黄花菜中甲基硫菌灵及其代谢物残留分析与膳食摄入风险评估

评估甲基硫菌灵在黄花菜中的安全使用,建立黄花菜中甲基硫菌灵及其代谢物多菌灵的检测方法,并对黄花菜中的残留量进行膳食摄入评估。黄花菜中甲基硫菌灵及其代谢物多菌灵用乙腈提取,N-丙基乙二胺(primary secondary amine, PSA)净化,离心后上清液过滤膜高效液相色谱-三重四极杆串联质谱法检测,甲基硫菌灵和多菌灵的仪器检出限为1×10^-3 ng,定量限为0.01 mg/kg。甲基硫菌灵在黄花菜(鲜)和黄花菜(干)中的添加回收率分别为84%-105%和101%-105%；多菌灵在黄花菜(鲜)和黄花菜(干)中的添加回收率分别为86%-96%和93%-99%。2020年在湖南省和江苏省两地甲基硫菌灵在黄花菜(鲜)和黄花菜(干)的降解半衰期分别为0.85 d、0.97 d和0.40 d、1.65 d；多菌灵在黄花菜(鲜)和黄花菜(干)的降解半衰期分别为1.62 d、1.88 d和1.66 d、1.88 d；不同施药次数、施药剂量及采收间隔期,甲基硫菌灵在黄花菜(鲜)和黄花菜(干)的最终残留量分别为<0.01-0.33 mg/kg和<0.01-1.51 mg/kg；多菌灵在黄花菜(鲜)和黄花菜(干)的最终残留量分别为<0.01-2.72 mg/kg和0.052-2.99 mg/kg。按试验设计方案进行施药,甲基硫菌灵(甲基硫菌灵和多菌灵之和,以多菌灵表示)的普通人群国家估算每日摄入量为1.19 mg,占允许日摄入量的63.1%,认为不会对一般人群健康产生造成不可接受风险。

Residue analysis and risk assessment of dietary intake of thiophanate-methyl and its metabolite in Hemerocallis citrina Baroni

Objective To establish an analytical method for the residues of thiophanate-methyl and its metabolite carbendazim in Hemerocallis citrina Baroni, and assess the risk of dietary intake for residues in Hemerocallis citrina Baroni, and evaluate its safety. Methods The thiophanate-methyl and its metabolites carbendazim were extracted with acetonitrile, primary secondary amine (PSA) was used for purification, centrifugated, the supernatant was filtered through the membranes, and analyzed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Results The limits of detection and limits of quantitation of thiophanate-methyl and its metabolite carbendazim were 1×10?3 ng and 0.01 mg/kg, respectively, the recoveries of thiophanate-methyl from the Hemerocallis citrina Baroni (fresh) and Hemerocallis citrina Baroni (dry) were 84%?105% and 101%?105%, respectively; the recoveries of carbendazim from the Hemerocallis citrina Baroni (fresh) and Hemerocallis citrina Baroni (dry) were 86%?96% and 93%?99%, respectively. In 2020, the the degradation half-lives of thiophanate-methyl in Hemerocallis citrina Baroni (fresh) and Hemerocallis citrina Baroni (dry) in 2 experiment sites of Hunan and Jiangsu were 0.85, 0.97 d and 0.40, 1.65 d, respectively; and the degradation half-lives of carbendazim in Hemerocallis citrina Baroni (fresh) and Hemerocallis citrina Baroni (dry) in the 2 experiment sites were 1.62, 1.88 d and 1.66, 1.88 d, respectively, under different application frequency, application dose and harvesting interval, the final residues of thiophanate-methyl in Hemerocallis citrina Baroni (fresh) and Hemerocallis citrina Baroni (dry) were <0.01?0.33 and <0.01?1.51 mg/kg, respectively; the final residues of carbendazim in Hemerocallis citrina Baroni (fresh) and Hemerocallis citrina Baroni (dry) were <0.01?2.72 and 0.052?2.99 mg/kg, respectively. Conclusion Under the conditions of 36% thiophanate-methyl suspension, 3-4 times at the recommended dose (active ingredient 675 ga.i./ha), 7 d interval and 14 d recommended safety interval, the international estimated daily intake of thiophanate-methyl (the sum of thiobacillazim methyl and carbendazim, represented by carbendazim) for the general population is 1.19 mg, 63.1% of the acceptable daily intake, and does not pose an unacceptable risk to the health of the general population.