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Fluorometric determination method for flavoxate hydrochloride

A technique for determination of flavonoid hydrochloride and fluorescence is applied in the field of determination of flavonoid drug content, which can solve the problems of weak fluorescence intensity and low determination sensitivity, and achieves the effects of reduced dosage of medication, simple test conditions and high sensitivity

Active Publication Date: 2015-07-15
HEBEI COLLEGE OF IND & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Fluorometric determination method for flavoxate hydrochloride
  • Fluorometric determination method for flavoxate hydrochloride
  • Fluorometric determination method for 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 (concentrations were all 0.20 mol / L) 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 spectrophotomet...

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Abstract

A fluorometric determination method for flavoxate hydrochloride comprises the steps that a sample solution of a flavoxate hydrochloride tablet is prepared, an FX standard curve with a series of concentration is drawn, and sample concentration is measured; when the sample concentration is measured, the diluted sample solution is heated in a boiling water bath under the strong alkali condition, fluorescence spectrum scanning is conducted on the cooled sample solution by using a fluorescence spectrophotometer, the fluorescence intensity is measured when lambda<ex> / lambda<em> = 302 / 410 nm, and the concentration of FX in the sample solution is calculated. Accordingly, the fluorometric determination method is used for measuring the FX content of the flavoxate hydrochloride tablet, the sensitivity degree is high, the analysis speed is high, the testing conditions are simple and convenient, the environment-friendly effect is achieved, and the needed sample dosage is greatly reduced.

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, Flavoxate hydrochloride, FX) belongs to the flavonoids, is a smooth muscle relaxant, selective for smooth muscle of the genitourinary system Its antispasmodic effect is 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 ...

Claims

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Application Information

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Patent Type & Authority Applications(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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