Analysis method for qualitatively analyzing unknown impurities in 3'-methoxypropiophenone process by using gas chromatography-mass spectrometry method
A methoxybenzene and gas chromatography-mass spectrometry technology, applied in the field of chromatographic analysis, can solve the problems such as the impurity qualitative method has not been involved, and achieve the effects of easy popularization, fast analysis speed and small error
Active Publication Date: 2021-01-22
JINAN ENLIGHTEN BIOTECH CO LTD +1
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Problems solved by technology
[0006] Gas chromatography is used in the published articles on the detection of m-methoxypropiophenone impurities, but the qualitative methods for impurities existing in the process have not been involved
Method used
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Embodiment 1
[0041] Utilize the analysis method of unknown impurity in m-methoxypropiophenone process by GC-MS, comprising the following steps:
[0042] (1) By-product impurities are prepared into the sample solution to be tested after enrichment; 5Kg m-methoxypropiophenone is distilled off by means of vacuum distillation, and the remaining still material (0.8g) is the impurity component after enrichment;
[0043] Wherein, the concrete condition of underpressure distillation: pressure is 1mm mercury column, T 内温 From 100°C to 150°C, T 汽温 From 90°C to 140°C.
[0044] (2) Use gas chromatography-mass spectrometry to test the sample solution to be tested:
[0045] Described gas chromatography-mass spectrometry instrument is: SHIMADZU GC / MS-QP2010 gas chromatography-mass spectrometry instrument;
[0046] Gas chromatography column: weak polarity column Rxi-1ms, column length 30m, inner diameter 0.25mm, film thickness 0.25μm;
[0047] Gas phase parameters: inlet temperature: 250°C; detector t...
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Abstract
The invention belongs to the field of chromatographic analysis, and relates to an analysis method for qualitatively analyzing unknown impurities in a 3'-methoxypropiophenone process by using a gas chromatography-mass spectrometry method. The analysis metehod comprises the following steps: removing 3'-methoxypropiophenone to be detected by reduced pressure distillation, and dissolving the residualkettle material, namely enriched impurity components, in an organic solvent to form a sample solution to be detected; and qualitatively analyzing impurity components of the to-be-detected sample solution by adopting a gas chromatography-mass spectrometry method, and performing analyzing to obtain a chemical structure of the impurity. The method for determining the chemical structure of the unknownimpurity in the 3'-methoxypropiophenone process is simple, convenient, accurate and reliable. A universal weak-polarity gas chromatographic column is adopted, a mass spectrum detector is adopted foranalyzing and detecting spectral peak information of impurities, and components contained in the impurities are judged. The method is high in analysis speed, low in detection limit, small in error, sharp in spectrogram peak pattern and good in symmetry. The method can be used as a qualitative detection means for unknown impurities in the 3'-methoxypropiophenone product process, and provides a technical basis for improvement of the production process and determination of the product quality.
Description
technical field [0001] The invention belongs to the field of chromatographic analysis, and in particular relates to an analysis method for identifying unknown impurities in m-methoxypropiophenone process by gas chromatography-mass spectrometry. Background technique [0002] The information disclosed in this background section is only intended to increase the understanding of the general background of the present invention, and is not necessarily taken as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to those skilled in the art. [0003] The yield of m-methoxypropiophenone is very high, and the amount of impurities generated is very small. But even so, there is still unavoidable generation of by-products in the whole process, and considering that the amount of by-products is very small, it has always been very difficult to enrich by-products, and it is even more difficult to characterize them. So far, there is no rep...
Claims
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Login to View More IPC IPC(8): G01N30/08G01N30/88
CPCG01N30/08G01N30/88
Inventor 姜瑞古静燕卫洁李新徐道林张磊孙越
Owner JINAN ENLIGHTEN BIOTECH CO LTD