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采用高效液相色谱(HPLC)法研究了0.2%苄嘧磺隆·丙草胺颗粒剂在稻田环境中的消解动态和最终残留。稻田水、谷壳、稻秆和水稻植株样品用二氯甲烷提取,土壤样品用V(二氯甲烷)∶V(甲醇)=9∶1的混合液提取,糙米样品用V(二氯甲烷)∶V(甲醇)=7∶3的混合液提取后再用二氯甲烷萃取;HPLC法测定。结果表明:当添加水平在0.05~1 mg/kg(或mg/L)时,苄嘧磺隆和丙草胺的平均回收率均在75%~103%之间,相对标准偏差(RSD)为1.6%~13%;苄嘧磺隆和丙草胺的检出限(LOD)均为0.02 mg/L,最小检出量均为4.0×10-10g,在稻田水中的最低检测浓度(LOQ)均为0.001 mg/L,在稻田土壤中的LOQ均为0.005 mg/kg,在水稻植株、谷壳和糙米中的LOQ均为0.01 mg/kg。在水稻移栽后5~7 d,采用直接撒施法在高剂量(270 kg/hm2,其中苄嘧磺隆有效成分为67.5 g/hm2,丙草胺有效成分为472.5 g/hm2)下施药1次的消解动态试验结果表明:在稻田水、土壤和水稻植株中,苄嘧磺隆的消解半衰期分别为5.06~5.83 d、9.76~11.55 d和4.52~4.82 d,丙草胺的消解半衰期分别为5.94~6.45 d、7.70~9.90 d和4.11~4.89 d。分别按低剂量(180 kg/hm2,其中苄嘧磺隆有效成分为45 g/hm2,丙草胺有效成分为315 g/hm2)和高剂量(270 kg/hm2)施药1次,在正常收获期收获的糙米中均未检出苄嘧磺隆和丙草胺残留。
High-performance liquid chromatography (HPLC) method was used to study the digestion kinetics and final residues of 0.2% bensulfuron-methyl-Draconazole granules in paddy field. The samples of paddy field water, chaff, rice straw and rice plants were extracted with dichloromethane. The soil samples were extracted with a mixture of V (dichloromethane): V (methanol) = 9: 1. The brown rice samples were extracted with V (dichloromethane) : V (methanol) = 7: 3 mixture was extracted with dichloromethane extraction; HPLC determination. The results showed that the average recoveries of bensulfuron - methyl and pretilachlor were between 75% and 103% at the level of 0.05-1 mg / kg (mg / L), and the relative standard deviations (RSDs) were The detection limit (LOD) of bensulfuron-methyl and pretilachlor were both 0.02 mg / L and the minimum detection limit was 4.0 × 10-10 g, respectively. The LOQ, And the LOQ of paddy soil was 0.005 mg / kg and LOQ was 0.01 mg / kg in rice plants, chaff and brown rice respectively. Five to seven days after transplanting rice was applied at high doses (270 kg / hm2, of which bensulfuron-methyl was 67.5 g / hm2 and pretilachlor was 472.5 g / hm2) by direct application. The results of one-time digestion dynamic test showed that the half-lives of bensulfuron-methyl were 5.06-5.83 d, 9.76-1 11.55 d and 4.52-4.82 d respectively in Paddy water, soil and rice plants, 5.94 ~ 6.45 d, 7.70 ~ 9.90 d and 4.11 ~ 4.89 d. The animals were treated with low dose (180 kg / hm2, of which the effective content of bensulfuron-methyl was 45 g / hm2, the effective component of pretilachlor was 315 g / hm2) and high dose (270 kg / No residues of bensulfuron and pretilachlor were detected in brown rice harvested at harvest.