UPLC-MS/MS法检测鸭表皮中松香酸残留量

Determination of the amount of rosin acid residues in duck skin by UPLC-MS/MS

建立了测定鸭表皮中松香酸残留量的方法。采用超高效液相色谱串联质谱(UPLC-MS/MS)法,以乙醇为提取溶剂,30℃超声提取10min,提取液经0.22μm滤膜过滤后直接进行液质分析,外标法定量。UPLC色谱柱为AcQuity UPLC~BEH C18,流动相为乙腈-0.1%甲酸水(75∶25),离子模式为ESI+,扫描方式为MRM,母离子为303.1m/z,子离子为123.1m/z,257.2m/z(定量)。松香酸的检测线性范围为1~100.0ng/m L,回收率为85.7%~105.1%。结论:该方法简便、结果准确、重复性好,整个分析过程仅耗时3.5min,适用于鸭表皮中松香酸残留量的测定。

A method for determination of the amount of rosin acid residues in duck skin was established. An ultra performance liquid chromatography - tandem mass spectrometry / mass spectrometry method was adopted, and ethanol was used as extraction solvent. After ultrasound at 30 ℃ for 10 min and filtration with 0.22μm filter membrane, the extracting solution was directly analyzed by UPLC - MS/ MS. The external standard method was used for quantification. UPLC chromatographic column was Ac- Quity UPLC BEH C18, mobile phase was acetonitrile - 0.1% formic acid water （75 ： 25） , ionization mode was ESI ＋ , scanning mode was MRM, parent - ion was 303. 1 m/z, and sub - ions were 123. 1m/z and 257.2m/z （quantification）. The linear range of determination of rosin acid was 1 ～ 100. 0ng/mL, and the recovery rate was 85.7% - 105.1%. Conclusion： this method was simple, accurate and reproducible, the whole analysis process only need 3.5 rain, and it was suitable for determination of the amount of rosin acid residues in duck skin.