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Preparation method of test solution for detecting aconitine-type alkaloids through high-efficiency liquid phase chromatography

A high-performance liquid chromatography and aconitum technology, which is applied in the field of preparation of a test solution for the detection of aconitum alkaloids by high-performance liquid chromatography, can solve the problem of low real content, drug quality control, use and treatment Unfavorable effects, unsatisfactory test results accuracy, etc., to achieve high sample recovery, improve sensitivity and detection limit

Active Publication Date: 2013-06-05
SICHUAN ACAD OF CHINESE MEDICINE SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The study found that the actual determination results of the tested products containing aconitum alkaloids by this method are often significantly lower than the real content, the accuracy of the test results is not satisfactory, and will lead to the quality control of related drugs , Adverse effects of use and therapeutic effect

Method used

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  • Preparation method of test solution for detecting aconitine-type alkaloids through high-efficiency liquid phase chromatography
  • Preparation method of test solution for detecting aconitine-type alkaloids through high-efficiency liquid phase chromatography
  • Preparation method of test solution for detecting aconitine-type alkaloids through high-efficiency liquid phase chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Take about 2 g of Baifu Tablet powder (through the No. 3 sieve), accurately weigh it, put it into a stoppered Erlenmeyer flask, add 50 ml of hydrochloric acid solution with a pH of 1~2, shake well, and perform ultrasonic treatment (power 300 W, frequency 40 kHz) for 30 min, let cool, centrifuged, took 25ml of the supernatant, put it on a D101 macroporous adsorption resin column (inner diameter about 1cm, column height about 10cm), washed with water about 3 times the volume of the column bed to remove impurities, discarded Remove the water solution, and then elute with about 4 times the volume of the column bed with ethanol-hydrochloric acid aqueous solution containing 70 (v)% alcohol at pH 1~2, collect the eluent containing alcohol, recover the solvent under reduced pressure below 60°C, and use methanol Dissolve, transfer to a 2ml measuring bottle, add methanol to the mark, shake well, filter, take the subsequent filtrate as the test solution for HPLC detection.

Embodiment 2

[0025] Take about 4 g of Pao Tianxiong powder (passed through No. 3 sieve), accurately weigh it, put it into a stoppered Erlenmeyer flask, add 100 ml of hydrochloric acid solution with a pH of 2~3 accurately, shake well, and perform ultrasonic treatment (power 250 W, frequency 30 kHz ) for 40 min, let cool, centrifuge, take 75 ml of the supernatant, put it on HPD100 macroporous adsorption resin column (inner diameter about 1.5 cm, column height about 10 cm), and use 2 times the column bed volume of water, pH 9- Wash with 10% sodium hydroxide aqueous solution and water to remove impurities, discard the aqueous solution, and then use 4 to 5 times the volume of the column bed to elute with ethanol-hydrochloric acid aqueous solution containing 60 (v)% alcohol at pH 2 to 3, and collect the alcohol-containing wash. Remove liquid, recover the solvent under reduced pressure below 60°C, dissolve it in water, transfer it to a 5ml measuring bottle, add water to the mark, shake well, centr...

Embodiment 3

[0027] Take about 2 g of iron bar hammer powder (passed through No. 4 sieve), accurately weigh it, put it into a stoppered Erlenmeyer flask, add 50 ml of sulfuric acid solution with a pH of 3~4, shake well, and perform ultrasonic treatment (power 100 W, frequency 40 kHz ) for 60 min, let cool, centrifuge, take 40 ml of the supernatant, adjust the pH to 7-8 with sodium bicarbonate, put it on a HPD300 macroporous adsorption resin column (about 1 cm in inner diameter, about 10 cm in height), and use 2~ Wash and remove impurities with 3 times column bed volume of pH 8-9 sodium bicarbonate solution and water, discard the water, and then use 4 times column bed volume of methanol-hydrochloric acid aqueous solution with pH 3~4 containing 70 (v)% alcohol Elution, collect the eluate, recover the solvent under reduced pressure below 60°C, dissolve it with 50(v)% ethanol, transfer it to a 2 ml volumetric flask, add 50(v)% ethanol to the mark, shake well, filter, Get continued filtrate as ...

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Abstract

Disclosed is a preparation method of test solution for detecting aconitine-type alkaloids through the high-efficiency liquid phase chromatography. The test solution is obtained after extracts of a tested product are dissolved by solvent allowed by pharmacopeia, wherein the extracts contain aconitine-type alkaloid components to be tested. After acidic water extracting solution which contains the aconitine-type alkaloid components and is less than or equal to 5 in potential of hydrogen (PH), of the tested product is absorbed by macroporous polymeric adsorbent, and the acid water extracting solution is washed through water or washed sequentially through alkali water with PH being 8-10 and water so as to remove impurities, the acid water extracting solution is then eluted through the use of acid alcohol-water solution which contains 50-100% alcohol in size and is less than or equal to 4 in PH and elution solution is collected, and the extracts of the tested product are obtained after the solvent is removed. The test solution obtained through the preparation method can be widely applicable to chromatographic conditions of detecting the aconitine-type alkaloids through the high-efficiency liquid phase chromatography, chromatographic separation effect (separation degree), reproducibility, stability, precision and the like all meet the demands of a Chinese traditional medicine standard analytical method, interference of other components can be greatly reduced, and detection limit (sensitivity) is improved.

Description

technical field [0001] The invention relates to a preparation method of a test solution for detecting aconitum alkaloids by high performance liquid chromatography. Background technique [0002] Medicinal plants of the genus Aconitum, such as aconite and aconitum, are commonly used Chinese herbal medicines and are widely used in clinical treatment. There are more than 350 kinds of Chinese patent medicines of Huanghuaconitou. The main toxic / effective ingredients in the medicinal plants of the genus Aconitum are diester alkaloids (aconitine, neoaconitine, hypoaconitine, etc.), monoester alkaloids (benzoyl aconitine, benzoyl aconitine, etc.) Formyl neoaconine, benzoyl hypoaconitine, etc.) and alcohol amine alkaloids (aconitine, neoaconitine, hypoaconitine, etc.), therefore, the medicinal materials of the genus Aconitum , decoction pieces and their preparations generally require detection of aconitine, hypoaconitine, neoaconitine, benzoyl aconitine, benzoyl hypoaconitine, benz...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 易进海黄志芳陈燕唐小龙刘玉红刘云华
Owner SICHUAN ACAD OF CHINESE MEDICINE SCI
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