Study On Establishment Of Novel Imported Pesticide Evaluation System And Detection Technology

With the development of technology in the application of agriculture, the pesticide application in agricultural production is becoming more and more widely. Traditional pesticide has the characteristics of high toxicity, low activity and large dosage. It will result in the environmental pollution of soil, air and water, and the destruction of ecological environment and even lead to problems such as excessive pesticide residues in foods if it was used unreasonably. To improve people’s living environment and quality of life, research and development for novel pesticides featured with board, high effect, low toxicity and minimum pollution have been showing an increasing trend. Meanwhile, pesticides are toxic and harmful chemicals whose applications are highly restricted; the content of effective components in a pesticide would determine its superiority and is the most significant test item and evaluation indicator for the quality of pesticides.Compared to foreign research institutions, there is a big gap in China for developing new technology of pesticide detection. In this paper, the determination technology of the qualitative and quantitative analysis for the great number of standard samples of novel imported pesticides in recent years has been studied. The main research contents are included in this paper shown as follows.1. The establishment of novel imported pesticide evaluation system. The three methods including IR, 1H-NMR, and LC-Q/TOF MS were used for the qualitative analysis of the standard sample composition of 63 kinds of novel imported pesticides. The three spectrograms were analyzed to establish the qualitative evaluation method of standard samples. And the results showed that the pesticides with the same type of structures had certain rules in the analysis spectrograms. In addition, the correlative standard of the active ingredient testing and non-standard literature methods of the hundreds of pesticides from all over the world were collected. According to their chemical structures, physical and chemical properties, all of the pesticides were classified, and “Novel Pesticides Detection Instruction Manual” was composed. And then, represented by three typical novel pesticides, the aveluation system for the detection methods of pesticides was established.2. The qualitative analysis of triazolopyrimidine sulfonamides herbicides. Represented by Flumetsulam, Florasulam, and Penoxsulam, their infrared absorption spectrograms were obtained with KBr pellet, and their characteristic absorption peaks were 3350 cm-1 or 3180 cm-1, 1630 cm-1, 1600 cm-1, near 1500 cm-1(two peaks), 1380 cm-1, 1300 cm-1, 1150 cm-1(two strong and sharp peaks). Nuclear magnetic resonance spectrograms were attained with deuterated dimethyl sulfoxide as the solvent to collect 1H-NMR signals. 1H-NMR characteristic peaks were δH 3.86~4.24 ppm(s,-OCH3 hydrogen), δH 7.46~9.83 ppm(Pyrimidine rings hydrogen), δH 10.82~11.91 ppm(s,-NHSO2 hydrogen). Mass spectra obtained by LC-Q/TOF MS showed that sulfamine bridging group was easy to break mostly, and the characteristic ion fragments of m/z 129 or m/z 195 were their common features.3. The quantitative analysis of Sulfoxaflor, Cyantraniliprole and Prodiamine. 1) A HPLC method was developed for the determination of active ingredient content in sulfoxaflor suspension concentrate and water dispersible granule. The chromatographic conditions were systematically investigated with C18 column as the stationary phase, the mixture of acetonitrile and acetic acid as the mobile phase at 260 nm. The relative standard deviations(RSD, n=6) were 0.160%, 0.087%, the recoveries were 98.86%~101.0%, 99.02%~100.2%. 2) A HPLC method was developed for determination of active ingredient content in cyantraniliprole oil-based suspension concentrate, with C18 column at 270 nm, and methanol-acetic acid aqueous solution was used as the mobile phase. The relative standard deviation(RSD, n=6) was 0.186%, the recovery was 99.92%~100.5%. 3) The GC and HPLC methods were developed for the simultaneous determination of active ingredient content in prodiamine water dispersiber granule. The GC conditions were determined with Di-N-pentyl phthalate as internal standard, DB-5 as the chromatographic column and FID as the detector. The HPLC conditions were determined with C18 as the chromatographic column, and acetonitrile-acetic acid solution as the mobile phase. The relative standard deviations(RSD, n=6) were 0.280%, 0.398%, the recoveries were 98.9%~100.6%, 99.2%~100.9%. It is showed that these methods both have high precision and accuracy, also the operation is simple and fast, which are suitable for the demands of daily quantitative analysis.