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Method for detecting coumarin components in vitex negundo and radix et rhizoma rhei granules

A technology of coumarin and detection method, which is applied in the field of medicine, can solve the problems that the safety and effectiveness of drugs cannot be guaranteed, and achieve the effect of good peak shape, good reproducibility, and no tailing

Pending Publication Date: 2022-07-01
LUNAN PHARMA GROUP CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are 13 domestic Jingfang granules on the market, and there is no perfect detection method for the determination of active ingredients, and the safety and effectiveness of the drug cannot be guaranteed.

Method used

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  • Method for detecting coumarin components in vitex negundo and radix et rhizoma rhei granules
  • Method for detecting coumarin components in vitex negundo and radix et rhizoma rhei granules
  • Method for detecting coumarin components in vitex negundo and radix et rhizoma rhei granules

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0091] (1) Preparation of reference solution

[0092] Reference substance stock solution: Precisely weigh 50.0 mg of strobilurin reference substance and place it in a 10ml volumetric flask, add 50% acetonitrile to dissolve and dilute to the mark, shake well to obtain stigma glucoside reference substance stock solution. Precisely weigh 12.5 mg of osthole reference substance and 25.0 mg of osthole reference substance, put them in 50ml volumetric flasks, add 50% acetonitrile to dissolve and dilute to the mark, shake well, and then get osthole and osthole Reference stock solution.

[0093] Reference substance positioning solution: Precisely measure 1.0ml of each reference substance stock solution, place them in a 100ml volumetric flask, add 50% acetonitrile to dilute to the mark, and shake well to obtain each reference substance solution.

[0094] Mixed reference substance solution: Precisely measure 1.0ml of each reference substance stock solution, place it in a 50ml volumetric ...

Embodiment 2

[0112] (1) Preparation of reference substance and test solution:

[0113] The reference solution and the test solution were prepared according to the method of Example 1.

[0114] (2) HPLC detection

[0115] The reference substance and the test solution were injected into the high-performance liquid chromatograph respectively, and the determination was carried out according to the following chromatographic conditions:

[0116] Chromatographic column: Ultimate XB-C18 (4.6mm×15cm, 3μm);

[0117] Column temperature: 25℃;

[0118] Mobile phase: acetonitrile-water solution;

[0119] Flow rate: 0.6ml / min;

[0120] Detector: diode array detector;

[0121] Wavelength: 330nm for the detection of floridin, and 200nm for osthole and alba.

[0122] Injection volume: 10 μl;

[0123] Gradient elution is used, and the elution gradient is as follows:

[0124]

[0125] (3) Record the chromatogram, determine the retention time of each component in the reference substance, and calculate...

Embodiment 3

[0129] (1) Preparation of reference substance and test solution:

[0130] The reference solution and the test solution were prepared according to the method of Example 1.

[0131] (2) HPLC detection

[0132] The reference substance and the test solution were injected into the high-performance liquid chromatograph respectively, and the determination was carried out according to the following chromatographic conditions:

[0133] Chromatographic column: Agilent ZORBAX SB-C18 (4.6mm×25cm, 3.5μm);

[0134] Column temperature: 40℃;

[0135] Mobile phase: acetonitrile-water solution;

[0136] Flow rate: 1.0ml / min;

[0137] Detector: diode array detector;

[0138] Wavelength: 340nm for the detection of floridin, and 210nm for the detection of osthole and alba.

[0139] Injection volume: 10 μl;

[0140] Gradient elution is used, and the elution gradient is as follows:

[0141]

[0142] (3) Record the chromatogram, qualitatively determine the retention time of each component ...

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Abstract

The invention belongs to the technical field of medicines, and particularly relates to a method for detecting coumarin components in Jingzhi granules. According to the method, high performance liquid chromatography is adopted for analysis and detection, octadecylsilane chemically bonded silica is used as a chromatographic column of filler, acetonitrile-water is used as a mobile phase, and a diode array detector is adopted for detection. According to the method, the contents of decurrin, osthole and praeruptorin A in the vitex negundo granules are determined by high performance liquid chromatography. The method disclosed by the invention is good in specificity, high in sensitivity, good in reproducibility, accurate and reliable; the chromatographic peaks among the components can be well separated, the peak shape is good, and the trailing phenomenon is avoided.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a method for detecting coumarin components in Jingfang granules. Background technique [0002] The prescription of Jingfang Granules comes from Jingfangbaidu Powder contained in Zhang Shichu's "Recipes for Recovering Lives" in the Ming Dynasty. A total of 11 traditional Chinese medicine composition. In the prescription, Nepeta mustard is mildly warm and divergent, which is good for dispersing wind and relieves the surface; Fangfeng Xinsan is sweet and mildly warm, which is a general medicine for treating wind, good for dispelling wind and dampness, and releasing pain relief. The two must have stronger medicinal power, and are used for treating exogenous wind-cold or damp pathogens, so they are the king medicine. Qianghuo is pungent, warm, bitter and dry, and it mainly enters the bladder meridian, which is good for eliminating wind-cold-damp pathogens above and on t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 张贵民陈小伟姚娜
Owner LUNAN PHARMA GROUP CORPORATION
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