油菜籽中高效氟吡甲禾灵及其代谢物的残留检测与膳食风险评估  

Residue detection and dietary risk assessment of haloxyfop-p-methyl and its metabolites in rapeseed

作　　者：张洋 杨丽华[1,2] 龚道新[1,2] 王寒[1,2] 郑蒋夫 卿朝霞 ZHANG Yang;YANG Lihua;GONG Daoxin;WANG Han;ZHENG Jiangfu;QING Zhaoxia(College of Resource and Environment,Hunan Agricultural University,Changsha,Hunan 410128,China;Institute of Agricultural Environmental Protection,Hunan Agricultural University,Changsha,Hunan 410128,China)

机构地区：[1]湖南农业大学资源环境学院,湖南长沙410128 [2]湖南农业大学农业环境保护研究所,湖南长沙410128

出　　处：《湖南农业大学学报（自然科学版）》2021年第3期326-331,共6页Journal of Hunan Agricultural University(Natural Sciences)

基　　金：农业农村部农药残留登记试验项目(CL21218086)。

摘　　要：通过添加回收试验建立高效氟吡甲禾灵及其代谢物氟吡禾灵在油菜籽中的残留检测方法;2018—2019年,在河南济源、安徽合肥、浙江杭州、湖北武汉、湖南长沙、四川彭州、云南昆明、广西南宁等8地开展高效氟吡甲禾灵最终残留量试验,并对其进行膳食摄入风险评估。结果显示:采用乙腈超声提取,经弗罗里硅土层析柱净化,结合高效液相色谱检测油菜籽样品中高效氟吡甲禾灵,采用NaOH-甲醇混合溶液提取,经N-丙基乙二胺净化,结合液相色谱质谱联用检测油菜籽样品中氟吡禾灵,在0.05、0.30、3.00 mg/kg 3个添加水平下,高效氟吡甲禾灵和氟吡禾灵在油菜籽中的平均添加回收率分别为77%~87%和77%~100%,相对标准偏差分别为6%~13%和1%~8%;48%高效氟吡甲禾灵乳油制剂按0.011 g/m^(2)用量施药,在油菜成熟期采收的油菜籽中高效氟吡甲禾灵及其代谢物氟吡禾灵的残留量均小于0.05 mg/kg,总量均小于0.10 mg/kg,推荐高效氟吡甲禾灵在油菜籽上的最大残留限量为0.10 mg/kg;普通人群高效氟吡甲禾灵的国家估算每日摄入量为0.046 56 mg,占日允许摄入量的105.58%,对一般人群健康可能产生不可接受的风险。A method for detecting the residues of haloxyfop-p-methyl and its metabolite haloxyfop-p in rapeseed was developed by recovery test.From 2018 to 2019,the final residue test of haloxyfop-p-methyl was carried out in Jiyuan of Henan,Hefei of Anhui,Hangzhou of Zhejiang,Wuhan of Hubei,Changsha of Hunan,Pengzhou of Sichuan,Kunming of Yunnan and Nanning of Guangxi,and the its dietary intake risk was then assessed.Ultrasonic extraction with acetonitrile,purification with Florisil column,combined with high performance liquid chromatography determination of haloxyfopp-methyl in rapeseed samples were applied,while extraction with NaOH-methanol mixed solution,purified with n-propyl ethylenediamine,combined with high performance liquid chromatography-tandem mass spectrometry determination of haloxyfop-p in rapeseed samples were applied.It was shown that the average recoveries of haloxyfop-p-methyl and haloxyfop-p in rapeseed were 77%-87%and 77%-100%respectively at three spiked concentration levels of 0.05,0.30,3.00 mg/kg,with the relative standard deviations were 6%-13%and 1%-8%respectively.When applying the dosage of the 48%haloxyfop-p-methyl emulsifiable concentrate was 0.011 g/m^(2),the residues of haloxyfop-p-methyl and its metabolite haloxyfop-p were less than 0.05 mg/kg at the rapeseed mature stage,and the total amount was less than 0.10 mg/kg.It is recommended that the maximum residue limit of haloxyfop-p-methyl in rapeseed is 0.10 mg/kg.The national estimate of haloxyfop-p-methyl in the general population is 0.04656 mg per day,accounting for 105.58%of the daily allowable intake,which may pose unacceptable risk to the health of the general population.

关 键 词：高效氟吡甲禾灵 氟吡禾灵 油菜籽 除草剂 残留检测方法 残留量 膳食风险评估 

分 类 号：S482.4[农业科学—农药学] O657.62[农业科学—植物保护]