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Method for separating and determining isoxepac and related substances of isoxepac by HPLC (High Performance Liquid Chromatography) method

A technology related to substances, isoxic acid, applied in the field of analytical chemistry, to achieve the effect of strong specificity, accurate sensitivity and high sensitivity

Active Publication Date: 2018-01-16
CHONGQING HUABANGSHENGKAI PHARM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] So far, there is no published method report that can effectively separate the above 7 impurities and other single impurities in isoket acid, and quantitatively determine the analytical method of their existence level

Method used

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  • Method for separating and determining isoxepac and related substances of isoxepac by HPLC (High Performance Liquid Chromatography) method
  • Method for separating and determining isoxepac and related substances of isoxepac by HPLC (High Performance Liquid Chromatography) method
  • Method for separating and determining isoxepac and related substances of isoxepac by HPLC (High Performance Liquid Chromatography) method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] The mensuration of embodiment 1 isoket acid related substances

[0058] 1. Instruments and conditions

[0059] Instrument: High performance liquid chromatography SHIMADZU LC-20A (LC2019);

[0060] Detector: UV detector;

[0061] Chromatographic column: Octylsilane bonded silica gel filler (Agilent Eclipse XDB-C8, 150mm×4.6mm, 5μm);

[0062] Mobile phase: mobile phase A: 0.02mol / L potassium hexafluorophosphate (adjust the pH value to 3.0 with phosphoric acid); mobile phase B: acetonitrile; use mobile phase A and B for linear gradient elution;

[0063] Detection wavelength: 220nm;

[0064] Column temperature: 25°C;

[0065] Flow rate: 1.0ml / min;

[0066] Injection volume: 20 μl.

[0067] The linear gradient elution conditions of mobile phase A and B are:

[0068]

[0069] 2. Experimental steps

[0070] (1) Impurity mixed stock solution: Accurately weigh 12.46mg of p-hydroxyphenylacetic acid, 12.53mg of phthalide, 12.44mg of OLO-SMb, 12.83mg of OLO-Z1a, 12.35mg of...

Embodiment 2

[0086] Example 2 Multiple batches of isoket acid related substances determination results

[0087] According to the method of Example 1, several batches of isoket acid samples of our company were tested for related substances. The calculation results are shown in the table below.

[0088]

[0089]

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Abstract

The invention belongs to the field of analytical chemistry, and particularly relates to a method for separating and determining isoxepac and related substances of isoxepac by an HPLC (High PerformanceLiquid Chromatography) method. A chromatographic column adopted by the method disclosed by the invention adopts octylsilane-bonded silica gel as filler, a mobile phase A and a mobile phase B are adopted to carry out gradient elution, and detection is carried out in a detector; the related substances include one or more of A-G; the mobile phase A is potassium hexafluorophosphate solution, and themobile phase B is organic solvent. The method can effectively separate the seven impurities and other individual impurity in isoxepac and quantitatively determine the existence levels. The method hasthe advantages of high separation degree, high specificity, high sensitivity and accuracy, and is of a great significance in the control of the quality of isoxepac and olopatadine hydrochloride.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for separating and measuring isoket acid and its related substances by HPLC. Background technique [0002] Isoket acid is a synthetic antihistamine and a key starting material for the synthesis of the new preferred antiallergic drug olopatadine hydrochloride. The molecular formula of isoket acid is C 16 h 12 o 4 , the chemical name is 6,11-dihydro-11-oxo-dibenzo[b,e]oxepin-2-acetic acid, and its chemical structure is as follows: [0003] [0004] Its synthetic route is as follows: [0005] [0006] It can be seen from its chemical structural formula and synthetic route that the following impurities may exist in isoket acid: [0007] [0008] [0009] In summary, there are many (7) impurities that may exist in isoket acid, and low wavelengths need to be selected for detection. The establishment of the analytical method requires high require...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 丁雄英唐舒堂
Owner CHONGQING HUABANGSHENGKAI PHARM
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