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Analysis method for content of 5-chloro-2-methoxycarbonyl-1-indanone ester

A methoxycarbonyl and analysis method technology, applied in the field of analysis of 5-chloro-2-methoxycarbonyl-1-indanone ester content, can solve inaccurate quantitative detection, chromatographic retention time interference, retention time increase, etc. problems, to achieve the effects of improving tailing phenomenon, stable retention time, and improving precision and stability

Active Publication Date: 2021-02-09
JINGBO AGROCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 5-Chloro-2-methoxycarbonyl-1-indanone ester is an intermediate of indoxacarb, but because it has two tautomers of keto and enol, it is difficult to detect. Through research, it is found that It has only one chromatographic peak in chromatographic analysis. It is detected in acidic and neutral mobile phase systems. The chromatographic peak is a broad tailing peak, which cannot be accurately quantitatively detected. In alkaline flow line systems such as triethylamine or ammonia water systems Although the chromatographic peak shape has been improved, the retention time changes very quickly with the pH of the mobile phase, and carbon dioxide in the air will interfere with the chromatographic retention time. With the prolongation of the detection time, the retention time gradually increases, resulting in Detection is unstable, and a diode array detector is used to detect and find that in acidic mobile phase and alkaline mobile phase systems, the ultraviolet spectrum of 5-chloro-2-methoxycarbonyl-1-indanone ester is completely different (see figure 1 and figure 2 ), so it is speculated that 5-chloro-2-methoxycarbonyl-1-indanone esters are two different configurations in the two mobile phase systems. Oxycarbonyl-1-indanone ester content analysis method plays an important role and practical significance in ensuring the quality of indoxacarb products

Method used

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  • Analysis method for content of 5-chloro-2-methoxycarbonyl-1-indanone ester
  • Analysis method for content of 5-chloro-2-methoxycarbonyl-1-indanone ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] 300 batches in production, obtain the toluene solution of 1600 kilograms of product 5-chloro-2-methoxycarbonyl-1-indanone esters, analyze the content of 5-chloro-2-methoxycarbonyl-1-indanone esters in the product, The method includes the following steps:

[0045] (1) Accurately weigh 0.0485g of 5-chloro-2-methoxycarbonyl-1-indanone ester standard substance, put it in a 100ml volumetric flask, add 90ml of acetonitrile, shake and dissolve, dilute to the mark with acetonitrile to obtain the standard substance The solution is ready for use, the mass fraction P of 5-chloro-2-methoxycarbonyl-1-indanone ester in the standard 1 = 99.0%;

[0046] Accurately weigh 0.3461g of the sample to be tested, place it in a 100ml volumetric flask, add 90ml of acetonitrile, shake to dissolve, dilute to the mark with acetonitrile, and obtain the sample solution to be tested for use;

[0047] (2) High-performance liquid chromatography is adopted, the chromatographic column is a SB-C8 chromat...

Embodiment 2

[0062] Small test sample 20200915 batches obtained 97.7g of solid, and the content of 5-chloro-2-methoxycarbonyl-1-indanone ester in the product was analyzed. The method includes the following steps:

[0063] (1) Accurately weigh 0.0521g of 5-chloro-2-methoxycarbonyl-1-indanone ester standard product, put it in a 100ml volumetric flask, add 90ml of acetonitrile, shake and dissolve, dilute to the mark with acetonitrile to obtain the standard product The solution is ready for use, the mass fraction P of 5-chloro-2-methoxycarbonyl-1-indanone ester in the standard 1 = 99.0%;

[0064] Accurately weigh 0.0561g of the sample to be tested, place it in a 100ml volumetric flask, add 90ml of acetonitrile, shake to dissolve, dilute to the mark with acetonitrile, and obtain the sample solution to be tested for use;

[0065] (2) High-performance liquid chromatography is adopted, and the chromatographic column is a SB-C8 reverse-phase chromatographic column. The column length of the chromat...

Embodiment 3

[0072] In production, 306 batches obtained the toluene solution of 1900 kilograms of 5-chloro-2-methoxycarbonyl-1-indanone esters of the product, and analyzed the content of 5-chloro-2-methoxycarbonyl-1-indanone esters in the product. The method includes the following steps:

[0073] (1) Accurately weigh 0.0365 of the standard 5-chloro-2-methoxycarbonyl-1-indanone ester, put it in a 100ml volumetric flask, add 90ml of acetonitrile, shake and dissolve, dilute to the mark with acetonitrile to obtain a standard solution Standby, the mass fraction P of 5-chloro-2-methoxycarbonyl-1-indanone ester in the standard 1 = 99.0%;

[0074] Accurately weigh 0.2456g of the sample to be tested, place it in a 100ml volumetric flask, add 100ml of acetonitrile, shake to dissolve, dilute to the mark with acetonitrile, and obtain the sample solution to be tested for use;

[0075] (2) Adopt high performance liquid chromatography with a diode array detector, the chromatographic column is a SB-C8 c...

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Abstract

The invention belongs to the technical field of chemical analysis and relates to ananalysis method for the content of 5-chloro-2-methoxycarbonyl-1-indanone ester. According to the analysis method, high performance liquid chromatography is adopted to detect the content of the 5-chloro-2-methoxycarbonyl-1-indanone ester; an SBC8 reversed phase chromatographic column is adopted as a chromatographic column; the temperature of the chromatographic column is 30 DEG C to 50 DEG C; a mobile phase is a mixed system of acetonitrile and ammonium carboxylate; the detection wavelength is 230 nm and 270 nm;impurities, a main peak and a solvent peak can be completely separated; the chromatographic peak shape is good; the retention time is stable; the integral calculation result is accurate; the repeatability is good; the reliability of the obtained result is high; and the method is particularly suitable for quality control of pesticide raw drug intermediate products.

Description

technical field [0001] The invention relates to the technical field of chemical analysis, in particular to a method for analyzing the content of 5-chloro-2-methoxycarbonyl-1-indanone ester. Background technique [0002] Indoxacarb is a new type of oxadiazine insecticide with high efficiency and low toxicity developed by DuPont Company of the United States. It has dual effects of contact killing and stomach poisoning, and can effectively solve resistant pests. There is no cross-resistance with other insecticides such as pyrethroids, organophosphorus, and carbamates, and it can well solve the problems of rice leaf rollers, rice stem borers and resistant diamondback moths that are difficult to control in the market. In addition, indoxacarb has a very wide insecticidal spectrum, and one drug can prevent multiple diseases. While preventing and controlling noctuid pests, it also has a good inhibitory effect on mirid bugs, so it is a very good comprehensive management tool. , can ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/54
CPCG01N30/02G01N30/54G01N2030/047
Inventor 许百红成道泉高洪奎王玉莹朱红玉张晓会崔敏孙志武成晓彤
Owner JINGBO AGROCHEM TECH CO LTD
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