the Pharmacopoeia are only general rules and guidelines, and do not describe the analysis methods of specific Chinese medicine varieties.

Method used

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  • Chinese medicine prepared aconite root and method for establishing fingerprint of alkaloid in extract thereof
  • Chinese medicine prepared aconite root and method for establishing fingerprint of alkaloid in extract thereof
  • Chinese medicine prepared aconite root and method for establishing fingerprint of alkaloid in extract thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0037] When adopting the method of the present invention to measure sample A, take C18 as filler (Phenomenex C18 (250mm * 4.6mm, 5 μ m)), methanol-buffer solution is mobile phase, buffer solution is 20mmol / L ammonium acetate-acetic acid buffer solution, Adjust the pH to 5.3 with acetic acid, the volume ratio of methanol to buffer is 48:52, and the detection wavelength is 234nm. The retention time of the chromatographic peak of neoaconitine is 48.12-48.25 minutes, and the number of theoretical plates of neoaconitine is not less than 2000.

Embodiment 2

[0039] When adopting the method of the present invention to measure sample B, take C18 as filler (KromasilC18 (250mm * 4.6mm, 5 μ m)), methanol-buffer is mobile phase, buffer is 0.2% triethylamine-acetic acid buffer, with Acetic acid was used to adjust the pH to 5.5, the volume ratio of methanol to buffer was 38:62, and the detection wavelength was 235nm. The retention time of the chromatographic peak of neoaconitine is 48.93-49.01min, and the number of theoretical plates is not less than 2000.

Embodiment 3

[0041] When adopting the method of the present invention to measure sample C, take C18 as filler (AlltimaC18 (250mm * 4.6mm, 5 μ m)), methanol-buffer solution is mobile phase, buffer solution is 0.05% triethylamine-10mmol / L ammonium acetate -Acetic acid buffer solution, the pH value is adjusted to 6.0 with acetic acid, the volume ratio of methanol to buffer solution is 50:50, and the detection wavelength is 230nm. The retention time of the chromatographic peak of neoaconitine is 47.89-47.99 minutes, and the number of theoretical plates is not less than 2000.

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Abstract

The invention relates to a method for establishing fingerprint of alkaloid in traditional Chinese medicine aconite or extract thereof. The method adopts an opposite phase high performance liquid chromatography, uses octadecylsilane chemically bonded silica or octadsilane chemically bonded silica as a filling agent, and uses an organic phase-buffer solution as a mobile phase, wherein pH value of the organic phase-buffer solution is 3.0 to 8.0, detection wavelength is 230 to 240 nanometers, the organic phase accounts for 20 to 70 percent of volume percentage of the mobile phase, and the organic phase is acetonitrile or methanol; the buffer solution is one of ammonium acetate-acetic acid buffer solution, triethylamine-acetic acid buffer solution, triethylamine-ammonium acetate-acetic acid buffer solution and triethylamine-acetic acid ammonium-acetic acid buffer solution; and the method comprises the following steps: using proper amount of aconitine, mesaconine or hypaconitine to prepare reference substance solution, preparing test solution, and pouring the reference substance solution and the test solution into a high performance liquid chromatograph respectively by accurately sucking to establish the fingerprint of the alkaloid in the traditional Chinese medicine aconite or the extract thereof.

Description

technical field [0001] The invention relates to an analysis method of traditional Chinese medicine and its extract, in particular to a method for establishing the alkaloid fingerprint in the traditional Chinese medicine aconite and its extract by using high performance liquid chromatography. Background technique [0002] Alkaloids are the main active ingredients of traditional Chinese medicine Aconitum. In Aconitum medicinal materials and their extracts, alkaloids are mainly diester-type and monoester-type aconitine alkaloids. The specific details of the nine main aconitine alkaloids are: The structure is as follows: [0003] [0004] It is recorded in the prior art that aconitine alkaloids have the effects of analgesic and heart-strengthening, and are used for recovering yang and rescuing adversity, tonifying fire and supporting yang, expelling wind and dehumidification, etc. [0005] The fingerprint test method of the present invention is tested according to the high-p...

Claims

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Application Information

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IPC IPC(8): A61K36/714G01N30/36G01N30/86
Inventor 杨春艳林彬刘跃跃王成乔德水高雪芹
Owner JIANGSU WANBANG BIOPHARMLS
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