HPLC method detects carboxy atractyloside and/or preparation method of test article

A carboxy atractyloside and atractyloside technology, which is applied in the field of preparation of the test product, can solve the problems of high requirements on instrument conditions, complex components, low content of components, etc., and achieve the effect of improving sensitivity and detection limit

Active Publication Date: 2016-05-11
SICHUAN ACAD OF CHINESE MEDICINE SCI
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Problems solved by technology

For cocklebur medicinal material or decoction pieces, the conventional water ultrasonic extraction solution can be directly used as the test solution, but for the compound preparation of traditional Chinese medicine, because of its complex composition, the content of atractylodes glycosides in it is low, and it is weakly absorbed at the end, so Due to the large interference of other components, the test solution prepared in a conventional way is often difficult to meet the requirements of HPLC analysis and detection
For this reason, Chen Lulu et al. reported the use of LC-MS in "Determination of the content of atractyloside, the toxic component in four kinds of compound granules containing Xanthium Fructus" (New Drugs and Clinical Pharmacology of Chinese Medicine, 2013,24(3):297). Chromatography has been used to determine the content of atractylodes in several compound granules, but it is difficult to be widely used because of its high requirements on instrument conditions

Method used

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  • HPLC method detects carboxy atractyloside and/or preparation method of test article

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Take about 1.0g of cocklebur powder (through No. 3 sieve), weigh it accurately, put it into a stoppered Erlenmeyer flask, add 20mL of water precisely, ultrasonicate (power 300W, frequency 40kHz) for 40min, take it out, centrifuge, and take the supernatant 10ml (pH6.2), adjust pH5 with hydrochloric acid solution, put on D101 macroporous adsorption resin column (inner diameter about 1cm, column height about 10cm), wash with pH5 water about 3 times the volume of the column bed to remove impurities, discard the water liquid, then elute with 50 (v)% ethanol about 4 times of the column bed volume, collect the ethanol eluate, and recover the solvent under reduced pressure below 60°C, then the said test sample can be obtained, or the ethanol can be After the solvent is recovered from the eluent, it is directly transferred to a 10ml measuring bottle with water, added to the mark, shaken up, filtered, and the subsequent filtrate is used as the test solution for HPLC detection.

Embodiment 2

[0020] Take about 0.5g of Biyuan pill powder, weigh it accurately, put it in a stoppered Erlenmeyer flask, add 25mL of water precisely, ultrasonicate (power 300W, frequency 40kHz) for 40min, take it out, centrifuge, take supernatant 15ml (pH value is about 6 ), adjust the pH to 5 with hydrochloric acid solution, pass through a D101 macroporous resin column (about 1.2 cm in inner diameter, about 10 cm in height), wash with 30 mL of pH 5 water and elute with 40 mL of 50% ethanol in sequence, collect the alcohol eluate and store it at 60 °C Concentrate under reduced pressure to about 5mL, pass through WAX solid-phase extraction column (pre-activated with 6mL of methanol and 6 mL of water), wash the utensils with appropriate amount of water, pass through the column together, and rinse with 5% formic acid aqueous solution and 6 mL of 5% formic acid methanol solution in sequence Remove impurities, then elute with 9mL 2% ammonia water methanol solution, collect the eluate, recover the...

Embodiment 3

[0022] Take about 0.5g of Tongqiao rhinitis granule powder, accurately weigh it, put it into a stoppered Erlenmeyer flask, add 25mL of pH5 buffer solution precisely, ultrasonicate (power 100W, frequency 40kHz) for 50min, take it out, centrifuge, and take 15ml of supernatant ( pH 5), adjusted to pH 4 with sulfuric acid solution, passed through a D101 macroporous resin column (about 1.2 cm in inner diameter, about 10 cm in height), washed with 25 mL of pH 6 water and eluted with 50 mL of 70% ethanol in turn, collected the alcohol eluate and washed it at 60 Concentrate under reduced pressure below ℃ to about 5mL, pass through a WAX solid-phase extraction column (pre-activated with 6mL of methanol and 6mL of water), wash the utensils with an appropriate amount of water, and pass through the column together, 10mL of 1% formic acid aqueous solution and 4mL of 7% formic acid in methanol Wash to remove impurities, then elute with 8mL 5% ammonia water methanol solution, collect the elua...

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Abstract

The invention relates to a preparation method of a test article for detecting carboxyatractyloside and / or atractyloside by use of HPLC (High Performance Liquid Chromatography). A tested article extract aqueous solution containing carboxyatractyloside and / or atractyloside and with the pH value of less than or equal to 6 is adsorbed by macroporous adsorption resin, water with the pH value of less than or equal to 6 is used for washing to remove impurities, an alcohol-water solution with the alcohol volume content of 50-70% is used for elution, eluant is collected and a solvent is removed, therefore, the test article is acquired; and the alcohol-water solution for elution is an ethanol-water solution or methanol-water solution. According to the method, impurity interference can be removed sufficiently, the sensitivity and the detection limit are improved, the detected atractyloside ingredient cannot be lost or damaged, the factors such as chromatographic separation effect (separation degree), reproducibility, stability, precision, recovery rate and the like meet the requirements of the standard traditional Chinese medicine quality analytical method.

Description

technical field [0001] The invention relates to a preparation method of a test sample for detecting carboxy atractyloside and / or atractyloside by high performance liquid chromatography. Background technique [0002] Fructus Xanthii is a commonly used poisonous traditional Chinese medicine with a long history of clinical use. It has the effects of dispersing wind and dehumidification, clearing the nose and resuscitating the nose. In recent years, there have been reports of adverse reactions such as kidney, liver, and heart damage or abdominal pain, nausea, and vomiting after taking Xanthium. Regarding the toxic material basis of Xanthium Fructus, modern researches generally believe that its toxic components are mainly water-soluble carboxyatractyloside (CAT, carboxyatractyloside), atractyloside (AT, atractyloside) and their derivatives. [0003] For the components of atractylodes glycosides in Fructus Xanthii, including carboxy atractylodes glycosides, atractylodes glycoside...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 易进海刘鹏刘玉红刘云华黄志芳陈燕
Owner SICHUAN ACAD OF CHINESE MEDICINE SCI
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