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A kind of detection method of residual 4-dimethylaminopyridine on equipment

A technology of dimethylaminopyridine and detection method, which is applied to measurement devices, instruments, scientific instruments, etc., can solve the problems of difficulty in sampling, inability to solve the problem of detection of 4-dimethylaminopyridine, and inability to use equipment to clean samples for testing, etc. , to achieve the effect of good stability and increased detection difficulty

Active Publication Date: 2022-04-29
天津天士力圣特制药有限公司
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Problems solved by technology

[0009] Although the detection objectives and methods are similar, Document 1 is only for the detection of common samples and cannot be applied to the testing of equipment cleaning samples
Due to the requirements of the cleaning solvent and the particularity of sampling (sampling needs to be done on the inner wall of the reactor), personnel cannot directly enter the sample detection after cleaning in the pharmaceutical process, and sampling is difficult, and different reactor materials are different, and the sampling effect will be different. To avoid the introduction of other impurities, the sampling solvent needs to be inspected, and more sensitive and safe detection methods are needed for detection. Common methods cannot solve the problem of 4-dimethylaminopyridine detection in the production process of zopiclone / eszopiclone, especially Detection of 4-dimethylaminopyridine after equipment cleaning

Method used

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  • A kind of detection method of residual 4-dimethylaminopyridine on equipment
  • A kind of detection method of residual 4-dimethylaminopyridine on equipment
  • A kind of detection method of residual 4-dimethylaminopyridine on equipment

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Embodiment 1

[0139] Embodiment 1: the detection method of residual 4-dimethylaminopyridine on equipment

[0140] 1. Equipment:

[0141] Reactor 1---Surface area: 8.6m 2 ;Material: enamel;

[0142] Reactor 2 - surface area: 8.6m 2 ;Material: enamel;

[0143] Carbon removal filter 3 --- surface area: 1.5m 2 ;Stainless steel

[0144] 2. Sampling:

[0145] Take 10ml / 100cm 2 / min According to the conversion of the actual rinsing area, take a certain amount of ethyl acetate solvent to evenly rinse the surface of the equipment, receive the eluent, and shake well.

[0146] 3. Solution preparation:

[0147] 3.1 The test solution: sample 1, shake the eluate after the above sampling, take 10ml into the syringe for filtration, filter with a 0.45μm nylon filter membrane, discard 2ml of the initial filtrate, and take the subsequent filtrate to obtain 4- Dimethylaminopyridine test solution.

[0148] 3.2 Reference substance solution:

[0149] ①Contrast solution stock solution: Accurately weigh ...

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Abstract

The present invention relates to the field of analytical chemistry, in particular to a method for detecting residual 4-dimethylaminopyridine on equipment. The method is high-performance liquid chromatography, comprising the following steps: sampling, blank solution, test solution and contrast Product solution preparation, detection.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to a detection method for residual 4-dimethylaminopyridine on equipment. Background technique [0002] 4-Dimethylaminopyridine (DMAP) is a novel high-efficiency catalyst widely used in chemical synthesis, and is often used in acylation reactions with high reaction rates. In addition, it can also significantly increase the rate of various types of reactions such as alkylation, etherification, and esterification, and is widely used in organic synthesis, analytical chemistry, and pharmaceuticals. [0003] 201210327647.6 (CN103664952A) discloses a preparation method of zopiclone, and 201110057090.4 (CN102675319A) discloses a preparation method of eszopiclone. Both documents use 4-dimethylaminopyridine as a catalyst in the synthesis process. 4-Dimethylaminopyridine (DMAP) is used as a catalyst for the synthesis of zopiclone. Due to its high toxicity, the residual amount of 4-dimethyl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/045
Inventor 彭娟娟王宝艺张弘颖郭建新李瑸
Owner 天津天士力圣特制药有限公司
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