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A HPLC isocratic elution method for simultaneous determination of four components in Semen Cassiae

A technology of isocratic elution and determination method is applied in the field of HPLC isocratic elution and simultaneous determination of the content of four components in Cassia seeds, which can solve the problems of unsatisfactory wave peak separation, cumbersome and complicated processing methods, time-consuming and labor-intensive, etc. Easy to popularize and master, low cost and high efficiency

Active Publication Date: 2021-07-20
北京岐黄科技有限公司
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  • Summary
  • Abstract
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Problems solved by technology

Reported from the literature 【2】 The liquid chromatogram shows that at about 18-19 minutes, the peak of orange cassiatin appears, and that of chrysophanol appears at about 32 minutes, and the separation of the peaks is not ideal
And the pretreatment method of its need testing solution is extremely loaded down with trivial details and complicated, needs methanol heating reflux to extract, takes appropriate amount of extract and evaporates to dryness, residue is then hydrolyzed with dilute hydrochloric acid, hydrolyzate is extracted four times with chloroform, extract is evaporated to dryness again, Make up to volume with solvent
A rough calculation shows that 195ml of organic solvent is needed to process a batch of samples, which takes about 5-6 hours. The method is time-consuming and labor-intensive, and seriously pollutes the environment.

Method used

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  • A HPLC isocratic elution method for simultaneous determination of four components in Semen Cassiae
  • A HPLC isocratic elution method for simultaneous determination of four components in Semen Cassiae
  • A HPLC isocratic elution method for simultaneous determination of four components in Semen Cassiae

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Embodiment

[0033] A. Chromatographic conditions and system suitability test: Octadecylsilane bonded silica gel is used as filler; acetonitrile-methanol-0.1% phosphoric acid with a volume ratio of 49:7:44 is used as mobile phase; detection wavelength: 222nm; column temperature 30°C; the number of theoretical plates is not less than 6000 based on the peak of orange-yellow cassiatin;

[0034] B. Preparation of reference substance solution Take an appropriate amount of orange cassiatin, emodin, chrysophanol and emodin methyl ether reference substance dried in a desiccator for 24 hours, accurately weighed, add methanol to make stock solution, and then take an appropriate amount of stock solution, Add 90% methanol to make a mixed solution containing 0.009 mg of arurinine cassiatin, 0.004 mg of emodin, 0.015 mg of chrysophanol and 0.004 mg of emodin methyl ether per 1 ml, as a reference solution;

[0035] C. The preparation of the test solution depends on 0.5g of cassia medicinal material fine ...

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Abstract

The invention relates to an HPLC isocratic elution method for simultaneously determining the contents of four components in Semen Cassiae. Its features: the sample processing time is only 1 / 9 of the literature, and the organic solvent is only 15% to obtain the test solution, using common chromatographic equipment, isocratic elution, and using a volume ratio of 49:7:44 Acetonitrile-methanol-0.1% phosphoric acid was used as the mobile phase. At 222±1nm, the content of arurin, emodin, chrysophanol and emodin methyl ether in the sample was simultaneously determined. The resolution of each peak met the requirements. Needle, 35 minutes to complete the peak. For the first time, the ordinary isocratic elution replaces the gradient elution that has been implemented; the environmental protection method without concentration, extraction, and evaporation replaces the cumbersome, time-consuming, high-cost, and environmental-polluting reporting method; simple, fast, and precise And the accuracy is improved, the practical range is expanded, the measurement cost is reduced, and it is easy to popularize and master.

Description

technical field [0001] The invention relates to an HPLC isocratic elution method for simultaneously determining the contents of four components in Semen Cassiae. That is, using a common high-performance liquid chromatograph, the four components of cassia cassiae, arurin, emodin, chrysophanol and emodin methyl ether were simultaneously determined by isocratic elution. Background technique [0002] Cassia seed is a commonly used Chinese medicinal material, mainly containing anthraquinones, such as orange cassiatin, emodin, chrysophanol, emodin methyl ether, meicassina, yellow cassiacin, cassiacin, aloe-emodin, etc. Anthraquinone aglycone and its glycosides combined with sugar. There are also naphthopyrrole ketones, fatty acids, amino acids and inorganic elements. It has the effects of clearing away heat and improving eyesight, moistening the intestines and laxative. It is used for conjunctival congestion, astringent pain, embarrassment, excessive tears, headache, dizziness,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/38G01N30/06
CPCG01N30/02G01N30/06G01N30/38G01N2030/045G01N2030/062G01N2030/388
Inventor 安丽娜申玉龙徐达刘勇金艳敏王立伟
Owner 北京岐黄科技有限公司
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