Piroxicam hapten and preparation method and application thereof

A technology of piroxicam and hapten, which is applied in the direction of material inspection products, instruments, analytical materials, etc., to achieve the effect of simple raw material components, low detection cost, and easy experimental operation

Inactive Publication Date: 2019-10-15
SHENZHEN BIOEASY BIOTECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no relevant report on piroxicam hapten in China at present

Method used

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  • Piroxicam hapten and preparation method and application thereof
  • Piroxicam hapten and preparation method and application thereof
  • Piroxicam hapten and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A kind of preparation method of piroxicam hapten:

[0034] 1) Take saccharin and ethyl bromoacetate mixed reaction to make intermediate product 1:

[0035] Weigh 13g of saccharin and dissolve it in 25mL of DMF, add 1.8g of NaH in batches under an ice bath, stir for 10min, then slowly add 6.5g of ethyl bromoacetate dropwise, react at room temperature for 1h, and then react at 80°C for 2.5h. After cooling down in an ice bath, pour the mixture into 100ml of ice water, filter the precipitated solid with suction, wash with water, and dry to obtain a white solid powder which is the intermediate product 1;

[0036] 2) intermediate product 2 is obtained after mixing intermediate product 1 with DMSO and MeONa and extracting:

[0037] Add 6g of intermediate product 1 to a mixed solution of DMSO (23ml) and MeONa (2.60g), control the temperature at less than 30°C, stir for 1h, and the color of the solution changes from yellow to brown; pour the reaction solution into 50ml of 3N hy...

Embodiment 2

[0045] A kind of preparation method of piroxicam hapten:

[0046]1) Take saccharin and ethyl bromoacetate mixed reaction to make intermediate product 1:

[0047] Weigh 10 g of saccharin and dissolve it in 20 mL of DMF, add 1.5 g of NaH in batches under an ice bath, and slowly add 6.07 g of ethyl bromoacetate dropwise after stirring for 10 min, react at room temperature for 1 h, and then react at 80°C for 2.5 h. After cooling down in an ice bath, pour the mixture into 100ml of ice water, filter the precipitated solid with suction, wash with water, and dry to obtain a white solid powder which is the intermediate product 1;

[0048] 2) intermediate product 2 is obtained after mixing intermediate product 1 with DMSO and MeONa and extracting:

[0049] Add 5g of intermediate product 1 to a mixed solution of DMSO (20ml) and MeONa (2.45g), control the temperature at less than 30°C, stir and react for 1h, the color of the solution changes from yellow to brown; pour the reaction soluti...

Embodiment 3

[0057] A kind of preparation method of piroxicam hapten:

[0058] 1) Take saccharin and ethyl bromoacetate mixed reaction to make intermediate product 1:

[0059] Weigh 20g of saccharin and dissolve it in 40mL of DMF, add 3g of NaH in batches under an ice bath, stir for 10min, then slowly add 12g of ethyl bromoacetate dropwise, react at room temperature for 1h, and then react at 80°C for 2.5h. After cooling down in an ice bath, pour the mixed solution into 200ml of ice water, filter the precipitated solid with suction, wash with water, and dry to obtain a white solid powder which is the intermediate product 1;

[0060] 2) intermediate product 2 is obtained after mixing intermediate product 1 with DMSO and MeONa and extracting:

[0061] Add 10g of intermediate product 1 to a mixed solution of DMSO (40ml) and MeONa (5g), control the temperature at less than 30°C, stir and react for 1h, the color of the solution changes from yellow to brown; pour the reaction solution into 100ml...

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Abstract

The invention aims to provide a piroxicam hapten and a synthesis method and application thereof, belonging to the field of drug safety detection. The preparation method comprises the following steps:1) mixing saccharin and ethyl bromoacetate for reacting to prepare an intermediate product 1; 2) mixing and extracting the intermediate product 1 with DMSO and MeONa to obtain an intermediate product2; 3) mixing the intermediate product 2 and CH3I for reacting to obtain an intermediate product 3; 4) mixing the intermediate product 3 and 6-aminonicotinic acid methyl ester for reacting to obtain anintermediate product 4; 5) after adding of the intermediate product 4 into a reagent for miscibility reaction, purifying to obtain the final product, namely the piroxicam hapten. Immunological detection method has the advantages of high sensitivity, strong specificity, simple sample pretreatment, short detection time, strong stability, no need of special equipment and reagents, intuitive judgmentof results and the like, thus being particularly suitable for rapid detection of illegal addition of piroxicam chemical drugs in vast basic inspection personnel and large quantities of anti-rheumatism Chinese patent medicines.

Description

technical field [0001] The invention belongs to the technical field of drug safety detection, and in particular relates to a piroxicam hapten and a preparation method and application thereof. Background technique [0002] Piroxicam (chemical name is 2-methyl-4-hydroxy-N-(2-pyridyl)-2H-1,2-benzothiazine-3-carboxamide 1,1-dioxide, molecular formula is C 15 h 13 N 3 o 4 S), is a benzothiazine non-steroidal anti-inflammatory analgesic and antipyretic drug for rheumatoid, rheumatoid arthritis, ankylosing spondylitis, osteoarthritis, gout, migraine and neuralgia, with Obvious analgesic, anti-inflammatory and detumescence effects. Illegal addition of piroxicam in anti-rheumatic Chinese patent medicines and health food is not uncommon, but long-term use can cause neutropenia, eosinophilia, dizziness, abnormal liver function, thrombocytopenia, toxic epithelial necrosis, and nausea , stomach pain, intestinal bleeding and other side effects. [0003] The main analysis methods of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D417/12G01N33/531G01N33/68
CPCC07D417/12G01N33/531G01N33/6854
Inventor 杨星星王炳志付辉金虹张鑫周巧妮颜文豪魏世塨陈奕耀陈立
Owner SHENZHEN BIOEASY BIOTECHNOLOGY CO LTD
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