Ultra-high performance liquid chromatography method for determining content of rheum lhasaense

An ultra-high performance liquid phase, Lhasa rhubarb technology, applied in measurement devices, material separation, analysis materials, etc., can solve the problems of difficulty in analyzing biological macromolecules and inorganic ions, high daily maintenance costs, and large consumption of mobile phase, etc. Application value, shortening the time of sample analysis and testing, and the effect of saving dosage

Active Publication Date: 2014-04-09
KPC PHARM INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

High-performance liquid chromatography has high analysis costs, requires various packing columns, has small capacity, is difficult to analyze biomacromolecules and inorganic ions, consumes a lot of mobile phase, and the instrument price and daily maintenance costs are expensive, and the analysis time is long

Method used

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  • Ultra-high performance liquid chromatography method for determining content of rheum lhasaense
  • Ultra-high performance liquid chromatography method for determining content of rheum lhasaense
  • Ultra-high performance liquid chromatography method for determining content of rheum lhasaense

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The extract of rhubarb in Lhasa was injected into the ultra-high performance liquid chromatography, and acetonitrile-0.1% phosphoric acid aqueous solution (10:90) was used as the mobile phase for gradient elution. , using the ultra-high pressure liquid chromatography column to separate deoxyrhubarb and other chemical components, so that they can reach the ultraviolet detector in turn and be identified; The response values ​​of glucoside peak and polydatin peak respectively correspond to the injection volume, and the content of each component in the Lhasa rhubarb sample is calculated by comparing the response value with the standard sample.

[0029] 1. Determine the detection wavelength

[0030] The standard samples of deoxyterraein, tristilbene and polydatin were dissolved in methanol to measure the UV spectrum, all of which had UV absorption curves, and the maximum absorption wavelengths of the three components were all between 318.5nm and 319.6nm, so The detection wa...

Embodiment 2

[0035] Take rhubarb from Lhasa and grind it into a coarse powder after drying, accurately weigh about 0.1g, put it in a 150ml conical flask with a stopper, add 50ml of 75% methanol accurately, weigh it, ultrasonic for 30 minutes, make up the lost weight with 75% methanol, Filter with a 0.22μm filter membrane to obtain the test solution.

[0036] Measuring conditions: C-18 chromatographic column of ultra-high pressure liquid phase; gradient elution with acetonitrile-0.1% phosphoric acid solution (10:90) as mobile phase, flow rate 0.61ml / min; column temperature 30°C; detection wavelength 319nm; The injection volume was 0.4 μl. The measurement results are shown in Tables 1 to 3. The chromatograms of each standard sample measured by UPLC are shown in Figure 5. Image 6 shown.

[0037] Table 1: Contents of trizaperone in different batches of rhubarb Lhasa medicinal materials

[0038]

[0039]

[0040] Table 2: Contents of polydatin in different batches of Lhasa rhubarb med...

Embodiment 3

[0045] Embodiment 3: methodological examination

[0046] (1) Reference substance and sample preparation

[0047] 1.1 Preparation of Tristilbene Reference Substance Solution

[0048] Accurately weigh 0.0100 g of tristilbene reference substance, put it in a 50 mL measuring bottle, add ethanol to dissolve and dilute to the mark, shake well, and obtain (each 1 mL contains tristilbene 0.2 mg). Precisely measure 0.50ml, 1.00ml, 1.50ml, 2.00ml, 2.50ml, 3.50ml of the reference substance solution, put them in 10mL measuring bottles, add ethanol to the mark, shake well, and the concentration is 0.01mg / ml, 0.02mg / ml, 0.03mg / ml, 0.04mg / ml, 0.05mg / ml, 0.07mg / ml reference substance solution.

[0049] 1.2 Preparation of polydatin reference solution

[0050] Accurately weigh 0.0100 g of polydatin reference substance, put it in a 50 mL measuring bottle, add ethanol to dissolve and dilute to the mark, shake well, and obtain (each 1 mL contains polydatin 0.2 mg). Precisely measure 0.10ml, 0...

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Abstract

The invention relates to the field of medicament analysis, and discloses an ultra-high performance liquid chromatography method for determining the content of rheum lhasaense. The method comprises the steps of: by taking acetonitrile-0.1% phosphoric acid water solution as a mobile phase, gradiently eluting rheum lhasaense-carried sample solution to enter an ultra-high performance liquid chromatograph; carrying out gradient elution by taking the acetonitrile-0.1% phosphoric acid water solution as a mobile phase; setting a standard sample, determining the response values of deoxyrhaponticin peak, triptophenolide peak, and polydatin peak in the rheum lhasaense sample by using an ultraviolet detector so as to respectively correspond to sample sizes, and calculating the content of ingredients in the rheum lhasaense sample through comparing the size of the response values with a standard sample. According to the method, the analysis and detection time of the sample can be shortened, the method has the characteristics of being good in separation effect, accurate to determine, high in sensitivity, strong in specificity, simple and convenient for an analysis method and the like, is also capable of saving the usage amount of a solvent, thus having great application prospects.

Description

technical field [0001] The invention relates to the field of drug analysis, in particular to an ultra-high performance liquid chromatography method for determining the contents of various components in rhubarb Lhasa. Background technique [0002] Rhubarb Lhasa is a Polygonaceae plant, mainly produced in Tibet, Sichuan, Yunnan and other places, and its rhizomes are dried and used as medicine. At present, through physical and chemical constants and spectral analysis, it has been identified that Lhasa rhubarb contains multiple stilbene components, among which the components with relatively rich content are deoxyrhebin, tristilbene and polydatin. [0003] Deoxyterraetin is 5-hydroxy-4'-methoxystilbene-3-O-glucopyranoside, the chemical structure is as follows: [0004] [0005] Tristilbene is the compound (E)-1-(3,5-dihydroxyphenyl)-2-(3-hydroxy-4-O-β-D-glucopyranosephenyl)ethylene, or 3 ,5,3',4'-tetrahydroxystilbene-3'-O-β-glucoside (also known as 3,5,4'-trihydroxy-stilbene...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 方芳龚云麒陈锦锌
Owner KPC PHARM INC
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