3种新烟碱类杀虫剂在蜂蜜中HPTLC残留分析方法的研究

建立了吡虫啉、噻虫胺和噻虫嗪在蜂蜜中残留的高效薄层色谱(HPTLC)检测方法,用乙腈机械震荡提取后涡旋并离心样品,于C-18固相萃取柱净化,CAMAGLinomatⅣ点样仪点样,二氯甲烷∶乙酸乙酯=3∶1(V∶V)混合溶液单向上行展开,于254nm波长进行HPTLC检测。结果表明,当3种农药在蜂蜜中的添加浓度分别0.05、0.5和1.0 mg·kg~(-1)时,添加回收率分别为71.58%~101.25%、72.29%~109.47%和79.88%~108.92%,相对标准偏差分别为9.31%~14.47%、7.79%~12.86%和9.24%~14.23%,均满足农残分析的基本要求。

Study on the residue analysis method of three neonicotinoid insecticides in honey

A method was developed for analysis of imidacloprid, clothianidin and thiamethoxam residues in honey by high performance thin layer chromatography (HPTLC). Samples were extracted with acetonitrile (accompanied by mechanical shaking), and cleaned up by C-18 solid-phase extraction column. The extracts were applied as bands to the glass-backed silica gel 60F_(254) HPTLC plates with system of methylene chloride: ethyl acetate = 3:1 (V/V) under unidirectional upward. The plates were developed with TLC scanner at 254 nm. The recoveries were respectively 71.58%-101.25%, 72.29%-109.47% and 79.88%-108.92% when the concentrations of three pesticides in honey added were 0.05, 0.5 and 1.0 mg·kg^-1, and RSDs were 9.31% - 14.47%, 7.79% - 12.86% and 9.24% - 14.23%, respectively. The method meets the basic requirements of pesticide residues analysis.