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[目的]建立气相色谱-电子捕获检测器(GC-ECD)检测绿豆和向日葵中福美双残留量的方法,为18%辛硫磷·福美双微囊悬浮剂在绿豆和向日葵上的田间应用提供科学用药参考。[方法]实验研究根据GB 2763—2014规定,将福美双衍生化为CS_2。样品在SnCl_2·HCl溶液中加热到85℃分解产生CS_2,正己烷吸收CS_2,GC-ECD检测,仪器的最小检出量(LOD)为2.52×10~(-11)g,最低检测质量分数(LOQ)为0.08 mg/kg。[结果]绿豆和向日葵中的福美双添加质量分数为0.13、0.67、5.33 mg/kg时,福美双在绿豆中的平均回收率为86.24%~101.72%,相对标准偏差为0.99%~5.10%,在向日葵中平均回收率为83.64%~100.52%,相对标准偏差为1.00%~5.60%。田间试验研究结果显示,福美双在绿豆和向日葵中的最终残留量(福美双转化为CS_2,以CS_2计)均低于0.08 mg/kg。[结论]绿豆按18%辛硫磷·福美双微囊悬浮剂推荐剂量1∶(80~53)(药种比)的制剂用量施用,向日葵按推荐剂量1∶(17~25)(药种比)的制剂用量施用,收获的成熟绿豆和向日葵是安全的。
[Objective] To establish a gas chromatography-electron capture detector (GC-ECD) method for the detection of the biodegradable residues in mung bean and sunflower, and provide the field application of 18% phoxim in the field of mung bean and sunflower Scientific medication reference. [Method] Experimental study According to the provisions of GB 2763-2014, the biuret derivation into CS_2. The sample was heated to 85 ℃ in SnCl 2 · HCl solution to decompose to produce CS_2. Hexane was absorbed by CS_2 and detected by GC-ECD. The minimum detectable volume (LOD) was 2.52 × 10 ~ (-11) g. The minimum detectable mass fraction LOQ) was 0.08 mg / kg. [Result] The average recoveries of thiram and mung bean in the mung bean and sunflower were 86.24% ~ 101.72% and 0.99% ~ 5.10%, respectively, at the concentrations of 0.13,0.67 and 5.33 mg / kg. The average recoveries of sunflower were 83.64% ~ 100.52% with relative standard deviations of 1.00% ~ 5.60%. The results of field trials showed that the final residues of thiram in mung bean and sunflower were both less than 0.08 mg / kg (the conversion from thiram to CS_2 to CS_2). [Conclusion] The mung bean was applied to the dosage of 1:18 (~ 53) (ratio of drug to drug) recommended by 18% phoxim and thiram microencapsulated suspension. Than the amount of the preparation dosage application, the harvest of mature green beans and sunflower is safe.