丙硫菌唑和肟菌酯在小麦中的残留规律与膳食风险评估

    Residues of prothioconazole and trifloxystrobin in wheat and their dietary risk assessment

    • 摘要: 为探讨在小麦中施用30%丙硫菌唑•肟菌酯悬浮剂后的残留规律及膳食摄入风险,按有效成分180 g/hm2的推荐剂量间隔5 d喷施2次,末次施药后28 d采收,开展了其在中国4个试验点小麦籽粒中的消解动态、12个试验点小麦籽粒和秸秆中的最终残留量试验。建立了QuEChERS-超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。样品经乙腈水溶液振荡提取、C18净化后,用ACQITY UPLC BEH C18色谱柱(50 mm × 2.1 mm,1.7 μm)分离,以0.1%甲酸水溶液-乙腈为流动相,采用电喷雾正离子(ESI+)扫描和多反应监测(MRM)模式检测,外标法定量。结果表明:脱硫丙硫菌唑、肟菌酯和肟菌酸在小麦籽粒中的消解均符合一级反应动力学模型,半衰期分别为2.2~10.2 d、1.9~4.0 d和3.7~10.3 d;除上海点脱硫丙硫菌唑最终残留量为0.026 mg/kg、低于国家规定的最大残留限量0.1 mg/kg外,三者在各试验点小麦籽粒中的最终残留量均低于0.02 mg/kg的定量限;三者在小麦秸秆中最终残留量的最高值分别为0.67、0.52和0.14 mg/kg。小麦籽粒中,脱硫丙硫菌唑和肟菌酯残留对中国居民膳食摄入长期风险商的贡献率分别为3%和0.8%,脱硫丙硫菌唑残留的短期风险商也处于较低水平(育龄妇女因没有相应数据未评估)。上述结果表明,在小麦中施用30%丙硫菌唑•肟菌酯悬浮剂,脱硫丙硫菌唑和肟菌酯的膳食摄入风险均较低(脱硫丙硫菌唑对育龄妇女的短期膳食摄入风险有待澄清)。

       

      Abstract: To investigate the residue patterns and dietary intake risk of 30% prothioconazole + trifloxystrobin suspension concentrate (SC) in wheat after application, experiments were conducted on its dissipation dynamics in wheat grains at 4 trial sites and final residues in wheat grains and straw at 12 trial sites in China. The formulation was applied twice at 5-day intervals at the recommended dosage of 180 g a. i./hm2. And an analysis method of QuEChERS (quick, easy, cheap, effective, rugged, and safe) pretreatment method with a ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed. After extraction by shaking with an acetonitrile-aqueous solution and purification using C18, the sample was separated by ACQITY UPLC BEH C18 column (50 mm × 2.1 mm, 1.7 μm). With aqueous 0.1% formic acid-acetonitrile as mobile phase, it was detected by electrospray positive ion (ESI+) scanning and multiple reaction monitoring (MRM) mode, and quantified using external standard method. The results showed that the dissipation of prothioconazole-desthio, trifloxystrobin and trifloxystrobin acid in wheat grains all conformed to first-order reaction kinetic models, with half-lives of 2.2-10.2 d, 1.9-4.0 d and 3.7-10.3 d, respectively; Except that the final residue of prothioconazole-desthio at the experimental site in Shanghai was 0.026 mg/kg, which was lower than the national maximum residue limit of 0.1 mg/kg, the terminal residues of the three substances were all lower than the limit of quantification of 0.02 mg/kg in wheat grains at all experimental sites; The highest final residual amounts of the three substances in wheat straw were 0.67, 0.52, and 0.14 mg/kg, respectively. The long-term risk quotient contribution rates of prothioconazole-desthio and trifloxystrobin residues in wheat grains to the dietary intake of Chinese residents were 3% and 0.8%, respectively. The short-term risk quotient of prothioconazole-desthio residue was also at a low level (due to the lack of relevant data, the risk to women of childbearing age has not been assessed). These results showed that, when 30% prothioconazole+trifloxystrobin SC was applied to wheat, the dietary intake risks of prothioconazole-desthio and trifloxystrobin to Chinese residents were both very low (short-term dietary intake risk of prothioconazole-desthio to women of childbearing age needs to be clarified).

       

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