固相萃取-高效液相色谱法测定生姜中涕灭威及其代谢物

建立了生姜中涕灭威、涕灭威砜和涕灭威亚砜残留量检测的固相萃取—高效液相色谱分析方法。样本采用乙腈提取,经C18固相萃取柱净化,浓缩定容后用HPLC-FLD检测分析,外标法定量。结果表明:该方法在0.02~8.0 mg/L标准曲线线性良好,相关系数均达到0.999以上,样本添加水平为2.0×10-2、4.0×10-2mg/kg时,回收率为80.25%~102.85%,相对标准偏差为3.64%~8.67%,方法检出限均低于2.5×10-3mg/kg。该方法具有准确度高及净化效果好等特点,能很好地满足实际样本残留分析要求。

Determination of Aldicarb and Its Metabolites Residues in Ginger by Solid Phase Extraction-High Performance Liquid Chromatography

A novel method has been developed to determine aldicarb,aldicarb sulfoxide,aldicarb sulfone residues in ginger by solid phase extraction/high performance liquid chromatography. Samples were extracted by acetonitrile and cleaned up by solid-phase C18 column. The eluate was condensed and injected into a high performance liquid chromatography equipped with a fluorescence detector(FLD)for the quantification of aldicarb, aldicarb sulfoxide,aldicarb sulfone by external standard method.The results showed that the method in 0.02~8.0 mg/L had standard curves with good linearity,the correlation coefficients were above 0.999,recovery rates for aldicarb,aldicarb sulfoxide,aldicarb sulfone in 6 varieties of blank ginger samples spiked at 2.0×10-2mg/kg and 4.0×10-2mg/kg ranged from 80.25% to 102.85%. The limit of detection(LOD)of this method was less than 2.5× 10-3mg/kg.The relative standard deviations was 3.64%~8.67%. This method was accurate,highly automated and presented high cleanup effectiveness. It could meet the requirements of pesticide residue analysis.