Characteristic chromatogram of ground beetle water extract and preparation thereof and construction method of characteristic chromatogram

A construction method and water extract technology, applied in the direction of instruments, measuring devices, scientific instruments, etc., can solve the problems of less characteristic peaks, poor separation effect, unsuitable quality detection, etc., and achieve good peak shape, stable baseline and effective quality detection Effect

Active Publication Date: 2022-05-13
BEIJING KANGRENTANG PHARMA
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  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, since the traditional Chinese medicine formula granules no longer have the characteristics of identifying the properties of decoction pieces, the above method is not suitable for the quality detection of preparations made from the ground beetle water extract such as the ground beetle formula granules. There are few characteristic peaks and the separation effect is poor. High performance liquid chromatography It is still a blank at present to carry out the qualitative detection of the characteristic map to the ground beetle water extraction and preparation thereof, how to improve the detection standard of the wood beetle water extraction and its preparation, and to comprehensively control the quality of the finished product is a technical problem to be solved in the present invention

Method used

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  • Characteristic chromatogram of ground beetle water extract and preparation thereof and construction method of characteristic chromatogram
  • Characteristic chromatogram of ground beetle water extract and preparation thereof and construction method of characteristic chromatogram
  • Characteristic chromatogram of ground beetle water extract and preparation thereof and construction method of characteristic chromatogram

Examples

Experimental program
Comparison scheme
Effect test

experiment example 1

[0054] Investigation of the Construction Method of Experimental Example 1

[0055] 1. Instruments, reagents and reagents

[0056] Instrument: Shimadzu LC-20AD HPLC: PDA detector, Labsolutions chromatographic workstation; Thermo Fisherman Thermo U3000, Chromeleon7 chromatographic workstation; XP26 (Mettler-Toledo), BSA124S electronic balance (Sartorius Scientific Instruments (Beijing) Co., Ltd.), BT25S electronic balance (Sartorius Technology Instrument (Beijing) Co., Ltd.), KQ-500DB ultrasonic cleaner (Kunshan Ultrasonic Instrument Co., Ltd.).

[0057] Chromatographic column: Venusil HILIC (4.6×150mm, 5μm), Waters Atlantis HILIC Silica (4.6*150mm, 5μm).

[0058] Reagent: Wood Beetle Formula Granules can be prepared by conventional methods in the art. For example, in the present invention, it is prepared according to the following steps: take 200 kg of decoction pieces of soil beetle, extract once by boiling (100° C.), and add 12 times the amount of decoction pieces (add water...

experiment example 2

[0141] Experimental Example 2 Methodological Verification

[0142] 1. Repeatability

[0143] Take 6 parts of the ground beetle formula granules (batch number: 20030752), measure according to the method of Example 1, obtain its characteristic spectrum, and take No. 5 peak as the reference peak, calculate its relative peak area and relative retention time. And calculate the RSD. The result is shown below.

[0144] Table 16 Retention time and relative retention time table for the repeatability investigation of characteristic chromatograms

[0145]

[0146] Table 17 Characteristic spectrum repeatability investigation peak area and relative peak area

[0147]

[0148]

[0149] Summary: According to the repeatability investigation results, the relative retention time RSD of each characteristic peak is 0% to 0.8%, and the relative peak area RSD is in the range of 0% to 1.8%, indicating that the characteristic spectrum has good repeatability.

[0150] 2. Intermediate precis...

Embodiment 1

[0179] This embodiment provides a method for constructing a characteristic map of wood beetle formula particles, including the following steps:

[0180] Preparation of the test solution: get an appropriate amount of this product, grind it finely, get about 0.3g, accurately weigh, put in a stoppered Erlenmeyer flask, add 25ml of 30% methanol accurately, weigh, ultrasonically process (power 250W, frequency 40kHz) for 30 minutes, let cool, weigh again, make up the lost weight with 30% methanol, shake well, filter, and take the filtrate to obtain the final product.

[0181] Preparation of reference substance solution: Take an appropriate amount of hypoxanthine reference substance, accurately weigh it, add 30% methanol to make a reference substance solution containing 10 μg per 1 ml, and use it as the reference substance reference solution.

[0182] Each 2 μ l of the above-mentioned ground beetle formula granule need testing solution and reference substance solution is injected int...

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Abstract

The invention belongs to the technical field of traditional Chinese medicine detection, and particularly discloses a ground beetle water extract and a construction method of a characteristic chromatogram of a preparation of the ground beetle water extract, and the construction method comprises the following steps: (1) preparing a test solution; and (2) the test solution is taken and detected by adopting a high performance liquid chromatography, propyl amide bonded silica gel is taken as a filler, a mobile phase comprises an aqueous solution and acetonitrile, a gradient elution procedure comprises 0-10-15 min-17-25 min, and the volume percentage of acetonitrile in the mobile phase is 90-92%-90%-65-88%. Propyl amide bonded silica gel is used as a filling agent, a mobile phase comprises water and acetonitrile, five common characteristic peaks can be obtained only through two elution procedures by optimizing gradient elution procedures, separation of the common characteristic peaks including uracil and hypoxanthine is achieved, the elution procedures are simple, the obtained characteristic chromatogram is stable in base line, and the method is suitable for industrial production. And the characteristic peak is good in shape and high in separation degree.

Description

technical field [0001] The invention belongs to the technical field of traditional Chinese medicine detection, and in particular relates to a characteristic map and a construction method of a water extract of wood beetle and its preparation. Background technique [0002] The ground beetle is the dried female body of Eupolyphaga sinensis Walker or Steleophagaplancyi (Boleny), an insect of the cockroach family, and is a traditional Chinese medicine commonly used in my country. The former is distributed in most parts of the country, while the latter is distributed in Hebei, Henan, Shaanxi, Gansu, Qinghai and Hunan. The wild ones are caught in summer and autumn, and the artificial breeders catch them at any time. After the catch, they are scalded to death with boiling water and dried in the sun. or tumble dry. The medicinal material of ground beetle was first recorded in "Shen Nong's Materia Medica", and was listed as a middle grade. Wood beetle is a species included in the 20...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/86G01N30/34
CPCG01N30/8686G01N30/8631G01N30/34Y02A50/30
Inventor 张志强吉艳慧史国华安琪付静董晨虹
Owner BEIJING KANGRENTANG PHARMA
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