Method for separating and measuring related substances contained in loxoprofen Acid and salt thereof

A loxoprofen acid and assay method technology, applied in material separation, measuring device, analysis material, etc., can solve problems such as no more effective method, and achieve the effects of strong specificity, easy operation, and broad economic benefits

Active Publication Date: 2019-05-07
康美(北京)药物研究院有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] For the related substances introduced in the process of synthesizing loxoprofen sodium and the degraded impurities in the storage process, it is necessary to carry out quality control in the raw material medicine. Therefore, to realize the separation of loxoprofen sodium and its related substances The synthesis of sodium profen sodium and the quality control of the storage process are of great significance, but at present, in terms of quality control, there has not been a more effective method in the prior art

Method used

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  • Method for separating and measuring related substances contained in loxoprofen Acid and salt thereof
  • Method for separating and measuring related substances contained in loxoprofen Acid and salt thereof
  • Method for separating and measuring related substances contained in loxoprofen Acid and salt thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] The specific separation and determination method is carried out according to the following steps:

[0063] Sample preparation: loxoprofen acid and its salt samples were dissolved in a diluent with a concentration of 2 mg / ml, and the loxoprofen acid and its salt samples were injected into the liquid chromatograph;

[0064] Diluent: methanol: [water: triethylamine: glacial acetic acid=1000:1:1]=40:60;

[0065] Column: T3( 4.6×250mm, 5μm);

[0066] Flow rate: 0.5ml / min;

[0067] Detection wavelength: 200nm;

[0068] Column temperature: 20°C;

[0069] Injection volume: 10μl;

[0070] Mobile phase: water phase: water: triethylamine: glacial acetic acid (900:1:1) organic phase: methanol, see Table 2 below for specific elution procedures.

[0071] Table 2 Gradient elution program

[0072]

[0073] The present invention can effectively separate loxoprofen acid and its salt-related substances by adopting T3 chromatographic column, carry out high performance liquid chr...

Embodiment 2

[0075] The specific separation and determination method is carried out according to the following steps:

[0076] Sample preparation: loxoprofen acid and its salt samples are dissolved in a diluent with a concentration of 0.5 mg / ml, and the loxoprofen acid and its salt samples are injected into the liquid chromatograph;

[0077] Diluent: methanol: [water: triethylamine: glacial acetic acid=1100:1:2]=50:50;

[0078] Column: T3( 4.6×250mm, 5μm);

[0079] Flow rate: 1.0ml / min;

[0080] Detection wavelength: 250nm;

[0081] Column temperature: 40°C;

[0082] Injection volume: 30μl;

[0083] Mobile phase: water phase: water: triethylamine: glacial acetic acid (1100:2:1) organic phase: methanol, see Table 3 below for specific elution procedures.

[0084] Table 3 Gradient elution program

[0085]

[0086] The present invention can effectively separate loxoprofen acid and its salt-related substances by adopting T3 chromatographic column, carry out high performance liquid ch...

Embodiment 3

[0088] The specific separation and determination method is carried out according to the following steps:

[0089] Sample preparation: loxoprofen acid and its salt samples were dissolved in a diluent with a concentration of 3 mg / ml, and the loxoprofen acid and its salt samples were injected into the liquid chromatograph;

[0090] Diluent: methanol: [water: triethylamine: glacial acetic acid=900:1:1]=30:70;

[0091] Column: T3( 4.6×250mm, 5μm);

[0092] Flow rate: 2.0ml / min;

[0093] Detection wavelength: 235nm;

[0094] Column temperature: 25°C;

[0095] Injection volume: 20μl;

[0096] Mobile phase: water phase: water: triethylamine: glacial acetic acid (1000:1:2) organic phase: methanol, see Table 4 below for specific elution procedures.

[0097] Table 4 Gradient elution program

[0098]

[0099] The present invention can effectively separate loxoprofen acid and its salt-related substances by adopting T3 chromatographic column, carry out high-performance liquid chr...

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Abstract

The invention provides a method for separating and measuring related substances contained in loxoprofen acid and salt thereof. The method comprises the steps of: injecting loxoprofen Acid and salt thereof samples into a liquid chromatograph for separation and detection, wherein the chromatographic column of the liquid chromatograph is a C8-C18 column, and the mobile phase is an aqueous phase-organic phase mixed in a certain ratio. The method can realize quantitative and qualitative measure of the related substances contained in loxoprofen Acid and salts thereof, thereby the quality of loxoprofen Acid and salt thereof is effectively controlled, and more effective quality monitoring of loxoprofen Acid and salt product thereof is realized. According to the method of the invention, there is practical guiding significance on improving the quality of related products. In addition, the method is strong in specificity, high in accuracy, convenient to operate, and worthy of being widely popularized and applied.

Description

technical field [0001] The invention relates to the field of quality control of loxoprofen acid and its salts, in particular to a method for separating and measuring related substances contained in loxoprofen acid and its salts. Background technique [0002] Loxoprofen acid and its salts are used for the treatment of rheumatoid arthritis, osteoarthritis, low back pain, periarthritis of the shoulder, neck, shoulder and wrist syndrome, anti-inflammatory and analgesic toothache, after surgery, after trauma, and tooth extraction Analgesic and anti-inflammatory, antipyretic and anti-inflammatory for acute upper respiratory tract inflammation. Among loxoprofen and its salts, the most common one is loxoprofen sodium, the chemical name is 2-[4-(2-oxocyclopent-1-ylmethyl)phenyl]propionate sodium dihydrate , formula C 15 h 17 NaO 3 .2H 2 O. The structural formula of loxoprofen sodium is: [0003] [0004] In the process of synthesizing the compound, there are several importa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 乐智勇张书彬冯小院肖慧许冬瑾马兴田
Owner 康美(北京)药物研究院有限公司
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