Characteristic chromatogram of rubia cordifolia charcoal and preparation thereof, construction method of characteristic chromatogram and content determination method

A technology of characteristic map and construction method, which is applied in the fields of characteristic map and its construction method and content determination of madder charcoal and its preparations, can solve the problems of poor peak shape, long detection time and low resolution of fingerprints, and achieve peak shape Good, short detection time, low limit of quantitation effect

Active Publication Date: 2022-05-13
BEIJING KANGRENTANG PHARMA
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Problems solved by technology

[0005] Therefore, the first object of the present invention is to solve the problems of poor peak shape, low peak height, long detection time, and low resolution of the fingerprints obtained when the method in the prior art detects madder charcoal and its preparations, and provides a Rubio charcoal and its preparation characteristic map and its construction method and content determination method of madia charcoal and its preparation

Method used

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  • Characteristic chromatogram of rubia cordifolia charcoal and preparation thereof, construction method of characteristic chromatogram and content determination method
  • Characteristic chromatogram of rubia cordifolia charcoal and preparation thereof, construction method of characteristic chromatogram and content determination method
  • Characteristic chromatogram of rubia cordifolia charcoal and preparation thereof, construction method of characteristic chromatogram and content determination method

Examples

Experimental program
Comparison scheme
Effect test

experiment example 1

[0061] 1. Test drug:

[0062] Rubia charcoal decoction pieces are all commercially available.

[0063] The preparation method of the standard decoction freeze-dried powder of madder charcoal is as follows: take the decoction pieces of madder charcoal, put them in a casserole, soak for 30 minutes, add 7 times the amount of water for decoction once decocting (add 7 ml of water per gram of decoction slices), bring to a boil over high heat, then decoct with slow fire Boil for 30 minutes, filter while hot, cool quickly, and set aside; add 6 times the amount of water to the decoction pieces for the second decoction (add 6 ml of water per gram of decoction pieces), boil with high fire, simmer for 20 minutes, filter while hot, and cool quickly for later use; combine the filtrates , concentrated (65°C), concentrated to a solid-liquid ratio of about 1:1 (relative density of 1.05-1.10 (60°C)), freeze-dried, that is.

[0064] The preparation method of madder charcoal formula granules is ...

experiment example 2

[0105] Experimental Example 2 Methodological Verification

[0106] 1. Precision

[0107] (1) Repeatability

[0108] Adopt Waters UPLC H-Class, TUV detector, get madder charcoal granule (lot number: K469CP01) sample appropriate, grind finely, get 0.5g, get 6 parts, prepare need testing solution by the method under the 2nd item of experimental example 1 and Determination, obtain its characteristic spectrum, take No. 4 peak as the reference peak, calculate its relative peak area and relative retention time. And calculate the RSD, the results are shown in the table below.

[0109] Table 7 Retention time and relative retention time table of madder charcoal repeated investigation

[0110]

[0111]

[0112] Table 8 The peak area and relative peak area table of the repeated investigation of madder charcoal

[0113]

[0114] The repeatability test results show that the relative retention time RSDs of the five identified peaks of the six repeatability test samples are in th...

experiment example 3

[0159] Investigation of Chromatographic Conditions in Experimental Example 3 Content Determination Method

[0160] 1. Test drug

[0161] Same as Experimental Example 1.

[0162] 2. The test method for the content of isocurbisin in madder charcoal preparation

[0163] (1) Preparation of the reference substance solution: take an appropriate amount of the reference substance of isoradicin, accurately weighed, and add 10% by volume methanol aqueous solution to make a reference substance solution containing 30 μg of isorubidin per 1 ml;

[0164] (2) Preparation of the test solution: prepare respective test solutions with madder charcoal, madder charcoal standard decoction freeze-dried powder or madder charcoal formula granules as the test samples, the specific method is as follows: take the test sample and grind it finely, Take about 0.5g, accurately weigh it, put it in a stoppered Erlenmeyer flask, add 20ml of methanol precisely, seal it tightly, weigh it, ultrasonically treat i...

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Abstract

The invention belongs to the technical field of traditional Chinese medicine detection, and particularly provides characteristic chromatograms of charred rubia cordifolia and a preparation thereof, a construction method of the characteristic chromatograms and a content determination method of the charred rubia cordifolia and the preparation thereof, and the construction method of the characteristic chromatograms of the charred rubia cordifolia and the preparation thereof comprises the following steps: (1) preparing a charred rubia cordifolia test solution; (2) the rubia cordifolia carbon test sample solution is taken and detected by adopting a high performance liquid chromatography, octadecylsilane chemically bonded silica is adopted as a filler, acetonitrile and water are adopted as a mobile phase, gradient elution is performed, the gradient elution procedure comprises 0-1 minute, 3 minutes, 9 minutes, 12 minutes and 20 minutes, the volume percent of acetonitrile in the mobile phase is 10%-20%-20%-30%-30%-35%, the volume percent of water in the mobile phase is 10%-20%-20%-30%-30%-35%, and the volume percent of water in the mobile phase is 10%-20%-30%-30%-35%. A specific elution procedure is obtained through a large number of experiment screening, five common characteristic peaks are obtained, effective separation of characteristic peaks containing isoalizarin is achieved, the peak shape is good, a base line is stable, and the detection time is short.

Description

technical field [0001] The invention belongs to the technical field of traditional Chinese medicine detection, and in particular relates to a characteristic map of madder charcoal and its preparation, its construction method and content determination method. Background technique [0002] Rubia is the dry root and rhizome of Rabia cardifolia L., a plant of the Rubiaceae family. It is bitter and cold in nature and belongs to the Liver Meridian. Traumatic hemorrhage, amenorrhea due to blood stasis, arthralgia, swelling and pain from tumbling. Rubia Charcoal is a decoction piece made from the traditional Chinese medicine Rubia Herb fried with charcoal. It is mainly used clinically to treat hematemesis, metrorrhagia, traumatic bleeding and other hemorrhagic diseases caused by blood stasis. The research on the chemical constituents of madder charcoal decoction pieces mainly focused on quinones, tannins, trace elements and so on. Among the quinone components, isorubidin is one of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/86G01N30/34
CPCG01N30/8686G01N30/34Y02A50/30
Inventor 张志强王冬月高扬姜筱璇李蕊董文凤
Owner BEIJING KANGRENTANG PHARMA
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