食品科学 ›› 2024, Vol. 45 ›› Issue (1): 204-209.doi: 10.7506/spkx1002-6630-20230209-093

• 安全检测 • 上一篇    

环嗪酮在蓝莓上的残留及其膳食风险评估

何红梅,徐玲英,张昌朋,王祥云,蒋金花,李艳杰,赵学平   

  1. (省部共建农产品质量安全危害因子与风险防控国家重点实验室,农业农村部农药残留检测重点实验室,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)
  • 发布日期:2024-02-05
  • 基金资助:
    财政部和农业农村部:国家现代农业产业技术体系资助项目(CARS-29);浙江省分析测试基金项目(2018C37013)

Quantitation and Dietary Risk Assessment of Hexazinone Residue in Blueberry Fruit

HE Hongmei, XU Lingying, ZHANG Changpeng, WANG Xiangyun, JIANG Jinhua, LI Yanjie, ZHAO Xueping   

  1. (State Key Laboratory for Managing Biotic and Chemical Threats to the Quality and Safety of Agro-products, Key Laboratory for Pesticide Residue Detection of Ministry of Agriculture and Rural Affairs, Institute of Agro-product Safety and Nutrition, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China)
  • Published:2024-02-05

摘要: 为探明环嗪酮在蓝莓上的最终残留量,在我国浙江、吉林、辽宁和北京4 地开展了75%环嗪酮水分散粒剂的田间残留实验。采用电喷雾电离正离子模式,建立超高效液相色谱-串联质谱法测定蓝莓中环嗪酮残留量的方法。样品经乙腈涡旋提取、盐包盐析,再用装有十八烷基键合硅胶(C18)和乙二胺-N-丙基硅烷材料的净化管净化后测定。考察方法的线性、基质效应、定量限、正确度和精密度(相对标准偏差)。在0.000 1~0.01 mg/L范围内,环嗪酮的标准曲线方程的线性关系良好,r>0.999 8;基质效应为-7.7%;方法定量限为0.01 mg/kg。在0.01、0.1 mg/kg和1.0 mg/kg添加量范围内,环嗪酮在蓝莓中平均回收率为87%~91%,相对标准偏差不高于3.7%。4 个实验点(浙江、北京、辽宁、吉林)最终残留实验结果显示:环嗪酮在实验点药后90 d和100 d的蓝莓样品中残留量均低于0.01 mg/kg,低于美国、日本和韩国制定的最大残留限量值(分别为0.6、0.2 mg/kg和0.05 mg/kg)。膳食风险评估结果表明:普通人群环嗪酮的国家估算每日摄入量为0.002 2 mg,膳食摄入风险的风险熵为0.084%,膳食风险小。因此,建议75%的环嗪酮水分散粒剂在蓝莓园使用时,最高施药剂量为有效成分1 800 g/hm2,施药1 次,安全间隔期为90 d。

关键词: 环嗪酮;蓝莓;残留;膳食风险评估

Abstract: In order to determine the residue of hexazinone in blueberry fruit, field experiments in Zhejiang, Jilin, Liaoning and Beijing, China were conducted using 75% hexazinone water dispersible granules. An analytical method was established for determining residual hexazinone in blueberry fruit utilizing ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with an electrospray ionization source in the positive ion mode (ESI+). The samples were extracted with acetonitrile while vortexing, salted out, and then purified on a column packed with primary secondary amine (PSA) and C18 before measurement. The linearity, matrix effect, limit of quantification (LOQ), trueness (recovery rate) and precision (relative standard deviation (RSD)) of the proposed method were studied. Good linearity (r > 0.999 8) was found in the concentration range from 0.000 1 to 0.01 mg/L. The matrix effect was −7.7%. The LOQ was 0.01 mg/kg. The average recovery of hexazinone from blueberry fruit at spiked concentration levels of 0.01, 0.1 and 1.0 mg/kg ranged from 87% to 91%, with a RSD less than 3.7%. The field experiments showed that the residual level of hexazinone in blueberry fruit was below 0.01 mg/kg at 90 and 100 days after application, which was lower than the maximum residue limits (MRL) established in the US, Japan and South Korea (0.6, 0.2 and 0.05 mg/kg, respectively). The results of chronic dietary risk assessment showed that the estimated daily intake of hexazinone for general populations was 0.002 2 mg. The dietary risk quotient (RQ) was only 0.084%, indicating a low risk of dietary hexazinone intake. Therefore, it is recommended that 75% hexazinone water dispersible granules (WG) be applied in a single dose up to 1 800 g/hm2 to blueberry orchards; the pre-harvest interval (PHI) be 90 days.

Key words: hexazinone; blueberry fruit; residue; dietary risk assessment

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