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[目的]为了准确评价甲基硫菌灵在芝麻上使用后其对芝麻的安全性,通过高效液相色谱法对其及代谢物多菌灵残留量进行测定,并建立快速分析方法。[方法]采用1%甲酸的乙腈溶液浸泡萃取,然后利用N-丙基乙二胺(PSA)和C18粉末净化,反相高效液相色谱法测定,外标法定量。[结果]在0.1~1.0 mg/kg添加水平范围内,多菌灵的添加回收率为76.37%~102.34%,RSD为3.36%~8.86%;甲基硫菌灵的添加回收率为87.29%~108.42%,RSD为3.81%~5.71%。多菌灵、甲基硫菌灵最小检出质量分数分别为0.015、0.002 mg/kg。2009、2010年芝麻中多菌灵平均残留量分别为0.0577、0.2437 mg/kg,甲基硫菌灵残留量分别为0.2663、0.3002 mg/kg。[结论]2010年芝麻中多菌灵的残留量高于无公害芝麻多菌灵残留限量指标(0.2 mg/kg);2009、2010年芝麻中甲基硫菌灵的残留量均高于欧盟残留限量标准(0.1 mg/kg)。
[Objective] The aim of the study was to evaluate the safety of thiophanate-methyl against sesame after being used on sesame seeds. The content of carbendazim and metabolites was determined by HPLC, and the rapid analysis method was established. [Method] The extract was extracted with acetonitrile solution of 1% formic acid and then purified by N - propyl ethylenediamine (PSA) and C18 powder, determined by reversed-phase high performance liquid chromatography with external standard method. [Result] The recoveries of carbendazim from 76.37% to 102.34% and RSD from 3.36% to 8.86% were obtained within the range of 0.1-1.0 mg / kg. The recoveries of carbendazim were 87.29% 108.42%, RSD 3.81% ~ 5.71%. Carbendazim, thiophanate-methyl detection minimum mass fraction of 0.015,0.002 mg / kg. The average carbendazim residues in sesame seeds in 2009 and 2010 were 0.0577 and 0.2437 mg / kg, respectively. The residues of thiophanate-methyl residues were 0.2663 and 0.002002 mg / kg, respectively. [Conclusion] The content of carbendazim in sesame in 2010 was higher than the limit of residue of carbendazim in non-pollution sesame (0.2 mg / kg). The residues of thiophanate-methyl in sesame in 2009 and 2010 were all higher than those in EU Limited standard (0.1 mg / kg).