Specific chromatogram of Chinese lobelia and preparation thereof and construction method of specific chromatogram

The technology of a characteristic map and a construction method, which is applied to the characteristic map of Lobelia and its preparations and the field of construction thereof, can solve the problems of not fully reflecting the integrity and characteristics of Lobelia formula granules and other preparations, and achieves good peak shape. , good repeatability and stability, little noise interference

Active Publication Date: 2021-12-07
BEIJING KANGRENTANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Therefore, the object of the present invention is to solve the problem that the characteristic spectrum of lobelia in the prior art cannot provide the chromatographic information and the pair of active ingredients in lobelia formula granules and other preparations simultaneously. Accurate positioning of the characteristic peaks cannot fully reflect the integrity and characteristics of lobelia formula granules and other preparations. A characteristic map and construction method of lobelia and its preparations are provided

Method used

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  • Specific chromatogram of Chinese lobelia and preparation thereof and construction method of specific chromatogram
  • Specific chromatogram of Chinese lobelia and preparation thereof and construction method of specific chromatogram
  • Specific chromatogram of Chinese lobelia and preparation thereof and construction method of specific chromatogram

Examples

Experimental program
Comparison scheme
Effect test

experiment example 1

[0079] 1 optimized chromatographic conditions and the test solution prepared in Experimental Example

[0080] 1, instrument, reagents and trials

[0081] Instrument: Waters Acquity H-Class Ultra Performance Liquid Chromatography; PDA Detector detector; TUV Detector detector; Empower 3 chromatography workstation; ME104E electronic balance (Mettler-Toledo), JY20002 electronic balance (Mettler-Toledo), BSA124S electronic balance (Sartorius instrument Technology (Beijing) Co., Ltd.), BT25S electronic balance (Sartorius instrument Technology (Beijing) Co., Ltd.), KQ-500DB ultrasonic cleaner (Kunshan ultrasonic instrument Co., Ltd.).

[0082] Column:

[0083] Waters ACQUITY Shield RP C18 (2.1 * 100mm, 1.7μm)

[0084] Waters (2.1 * 100mm, 1.6μm).

[0085]Reagent: Lobelia standard soups freeze-dried powder: 190513-221700-01,190513-223800-02,190613-221700-03,190618-223900-08,190618-221200-11,190708-221700-14,190708- 213300-15,190708-226100-16,190708-211600-17,190708-225800-18,190903-221...

experiment example 2

[0126] Lin established standard decoction lyophilized powder characteristic spectrum half Experimental Example 2

[0127] 1, to establish a method to build lobelia characteristic spectrum of lyophilized standard decoction

[0128] 1, lobelia determined according to standard decoction lyophilized powder Experimental Example proteome characterized as follows:

[0129] (1) Preparation of test solution for: lobelia standard decoction take lyophilized powder amount, fine, take about 0.5g, accurately weighed, set stoppered Erlenmeyer flask, water was added precision 25ml, weighed and the weight, sonication (power 250W, frequency 40kHz) 30 minutes, filtered, the filtrate was extracted with ethyl acetate and shaken 2 times 15ml, combined ethyl acetate extracts were evaporated to dryness, the residue amount of methanol to dissolve and dilute to 5ml volumetric flask, filtered, the filtrate, i.e., too.

[0130] (2) HPLC Assay: precision drawing test solution 2 l, into the liquid chromatograp...

experiment example 3

[0166] Experimental Example 3 lobelia standard decoction lyophilized powder was validated feature map

[0167] 1, precision

[0168] (1) Repeatability

[0169] Take lobelia standard decoction lyophilized powder (Lot: 190513-221700-01) 6 parts, measured as in Experimental Example 1 in item 2, characterized in spectrum obtained, peak to peak No. 6 as a reference, to calculate the relative peak area and the relative retention times. And calculate the RSD. The results showed that the relative retention time of each characteristic peak in the range of 0.06 to RSD 1.59% RSD relative peak area in the range of 2.15 ~ 5.31%, indicating good reproducibility of the characteristic spectrum.

[0170] (2) Intermediate precision

[0171] Using Waters UPLC H-Class, TUV detector, taking lobelia standard decoction lyophilized powder (Lot: 190513-221700-01) 6 parts, measured as in Experimental Example 1 in item 2, characterized in spectrum obtained to peak No. 6 as a reference peak, to calculate the...

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Abstract

The invention belongs to the technical field of traditional Chinese medicine detection, and particularly provides a construction method of a specific chromatogram of Chinese lobelia and a preparation thereof. The construction method comprises the steps that (1) a test solution is prepared; (2) the test solution is taken and detected by adopting a high performance liquid chromatography to obtain the specific chromatogram, in the detection process, octadecylsilane chemically bonded silica is adopted as a filler, a mobile phase is an acid-containing aqueous solution-acetonitrile, gradient elution is performed, the gradient elution procedure comprises 0, 20 min, 30 min and 50 min, the volume percentage of acetonitrile in the mobile phase is 12%, 14%, 22% and 35%, six common characteristic peaks are obtained, the diosmetin peaks are separated, the positions of the diosmetin peaks are accurately positioned, the obtained specific chromatogram is stable in base line, low in noise interference and good in characteristic peak shape, the integrity and characteristics of the Chinese lobelia and the preparation thereof are fully reflected, and a basis is provided for quality detection and control of the Chinese lobelia and the preparation thereof.

Description

Technical field [0001] The present invention belongs to the technical field of traditional Chinese medicine detection, particularly relates to one kind of pattern features and Lobelia preparation and construction method. Background technique [0002] Chinese medicine formulations particles is in line with Chinese Herbal Medicine processing standards of quality raw materials, the use of modern high-tech flavor concentrate extracted from the single particle, its taste, Meridian, native drug efficacy and consistent. Chinese medicine granules formulation of reform is part of traditional Chinese medicine, instead of the traditional use Pieces, calling for "Pieces from above the Pieces." In clinical use of the drug to achieve a "safe and efficient, stable and controllable, convenient health." Because of Chinese medicine formulations particles with a small dosage, efficacy, quick, take, carry, easy storage and other features, is very adapt to the needs of modern society, including the i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/86G01N30/06G01N30/34
CPCG01N30/8634G01N30/8686G01N30/06G01N30/34Y02A40/81
Inventor 张志强付静李蕊鲁彤高扬
Owner BEIJING KANGRENTANG PHARMA
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