Quick analysis method for reaction process of emamectin benzoate

A technology of methylamino abamectin and benzoate, which is applied in the analysis field of the intermediate process of chemical reaction, can solve the problems of incomplete monitoring of production process, long high-performance liquid chromatography analysis time, and inability to detect in time, and the like, To achieve the effect of easy operation, saving raw materials and easy operation

Active Publication Date: 2011-05-04
HARBIN INST OF TECH
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  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to solve the problem that the current high performance liquid chromatography analysis takes a long time, the operation steps are cumbersome, the detection is time-consuming, a large number of samples are required for the me...

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  • Quick analysis method for reaction process of emamectin benzoate
  • Quick analysis method for reaction process of emamectin benzoate
  • Quick analysis method for reaction process of emamectin benzoate

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specific Embodiment approach 1

[0009] Specific embodiment one: the rapid analysis method in the emamectin benzoate reaction process of this embodiment is as follows: The abamectin B1a concentration is the sample of 0~25% and the sample of double protective substance concentration is 0.5%~3.5%, set up the sample database; -1 ~4000cm -1 Collect sample spectra within a certain range and establish a sample spectral library; 3. Use the method of combining the average value and normal distribution to select samples with different contents and different reaction times; 4. Use the derivative method and normalization method to predict the selected sample spectra. Treatment; 5. Utilize the methyl and methylene, hydroxyl and amino groups in Abamectin B1a at a wavelength of 8800-4200cm -1 The information of combined frequency and double frequency absorption peaks between these information is used to establish a standard sample model; 6. The partial least squares method is used to establish a quantitative analysis mode...

specific Embodiment approach 2

[0028] Embodiment 2: The difference between this embodiment and Embodiment 1 is that in the process of optimizing the analysis model in step 6, the spectrum interval and the number of principal components are determined according to the model evaluation index determination coefficient and the corrected mean square error. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0029] Specific embodiment three: the difference between this embodiment and specific embodiment one or two is step 2: using a Fourier transform near-infrared spectrum analyzer at a wavelength of 12000cm -1 ~4000cm -1 Collect the sample spectrum within the range, build a sample spectrum library, and the resolution of the Fourier transform near-infrared spectrum analyzer is 8cm -1 , the number of scans is 32 times; step 3: select samples with different contents and different reaction times by means of combining the average value and normal distribution; step 4: use the derivative method and the normalization method to preprocess the selected sample spectrum; Step 5: Use Abamectin B1a methyl group and methylene group, hydroxyl group and amino group at a wavelength of 8800-4200cm -1 The information of the combined frequency and double frequency absorption peaks between these information establishes the standard sample model; Step 6: adopts the partial least squares method to est...

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Abstract

The invention discloses a quick analysis method for a reaction process of emamectin benzoate and relates to an analysis method for a chemical reaction intermediate process. By utilizing the method, the problems that the time for high performance liquid chromatograph is long, the operation steps are minute and complicated, the detection is time-consuming, a large number of samples need to be measured, the provided experimental data often lags behind the production process, the monitoring of the production process is incomplete and problems can not be found in time are solved. The method comprises the following steps: 1) establishing a sample library; 2) establishing a sample spectral pattern library; 3) selecting a sample; 4) carrying out pretreatment on the sample; 5) establishing a standard sample model; 6) establishing a quantitative analysis model, and getting an optimal quantitative analysis model; and 7) collecting spectral information of the sample to be tested, and predicting the contents of residual avermectin B1a and double-protection matter in the sample to be tested through the optimal quantitative analysis model. The analysis of the sample can be completed within 1 minute by the method, thus the method is time-saving, labor-saving and cost-saving and is easy for operation.

Description

technical field [0001] The invention relates to an analysis method for the intermediate process of a chemical reaction. Background technique [0002] Emamectin benzoate (referred to as emamectin benzoate) is a super efficient green insecticide. Starting from avermectin B1a, the emamectin benzoate synthesized by chemical modification has the characteristics of ultra-high efficiency, broad spectrum, near non-toxicity and no residue, and has been widely used in the agricultural field. [0003] At present, the synthesis of emamectin benzoate is mainly through reactions such as oxidation, amination and reduction of abamectin B1a. In the oxidation process, to prevent the hydroxyl group in the abamectin B1a from being oxidized, the hydroxyl group is first protected, but in this process, the degree of the reaction is tested. Routine analysis method checks the content of residual abamectin B1a and the content of abamectin protective substance, usually adopts high performance liquid...

Claims

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Application Information

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IPC IPC(8): G01N21/35G01N21/359
Inventor 姜波黄玉东刘丽
Owner HARBIN INST OF TECH
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