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

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 ...

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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

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