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Method for measuring three active ingredients in Zhikeningsu capsules at same time

An active ingredient, Ningsoujiao technology, applied in the field of medicine, can solve problems such as inability to separate active ingredients, corrosion of instruments and chromatographic columns, harsh chromatographic conditions, etc., and achieve good peak shape, high resolution, reproducibility and stability Good results

Inactive Publication Date: 2017-10-13
JILIN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, due to the high concentration of acetic acid in the mobile phase, the above chromatographic conditions will corrode the instrument and the chromatographic column during the measurement process; at the same time, the flow rate needs to be controlled at 0.35mL min -1 , which also has certain requirements for the selection of instruments, and the chromatographic conditions are too harsh
Most importantly, there are many components in Zhike Ningsou Capsules. Under the above-mentioned chromatographic conditions, there is still a single sample peak that is not completely separated between the chromatographic peaks of chlorogenic acid and hesperidin, and it is impossible to separate the components in Zhike Ningsou Capsules. Other active ingredients are efficiently separated

Method used

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  • Method for measuring three active ingredients in Zhikeningsu capsules at same time
  • Method for measuring three active ingredients in Zhikeningsu capsules at same time
  • Method for measuring three active ingredients in Zhikeningsu capsules at same time

Examples

Experimental program
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Effect test

Embodiment 1

[0027] (1) Preparation of the mixed reference solution: accurately weigh 0.00234g of chlorogenic acid, 0.00230g of hesperidin and 0.00305g of hyperin, place them in a 5mL volumetric flask, dissolve them with methanol and set the volume to the mark ; The prepared concentration was 468μg·mL -1 , 460μg·mL -1 and 610μg·mL -1 standard solution; respectively pipette 150 μL of each standard solution and mix to prepare a mixed reference solution;

[0028] (2) Preparation of the test solution: take 16 Zhike Ningsou capsules, remove the shell of the capsule, accurately weigh 4.18535g, use 80mL methanol as solvent for Soxhlet extraction for 5h, cool the extract to room temperature and transfer to 100mL capacity In the bottle, dilute methanol to the volume, and use it as the test solution for detection;

[0029] (3) Chromatographic conditions: Chromatographic column: TC-C 18 (4.6mm×250mm, 5μm); mobile phase: A is acetonitrile, B is gradient elution with 0.2% glacial acetic acid aqueou...

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Abstract

The invention provides a method for measuring three active ingredients in Zhikeningsu capsules at the same time. The method comprises the specific steps that firstly, chlorogenic acid, hesperidin and hyperoside are precisely weighed, then placed in 5 mL volumetric flasks respectively and dissolved with methyl alcohol respectively, the volume is set to the calibration line, standard substance solutions are prepared respectively, then the standard substance solutions are transferred respectively to be mixed, and a mixed reference substance solution is prepared; secondly, the Zhikeningsu capsules are obtained, the capsule shells are removed, precise weighing is conducted, Soxhlet extraction is conducted by using methyl alcohol as a solvent for 5 h, the extracting solution is cooled to the room temperature, then transferred to a 100 mL volumetric flask for volume setting with methyl alcohol and used as a test sample solution, and the test sample solution is used for detection; thirdly, separation detection is conducted, wherein the TC-C18 chromatographic column is used, acetonitrile as a mobile phase A and a 0.2% glacial acetic acid water solution as a mobile phase B are used for gradient elution, the flow velocity is 1.0 mL.min<-1>, the VWD is adopted to detect the wave length, the wavelength is 327 nm within 0-10 min, the wavelength is 280 nm within 10-48 min, the column temperature is 25 DEG C, and the sample size is 10 microliter. The method is simple in operation, reliable in result and capable of providing a reference basis for the quality control over the Zhikeningsu capsules.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a method for detecting active ingredients in Zhike Ningsou capsules, a Chinese patent medicine, specifically a method for simultaneously measuring three active ingredients in Zhike Ningsou capsules by switching wavelengths. Background technique [0002] Zhike Ningsou Capsules are included in the "Drug Standards of the Ministry of Health Traditional Chinese Medicine Prescriptions (Volume Ninth)". It is composed of 11 traditional Chinese medicines such as bitter almond, windproof, bellflower, Nepeta, and tangerine peel. Table, the efficacy of antitussive and expectorant, clinically used for symptoms such as wind-cold cough, vomiting, sore throat. [0003] At present, it has been reported that the content of hesperidin, bitter almond or hesperidin and chlorogenic acid in Zhike Ningsou capsules has been determined by HPLC. For example: the sample is ultrasonically extracted with meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/74
CPCG01N30/06G01N30/74
Inventor 孙艳涛赵磊崔克宇王丽王龙赵艳方袁美玉
Owner JILIN NORMAL UNIV
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