李文希, 浦恩堂, 代雪芳, 黄丽, 张雪燕. 百菌清及其代谢物4-羟基百菌清在三七上的残留行为及膳食风险评估[J]. 农药学学报, 2020, 22(3): 510-520. DOI: 10.16801/j.issn.1008-7303.2020.0030
    引用本文: 李文希, 浦恩堂, 代雪芳, 黄丽, 张雪燕. 百菌清及其代谢物4-羟基百菌清在三七上的残留行为及膳食风险评估[J]. 农药学学报, 2020, 22(3): 510-520. DOI: 10.16801/j.issn.1008-7303.2020.0030
    LI Wenxi, PU Entang, DAI Xuefang, HUANG Li, ZHANG Xueyan. Residual behavior and dietary risk assessment of chlorothalonil and its metabolite 4-hydroxy chlorothalonil in Panax notoginseng[J]. Chinese Journal of Pesticide Science, 2020, 22(3): 510-520. DOI: 10.16801/j.issn.1008-7303.2020.0030
    Citation: LI Wenxi, PU Entang, DAI Xuefang, HUANG Li, ZHANG Xueyan. Residual behavior and dietary risk assessment of chlorothalonil and its metabolite 4-hydroxy chlorothalonil in Panax notoginseng[J]. Chinese Journal of Pesticide Science, 2020, 22(3): 510-520. DOI: 10.16801/j.issn.1008-7303.2020.0030

    百菌清及其代谢物4-羟基百菌清在三七上的残留行为及膳食风险评估

    Residual behavior and dietary risk assessment of chlorothalonil and its metabolite 4-hydroxy chlorothalonil in Panax notoginseng

    • 摘要: 为保证百菌清的安全使用,明确百菌清及其代谢物4-羟基百菌清在三七上的残留行为,2017年在云南三七主产区丘北、广南、弥勒和石林4地进行了百菌清在三七上的规范残留试验,建立了气相色谱 (GC-ECD) 测定三七中百菌清和超高效液相色谱-串联质谱 (UPLC-MS/MS) 测定4-羟基百菌清残留的分析方法。样品中百菌清用V (乙酸乙酯) : V (正己烷) = 2 : 8混合溶液提取,硅胶固相萃取柱净化,GC-ECD检测;4-羟基百菌清用乙腈提取,N-丙基乙二胺 (PSA) 分散固相萃取净化,UPLC-MS/MS检测,外标法定量。结果表明:百菌清在三七块根和须根中的添加回收率为93%~98%,相对标准偏差 (RSD) 为3%~6%,定量限 (LOQ) 为0.05 mg/kg;4-羟基百菌清在三七块根和须根中的添加回收率为75%~94%,RSD为3%~9%,LOQ为0.02 mg/kg。丘北和广南的消解动态试验结果显示:百菌清在三七植株上的半衰期为8.4~8.5 d,4-羟基百菌清为16.5~17.3 d;百菌清和4-羟基百菌清在三七地下部分根系中的消解不符合一级动力学反应模型,在施药后45 d内,百菌清呈波动性缓慢下降,4-羟基百菌清呈波动性缓慢上升的趋势。4地的最终残留试验结果表明:采用40%百菌清悬浮剂,分别按其有效成分2 400和3 600 g/hm2的剂量喷雾施药3~4次,每次施药间隔为7 d,于末次施药后21 d采样测定,三七块根中百菌清的残留量为<0.05~3.14 mg/kg,4-羟基百菌清为0.19~1.54 mg/kg;三七须根中百菌清的残留量为0.085~0.760 mg/kg,4-羟基百菌清为0.46~4.48 mg/kg。膳食摄入风险评估结果显示,百菌清的国家估算每日摄入量 (NEDI) 为0.967 mg,风险概率 (RQ%) 为76.8%,4-羟基百菌清的NEDI为0.012 mg,RQ%为2.4%,对一般人群健康不会产生不可接受的风险。

       

      Abstract: To ensure the safe use of chlorothalonil and clarify the residual behavior of chlorothalonil and its metabolite 4-hydroxy chlorothalonil in P. notoginseng, the supervised field trials were conducted in the main producing areas of P. notoginseng in Yunnan Province, including Qiubei, Guangnan, Mile and Shilin in 2017. In addition, analytical methods were established for the determination of chlorothalonil and 4-hydroxy chlorothalonil in P. notoginseng using gas chromatography (GC-ECD) and ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), respectively. Chlorothalonil in samples were extracted with V (ethyl acetate) : V (n-hexane) = 2 : 8 mixed solvent, cleaned-up by silica gel solid phase extraction column, and detected by GC-ECD. 4-Hydroxy chlorothalonil was extracted with acetonitrile, cleaned-up by N-propyl ethylenediamine (PSA) dispersible solid phase extraction, and detected by UPLC-MS/MS. Both analytes were quantified with external standard method. Satisfactory recoveries of 93%-98%, relative standard deviations (RSDs) of 3%-6%, and limit of quantity (LOQ) of 0.05 mg/kg for chlorothalonil, and satisfactory recoveries of 75%-94%, RSDs of 3%-9%, and LOQ of 0.02 mg/kg for 4-hydroxy chlorothalonil were obtained in P. notoginseng root and fibrous root. The dissipation experiments in Qiubei and Guangnan showed that the half-life of chlorothalonil was 8.4-8.5 d, and the half-life of 4-hydroxy chlorothalonil was 16.5-17.3 d on P. notoginseng plant. However, the dissipation of chlorothalonil and 4-hydroxy chlorothalonil in the underground root system of P. notoginseng did not conform to the first-order kinetic model. It was observed that, within 45 days after the application, the residues of chlorothalonil decreased slowly, while the residues of 4-hydroxy chlorothalonil increased slowly, and both followed a fluctuating trend. The terminal residue experiments in the above 4 sites showed that when 40% chlorothalonil suspension applied for 3-4 times with an interval of 7 d at doses of 2 400 and 3 600 g (a.i)/hm2, the residues of chlorothalonil and 4-hydroxy chlorothalonil were <0.05-3.14 mg/kg and 0.19-1.54 mg/kg in root, and 0.085-0.760 mg/kg and 0.46-4.48 in fibrous root, respectively, 21 d after the last application. The results of the risk assessment of dietary intake revealed it would not pose an unacceptable risk to the health of the general population. Given that the national estimated daily intake (NEDI) of chlorothalonil was 0.967 mg, its risk quotient (RQ%) was 76.8%. Given that NEDI of 4-hydroxy chlorothalonil was 0.012 mg, its RQ% is 2.4%.

       

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