A kind of fluorescence assay method of flavoxate hydrochloride

A technique for the determination of flavoxate hydrochloride and fluorescence, which is applied in the field of determination of the content of flavonoids, can solve the problems of low determination sensitivity and weak fluorescence intensity, and achieve the effects of simple test conditions, reduced dosage, and environmental friendliness

Active Publication Date: 2018-01-02
HEBEI COLLEGE OF IND & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the fluorescence intensity of MFA itself is weak and the surfactant cannot sensitize the compound, the test concentration of MFA methanol solution is 4 μg / mL, and the determination sensitivity is not high

Method used

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  • A kind of fluorescence assay method of flavoxate hydrochloride
  • A kind of fluorescence assay method of flavoxate hydrochloride
  • A kind of fluorescence assay method of flavoxate hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0026] Step a, preparation of sample solution

[0027] Grind the flavoxate hydrochloride tablet and soak it in methanol for more than 12 hours, extract the supernatant and place it in a volumetric flask, dilute it with methanol to form a sample solution, and prepare the flavoxate hydrochloride tablet sample solution with a concentration of 0.10-0.01mg / ml. The methanol is chromatographically pure methanol solution.

[0028] Step b, drawing a standard curve

[0029] Dissolve analytically pure flavoxate hydrochloride with methanol and dilute it into standard solution of different concentrations. The concentration range of the standard solution is 1-10 μg / mL. In a series of 10ml volumetric flasks, add a certain volume of the standard solution, It is used to prepare a series of standard solutions with a gradient concentration, so that the concentration range of the standard solution after constant volume is 0.020-0.500 μg / mL, and the volume percentage of methanol in the standard s...

Embodiment 1

[0040] Instruments used: F-7000 fluorescence spectrophotometer (Hitachi), equipped with 150W xenon lamp, 1cm fluorescent cell, selective excitation and emission slit (slit) of 5.0 nm, UV-29 filter, photomultiplier tube negative high voltage (PMT) ) for 700 V.

[0041] Agent: flavoxate hydrochloride (TCI Japan, F0717, MW: 427.93), prepared with methanol (Tedia Company, Inc. HPLC grade, USA) to prepare 101.4 μg·mL -1 Stock solution, diluted with methanol when used.

[0042] 3-Methylflavone-8-carboxylic acid (Japan TCI, M2371, MW: 280.28), prepared in methanol to 147.2 μg·mL -1 Stock solution, diluted with methanol when used; flavoxate hydrochloride tablets (Jilin Jinheng Pharmaceutical Co., Ltd.).

[0043] Adopt standard curve method to measure the concentration of FX in the sample, described steps are as follows:

[0044] a. Preparation of sample solution

[0045] Grind flavoxate hydrochloride tablets, accurately weigh 0.0509g of powder, place in a 100mL volumetric flask, s...

Embodiment 2

[0065] Effect of Experimental Conditions on Fluorescent Response

[0066] Reagents and instruments used are the same as in Example 1

[0067] 1. The effect of the pH value of the solution on the fluorescence reaction

[0068] In a series of 10 mL volumetric flasks, add the standard solution of FX respectively, and the standard solution of FX is prepared according to step b of Example 1, so that the concentration after constant volume is c FX is 0.4056 μg / mL. A pH buffer solution was added to each volumetric flask to adjust the pH values ​​of different solutions. The pH buffer solution was a Britton-Robinson buffer solution, and a mixed solution of phosphoric acid, boric acid and acetic acid (0.20 mol / L in concentration) was mixed with NaOH solution ( 1.0 mol / L) in a certain proportion. Dilute to about 7 mL with water in a volumetric flask, heat in a boiling water bath for 2 h, cool to room temperature, make up to volume with water, use a fluorescence spectrophotometer to sca...

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Abstract

A fluorescence assay method for flavoxate hydrochloride comprises the following steps: preparing a sample solution of flavoxate hydrochloride tablets, drawing a series of concentration FX standard curves and measuring the sample concentration. When measuring the sample concentration, heat the diluted sample solution in a boiling water bath under a strong alkaline environment, and after cooling, use a fluorescence spectrophotometer to scan the fluorescence spectrum, measure the fluorescence intensity at λex / λem=302 / 410 nm, and calculate the sample solution Concentration of FX in . The invention uses a fluorescence measurement method to measure the FX content in the flavoxate hydrochloride tablets, has high sensitivity, fast analysis speed, simple and convenient test conditions, is environmentally friendly, and greatly reduces the amount of required samples.

Description

technical field [0001] The invention relates to the technical field of drug analysis and detection, in particular to a method for determining the content of flavonoid drugs. Background technique [0002] Flavoxate hydrochloride (3-methylflavone-8-carboxylic acid piperidinyl ester hydrochloride, Flavoxatehydrochloride, FX) belongs to flavonoids, is a smooth muscle relaxant, selective for smooth muscle of the genitourinary system Antispasmodic effect, clinically used in the form of tablets or capsules to treat various lower urinary tract infections or obstructive diseases, and can eliminate lower abdominal pain caused by frequent urination, urgency, urinary incontinence and urethral bladder smooth muscle spasm. Pharmacokinetic studies have shown that FX is rapidly absorbed and metabolized into 3-methylflavone-8-carboxylic acid (MFA) in the body when administered intravenously or orally, and excreted in the urine. There are many methods for quantitative analysis of FX and its ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/64
Inventor 李文红魏永巨李树山郭立达吕芳
Owner HEBEI COLLEGE OF IND & TECH
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