气相色谱-串联质谱法测定柑橘中5种杀螨剂残留

建立了气相色谱-串联质谱法(GC-MS/MS)检测柑橘中5种杀螨剂残留分析方法。样品经乙腈提取、氯化钠盐析后,取有机相用Qu EChERS方法净化,利用GC-MS/MS在多反应监测(MRM)模式下进行测定,外标法定量。5种杀螨剂在0.005~0.5mg/L浓度范围内呈现良好的线性关系,相关系数r^2均>0.996,方法定量限为0.005 mg/kg。在0.005、0.01和0.1mg/kg 3种添加水平下,加标回收率为70.6%~111.3%,相对标准偏差(RSD)为1.07%~14.64%。本方法简便、重现性良好,可用于柑橘类水果样品中杀螨剂的日常检测。

Analysis of Five Acaricides Residues in Citrus by GC-MS/MS

A method was developed for the simultaneous determination of the five acaricide residues in citrus fruits by gas chromatography tandem mass spectrometry(GC-MS/MS).The pesticide residues in citrus fruits samples were extracted into acetonitrile and salted out by NaCl.The organic phase was purified by QuEChERS method.The targeted compounds was analyzed and identified by GC-MS/MS system under the mode of multi-reaction monitoring(MRM),and quantified by the external standard method.The method showed a good linear relationship in the concentration range of 0.005~0.5 mg/L for all the 5 acaricides,the correlation coefficient(r^2)was greater than0.996,and the limit of quantization(LOQ)was 0.005 mg/kg.The recovery ratio of citrus fruits at levels of 0.005 mg/kg,0.01 mg/kg and 0.1 mg/kg were found to be in the range of 70.6%~111.3%,with the relative standard deviations(RSD)of 1.07%~14.64%.The method is simple and reproducible enough for the determination of the acaricide residues in Citrus fruits samples.