摘要
建立了采用高效液相色谱(HPLC)测定水稻和稻田中2-(乙酰氧基)苯甲酸残留量的分析方法。稻田水样中残留的2-(乙酰氧基)苯甲酸用酸性三氯甲烷直接提取;而稻田土壤、水稻茎秆和稻壳样品则先用酸性乙醇和三氯甲烷的混合液提取,再用三氯甲烷萃取;糙米样品先用乙醇和三氯甲烷混合液提取,再用三氯甲烷萃取。各萃取液经弗罗里硅土柱层析净化后,经ODS Hypersid柱分离,采用紫外检测器检测,外标法定量。在0.10～3.06 mg/L范围内,2-(乙酰氧基)苯甲酸的峰面积与其质量浓度间呈良好的线性关系,相关系数为0.999 8。在稻田水中添加0.1～1.0 mg/L,稻田土壤、水稻茎秆、稻壳和糙米中添加0.1～1.0 mg/kg的2-(乙酰氧基)苯甲酸,其平均回收率在80.8%～103.0%之间,相对标准偏差在0.74%～6.11%之间,其在稻田水、稻田土壤和水稻茎秆、稻壳和糙米中的最低检测浓度(LOQ)均为0.10 mg/kg(或mg/L)。田间试验结果表明:2-(乙酰氧基)苯甲酸在稻田样品中的消解动态曲线符合一级动力学方程,其在稻田水、土壤和水稻茎秆中消解迅速,半衰期分别为2.44～2.60、4.44～5.21、3.95～4.04 d。在低剂量和高剂量(有效成分0.027和0.041 g/m2)下在水稻成熟期施药3次和4次,至水稻收获时,其在糙米中的最终残留量未超过0.042 mg/kg。推荐我国对2-(乙酰氧基)苯甲酸在糙米中的最大允许残留水平(MRL)值为0.10 mg/kg。
A high performance liquid chromatographic （HPLC） method was established for the analysis of 2-ethanoyldroxybenzoic acid residue in rice and paddy field. The paddy water was extracted with acidic chloroform. For the paddy soil, rice culm and rice hull, samples were firstly extracted with acidity ethanol. For brown rice, it was first extracted with ethanol, followed by chloroform. The extracts were then cleaned-up on a Florisil column and detected by high performance liquid chromatography with an ultraviolet detector （UVD） on a ODS Hypersid column （4.0 mm x 25 cm x 10 p^m）. The calibration curve showed good linearity from 0.10 mg/L to 3.06 mg/L with the correlation coefficient more than 0. 999 8. The average recoveries of this method were from 80.8% to 103.0% with the
出处
《农药学学报》
CAS
CSCD
北大核心
2012年第5期527-532,共6页
Chinese Journal of Pesticide Science
关键词
2-(乙酰氧基)苯甲酸
水稻
农药
残留
高效液相色谱
2-ethanoyldroxybenzoic
rice
pesticide
residue
high performance liquid chromatography(HPLC)
