Rhizoma bletillae small molecule characteristic fingerprint spectrum analysis method

A characteristic fingerprint and spectrum technology, applied in the field of pharmaceutical analysis, can solve problems such as different liquid phases and no standard products

Pending Publication Date: 2020-09-18
SUZHOU QINGLAN BIOMEDICAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no standard contrast in this prior art, and the conditions of the liquid phase are also completely different, including wavelength, etc., and even the obtained chromatographic peaks are completely different from the present application

Method used

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  • Rhizoma bletillae small molecule characteristic fingerprint spectrum analysis method
  • Rhizoma bletillae small molecule characteristic fingerprint spectrum analysis method
  • Rhizoma bletillae small molecule characteristic fingerprint spectrum analysis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0134] Embodiment 1: white and test sample solution preparation

[0135] (1) Selection of different extraction solvents

[0136] ①Preparation of test sample solution: Accurately weigh three parts of Baiji sample, pulverize, pass through a No. 4 sieve to obtain 1.00g of Baiji powder, put it in a 100mL conical flask with a stopper, add pure water, 75% methanol, Ethanol 25mL, ultrasonic at room temperature for 30min, ultrasonic power 280W, frequency 40KHz, let cool, shake well, filter with 0.45μm microporous membrane to obtain the standard sample solution.

[0137] ②HPLC analysis conditions: C18 chromatographic column (250mm*4.6mm, 5μm); mobile phase adopts binary gradient elution system, phase A: 0.2% formic acid, phase B: acetonitrile; detection wavelength 280nm; column temperature 35℃ ; The elution gradient is shown in Table 1, the flow rate is 1.0 mL / min, and the injection volume is 10 μL.

[0138] Table 1 White and elution gradient

[0139]

[0140] ③Fingerprint establ...

Embodiment 2

[0169] Embodiment 2: white and chromatographic conditions are determined

[0170] (1) Selection of different column temperatures

[0171] ①Preparation of test sample solution: Accurately weigh the white powder, crush it, pass through a No. 4 sieve to obtain 1.00 g of white powder, put it in a 100 mL conical flask with a stopper, add 25 mL of 75% methanol, and ultrasonicate for 30 minutes at room temperature. Ultrasonic power 280W, frequency 40KHz, let cool, shake well, filter with 0.45μm microporous membrane to obtain standard sample solution.

[0172] ② HPLC analysis conditions: compare the influence of different column temperatures of 25° C., 35° C., and 45° C. on the separation performance, and other conditions are the same as in Example 1 (1) and ②.

[0173] ③Fingerprint establishment and result analysis: The higher the temperature, the better the chromatographic peaks of Baiji's fingerprint, but considering that higher column temperature will affect the life of the colum...

Embodiment 3

[0196] Embodiment 3: Determination of white and fingerprint spectrum methodology

[0197] (1) Determination of precision of white and fingerprint spectrum

[0198] ①Preparation of test sample solution: Accurately weigh the white powder, crush it, pass through a No. 4 sieve to obtain 1.00 g of white powder, put it in a 100 mL conical flask with a stopper, add 25 mL of 75% methanol, and ultrasonicate for 30 minutes at room temperature. Ultrasonic power 280W, frequency 40KHz, let cool, shake well, filter with 0.45μm microporous membrane to obtain standard sample solution.

[0199] ②HPLC analysis conditions: Agilent 1200LC HPLC; Stamsil-BpC18 column (250mm*4.6mm, 5μm); mobile phase adopts binary gradient elution system, phase A: 0.2% formic acid water, phase B : Acetonitrile; detection wavelength 280nm; column temperature 35°C; elution gradient as shown in Table 1, flow rate 1.0mL / min, injection volume 10μL.

[0200] 3. Get the same batch of Baiji sample, after preparing it acco...

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Abstract

The invention provides a rhizoma bletillae characteristic fingerprint establishing method and a rhizoma bletillae detection method. A rhizoma bletillae characteristic fingerprint is obtained. The method is simple in condition, accurate in result and good in reproducibility, meets the fingerprint spectrum precision test requirement, and is good in sample stability within 24 hours. Therefore, the method can comprehensively reflect the variety and quantity of chemical small molecule components contained in the rhizoma bletillae medicinal material. Meanwhile, the three selected common chromatographic peaks can objectively reflect the internal quality of rhizoma bletillae and serve as quality control indexes of rhizoma bletillae.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, and relates to a method for establishing fingerprints of traditional Chinese medicinal materials, in particular to establishing a method for analyzing characteristic fingerprints of white and small molecules, and the characteristic fingerprints of white and small molecules obtained by the method. Background technique [0002] Baiji is the dry tuber of Bletilla striata (Thunb.) Reichb.f., a plant of the family Orchidaceae, also known as Galangal and Violet. Li Shizhen explained its name and said: Its roots are white, and grow together, so it is called Baiji. It has been recorded in "Shen Nong's Materia Medica", and it has become one of the varieties collected in various editions of Pharmacopoeia since 1963. Its taste is bitter, sweet, astringent, flat and cool in nature, and it belongs to the lung, stomach and liver meridians. Baiji has the functions of nourishing the lungs, stopping bleed...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/86
CPCG01N30/02G01N30/8631G01N30/8686
Inventor 姜双英谭以正郑美玲于颖
Owner SUZHOU QINGLAN BIOMEDICAL TECH CO LTD
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