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作 者:王晓梅 骆玉琴 赵学平[2] 陆兰菲 方楠 王祥云[2] 蒋金花[2] 何红梅[2] 张昌朋[2] 王强 WANG Xiaomei;LUO Yuqin;ZHAO Xueping;LU Lanfei;FANG Nan;WANG Xiangyun;JIANG Jinhua;HE Hongmei;ZHANG Changpeng;WANG Qiang(College of Life Sciences,China Jiliang University,Hangzhou 310018,China;Institute of Agro-Products Safety and Nutrition,Zhejiang Academy of Agricultural Sciences,Hangzhou 310021,China)
机构地区:[1]中国计量大学生命科学学院,浙江杭州310018 [2]浙江省农业科学院农产品质量安全与营养研究所,浙江杭州310021
出 处:《浙江农业学报》2024年第7期1666-1676,共11页Acta Agriculturae Zhejiangensis
基 金:浙江省基础公益研究计划(LGN21C140006);浙江省农业标准化生产示范创建(“一县一品一策”)项目(ZJNY2022001-014)。
摘 要:建立一种可同时检测氟吡菌酰胺及其代谢物2-(三氯甲基)苯甲酰胺(BZM)在铁皮石斛(鲜样和干样)中残留量的分析方法,采用盆栽实验探究氟吡菌酰胺和BZM在铁皮石斛上的残留行为,评估氟吡菌酰胺的长期膳食风险。建立的检测方法为样品经乙腈提取后,用十八烷基硅烷键合硅胶、N-丙基乙二胺和石墨化碳净化,之后用超高效液相色谱串联质谱法进行检测。在0.001~0.1 mg·L^(-1)范围内,所建立的氟吡菌酰胺和BZM检测方法线性关系良好,决定系数(R^(2))≥0.9981。在0.01、0.1、15 mg·kg^(-1)的添加水平下,氟吡菌酰胺和BZM在铁皮石斛中的回收率分别为85.71%~97.98%、94.14%~112.21%,相对标准偏差分别为0.39%~5.93%、1.22%~6.73%。41.7%的氟吡菌酰胺悬浮剂以推荐剂量(有效成分375.3 g·hm^(-2))或2倍推荐剂量施用1次,氟吡菌酰胺在铁皮石斛鲜茎和干茎上的消解均符合一级动力学方程,消解半衰期为19.20~28.76 d,属于易降解农药。在实验条件下,施药后75 d,氟吡菌酰胺和BZM在铁皮石斛中的残留量分别不超过1.98、0.09 mg·kg^(-1)。经测算,氟吡菌酰胺的全膳食国家估算每日摄入量为0.3806 mg,对应的风险商为60.41%,说明41.7%的氟吡菌酰胺悬浮剂在推荐剂量下施用于铁皮石斛上并不会对人体健康产生不可接受的风险。A method was established for the simultaneous determination of fluopyram and its metabolite 2-(trifluoromethyl)benzamide(BZM)in both fresh and dried Dendrobium officinale.Pot experiment was conducted to investigate the residue behaviors of fluopyram and BZM in D.officinale,and the long-term dietary risk of fluopyram was evaluated.The established determination method was as follows:the samples were extracted with acetonitrile,purified with octadecyl bonded silica gel(C_(18)),primary secondary amine(PSA)and PestiCarb(PC),and detected by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The result showed that fluopyram and BZM had linearities that ranged from 0.001 to 0.1 mg·L^(-1),with correlation coefficient≥0.9981.The recoveries of fluopyram and BZM in D.officinale at three spiked levels(0.01,0.1,15 mg·kg^(-1))were 85.71%-97.98%,94.14%-112.21%,respectively,with relative standard deviations of 0.39%-5.93%,1.22%-6.73%,respectively.When fluopyram was applied at recommended does(375.3 g·hm^(-2),based on the available ingredient)or double recommended does to D.officinale,the dissipation dynamics of fluopyram fitted the first-order kinetics equation,and the half-life of fluopyram in D.officinale was 19.20-28.76 d,indicating that fluopyram fell under the category of easily degradable pesticides.The residues of fluopyram and BZM in D.officinale did not exceed 1.98,0.09 mg·kg^(-1) after 75 days of application under the experiment contions.Calculation results showed that the national estimated daily intake of fluopyram was 0.3806 mg for the general population under the given conditions,and the corresponding dietary risk quotient was 60.41%,which indicated that applying 41.7%fluopyram suspension concentrate(SC)at the recommended dosage on D.officinale would not pose an unacceptable risk to human health.
关 键 词:氟吡菌酰胺 铁皮石斛 超高效液相色谱串联质谱 农药残留 膳食风险评估
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