高效液相色谱质谱法测定动物源食品中咪唑菌酮及其代谢物的残留量

Determination of the Residues of Fenamidone and MPID in Animal Source Foods by HPLC-MS

摘要:

建立了采用高效液相色谱串联质谱仪测定动物源食品中咪唑菌酮及其代谢物5-甲基-5-苯基-2,4-咪唑烷二酮(MPID)残留量的分析方法。样品经乙腈提取，固相萃取苯乙烯二乙烯苯共聚物小柱、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（MRM）检测。结果表明：咪唑菌酮在0.05~0.8 μg/mL，MPID在0.5~8.0 μg/mL范围内呈现良好的线性关系，相关系数（r2）均大于0.999。在此范围内两者的加标回收率为82.09%~109.16%，相对标准偏差（RSD）为2.46%~7.89%，咪唑菌酮检测限为2.0 μg/kg，MPID检测限为20.0 μg/kg。该方法简便快捷，且能消除样品中色素等杂质的干扰，具有较高的准确度和精密度，适用于动物源食品中咪唑菌酮及其代谢物MPID残留量的测定。

Abstract:

The samples were extracted with acetonitrile, purified by activated PS-DVB and carbon column, and analyzed on C18 column by using a gradient elution using acetonitrile (A)- 5 mmol/L ammonium acetate methanol aqueous solution (B) (V:V=40:60) as mobile phase. The calibration curve presented a good linear relationship between the peak areas and concentrations in the range of 0.05~0.8 μg/mL fenamidone and 0.5~8.0 μg/mL MPID, with correlation coefficients more than 0.999. The average recoveries of standard addition at this concentration level ranged from 82.09% to 109.16%, and the relative standard deviation (RSD) was in the range of 2.46% to 7.89%. The limits of quantification of fenamidone and MPID in animal source foods were 2.0 μg/kg and 20.0 μg/kg. It was suitable for determination of fenamidone and MPID residues in animal source foods with high sensitivity and selectivity.