液相色谱质谱法测定食品中咪唑菌酮残留量

Determination of the Residue Amout of Fenamidone in Plant Source Foods by High Performance Liquid Chromatography-mass spectrometry

建立采用高效液相色谱串联质谱仪测定植物源食品中咪唑菌酮残留量的分析方法。样品经丙酮提取,固相萃取活性炭柱净化,C18色谱柱分离,以乙腈和5 mmol/L乙酸铵甲醇水(v∶v=40∶60)溶液为流动相进行梯度洗脱,电喷雾正离子(ESI+)模式电离,多反应选择离子监测(MRM)。结果表明:咪唑菌酮在0.05μg/m L^0.8μg/m L范围内呈现良好的线性关系,相关系数(r2)大于0.999。在此范围内加标回收率为80.08%~108.53%,相对标准偏差(RSD)为1.16%~6.03%,检测限为1.0μg/kg。该方法可以满足植物源食品中咪唑菌酮残留量监测的需求。

A new method was established to detect the residue amout of fenamidone in plant source foods by high performance liquid chromatography coupled to tandem mass spectrometry （HPLC-MS/MS）. The samples were extracted with acetone, then purified by activated carbon column, and detected on C18 column by a gradient elution using acetonitrile （A）-5 mmol/L ammonium acetate methanol aqueous solution （B） as mobile phase. The calibration curve were good linear between the peak areas and concentrations in the range of 0.05 μg/mL-0.8 μg/mL, with correlation coefficients more than 0.999. The average recoveries at this concentration levels ranged from 80.08%to 108.53%, the RSD was in the range of 1.16%to 6.03%. The limits of quantification of fenamidone in plant source foods were below 1.0 μg/kg. It was suitable for the determination of fenamidone residues in plant source foods with high sensitivity and selectivity.