水稻、土壤和田水中氟啶脲残留检测与消解动态研究  

Residue detection and degradation of chlorfluazuron in rice,soil and field water

作　　者：霍九春[1] 孙扬[1] 徐应明[1] 秦旭[1] 戴晓华[1] 魏丹[1] 

机构地区：[1]农业部环境保护科研监测所污染防治研究室,农业部/天津市产地环境与农产品安全重点开放实验室,天津300191

出　　处：《安全与环境学报》2010年第6期13-18,共6页Journal of Safety and Environment

基　　金：农业部农药登记残留试验项目(2008P340)

摘　　要：为了解氟啶脲在水稻、土壤和田水中的消解动态及其残留状况,建立了氟啶脲在水稻、土壤和田水中的液相色谱检测方法,并在天津、浙江杭州和广西南宁开展了两年氟啶脲在水稻和土壤中消解动态规律和残留状况田间试验。结果表明,采用乙腈提取水稻稻米、稻壳和茎叶样品,丙酮提取土壤和田水样品,液相色谱仪带紫外检测器测定,外标法定量,在0.03～1mg·kg^(-1)添加水平范围内,水稻、土壤和田水中氟啶脲的平均添加回收率为84.94%～98.73%,变异系数为2.84%～9.44%;水稻、土壤和田水中氟啶脲的最小检出量为5.6×10^(-11)g,最低检出质量比为:茎叶0.01mg·kg^(-1),稻壳0.01mg·kg^(-1),稻米和土壤0.005 mg·kg^(-1),田水0.003 mg·kg^(-1)。田间试验表明,氟啶脲在水稻、土壤和田水中残留消解动态规律符合方程C_t=C_0e^(-kt);氟啶脲·三唑磷31%乳油在水稻茎叶、土壤和田水中的消解半衰期分别为6.27～7.83 d、5.28～7.36 d和6.01～7.06 d。最终残留试验结果表明,在水稻上手动喷雾施药氟啶脲·三唑磷31%乳油,按推荐剂量325.5g^(a.i.)·hm^(-2)和1.5倍推荐剂量488.25g^(a.i.)·hm^(-2)施药,兑水喷雾处理1～2次,两次施药间隔为7 d,距最后一次施药采收间隔期为35 d时,氟啶脲在水稻稻米和土壤中的残留量分别为ND～0.028 0mg·kg^(-1)和ND～0.014 8 mg·kg^(-1)。参照日本"肯定列表制度"规定氟啶脲在稻米中的最大允许残留限量MRL值为0.05 mg·kg^(-1),按照1.5倍推荐剂量在水稻上施药1～2次,其有效成分之一氟啶脲在水稻稻米中残留是安全的。The paper studied the analytical methods and residues of chlorfluazuron in rice field water, soil, plant, rice shell and unpolished rice. Chlorfluazuron residue was extracted by acetnnitrile in plant, rice shell and unpolished rice, and by acetone in soil and rice field water, and determined by HPLC equipped with a UV detector. The experimental results showed that the average recoveries of ehlorfluazuron stood with a range of 87.93%- 97.18%, 90.44%- 95.38%, 84.94% - 89.30%, 87.96%- 89.79% and 92.21%- 98.73% with their relative standard deviations of 2.84%- 8.50%, 4.52%-9.40%, 4.79%-7.51%, 3.15%-8.30% and 3.81%- 7.94% in rice field water, soil, plant, rice shell and unpolished rice. Limit of detection was 5.6 × 10^-11 g and the lowest concentrations detected were 0.01 mg· kg^-1 in plant and rice shell, 0.005 mg·kg^-1 in unpolished rice and soil, and 0.003 mg·kg^-1 in rice field water, respectively. An control and contrast trial experiment in Tianjin, Zhejiang province and Guangxi was done. The degradation of chlorfluazuron in plant, soil and rice field water could be described with equation： Ct = C0e^- kt. The half-life of chlorfluazuron turns to be 6.27-7.83 d, 5.28 -7.36 d and 6.01 -7.06 d in plant, soil and rice field water, respectively. The results demonstrate that chlorfluazuron belonged to non-persistent pesticides （ T1/2 〈 30 d） . Be- yond this, according to the field experiment, when 31% chlorfluazuron ＆ triazophos EC was applied once and twice at an interval of 7 d with the dosages of 325.5 - 488.25 g^a.i.· hm^-2 during its whole culture process. At the 35th day after the last application, the final residues of the chlorfluazuron were ND - 0. 028 0 mg · kg^- 1 in rice and ND- 0.014 8 mg·kg^-1 in soil. According to Japanese standards, The Maximum Residue Limits（MRLs） for chlorfluazuron was low than 0.05 mg· kg^- 1 in rice. Therefore, we recommend that 31% chlorfluazuron and triazophos EC was applied as foliage spray twice times at 1.5 times recommended dosage for rice with a safe int

关 键 词：农药学 氟啶脲 水稻 土壤 残留 液相色谱法 

分 类 号：X592[环境科学与工程—环境工程]