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采用超高效液相色谱-串联质谱(UPLC-MS/MS)方法,研究了乙基多杀菌素中2种主要组分(XDE-175-J和XDE-175-L)在稻田水、土壤和水稻植株中的残留分析及消解动态。土壤和植株样品采用乙腈提取,乙二胺-N-丙基硅烷(PSA)净化;田水样品用0.1%甲酸溶液和乙腈稀释;UPLC-MS/MS分析。结果表明:XDE-175-J和XDE-175-L在田水、土壤和植株中的检出限(LOD)分别为2.5×10-4mg/L和5.0×10-4、0.001 mg/kg,定量限(LOQ)分别为0.001 mg/L和0.002、0.005 mg/kg。当添加水平为0.001~0.5 mg/kg(L)时,乙基多杀菌素在田水、土壤和水稻植株中的平均回收率为83%~102%,相对标准偏差(RSD)为1.9%~6.2%。消解动态试验结果表明:6%乙基多杀菌素悬浮剂(SC)按1.5倍推荐使用高剂量(有效成分40.5 g/hm2)于水稻拔节期施药1次,乙基多杀菌素在田水、土壤及水稻植株中的消解动态规律均符合一级动力学方程,半衰期分别为0.35、6.8和1.1 d;施药21 d后,其在水稻植株和田水中的消解率均在95%以上,在土壤中的消解率为86.1%;属易消解型农药。
The effects of two main components of ethyl spinosad (XDE-175-J and XDE-175-L) on water, soil and paddy field were studied by UPLC-MS / MS Residue Analysis and Digestion Dynamics in Rice Plants. Soil and plant samples were extracted with acetonitrile and purified with ethylenediamine-N-propylsilane (PSA); field water samples were diluted with 0.1% formic acid and acetonitrile; UPLC-MS / MS analysis. The results showed that the detection limits (LOD) of XDE-175-J and XDE-175-L in the field water, soil and plant were 2.5 × 10-4mg / L and 5.0 × 10-4,0.001 mg / The limits of quantitation (LOQ) were 0.001 mg / L and 0.002,0.005 mg / kg, respectively. The average recoveries of spinetoram in field water, soil and rice plants ranged from 83% to 102% and the relative standard deviations (RSDs) ranged from 1.9% to 1.0 mg / kg at the additive levels of 0.001-0.5 mg / kg (L) 6.2%. The results of the dynamic test of digestion show that 6% ethyl spinosyn SC (SC) is recommended to use 1.5 times of high dosage (active ingredient 40.5 g / hm2) , The dynamic laws of digestion in soil and rice plants were in accordance with the first-order kinetic equation with half-lives of 0.35, 6.8 and 1.1 d, respectively. After 21 d of application, their digestion rates in rice plants and Tian water were over 95% Soil digestion rate was 86.1%; is a digestion-prone pesticide.