SPE-HPLC-MS/MS检测动物源性食品中金刚烷胺残留

Determination of Amantadine in Animal-derived Food by Combining SPE with HPLC-MS/MS

建立一种固相萃取-高效液相色谱-串联质谱(Solid phase extraction coupled to high performance liquid chromatography tandem mass spectrometry,SPE-HPLC-MS/MS)检测动物源性食品中金刚烷胺残留的方法。研究采用Oasis MCX固相萃取小柱为基质净化柱,以Agilent SB-C18柱(2.1 mm×150 mm,3.5μm)为液相分离柱,0.1%甲酸-乙腈为(体积比,80∶20)为流动相,流速0.2 m L/min。用电喷雾离子源正离子多反应监测(Multi-reaction monitoring,MRM)模式进行检测,外标法定量。在0.1μg/L^100.0μg/L范围内具有较好的线性关系,相关系数>0.999。该方法检出限(Limit of detection,LOD)为1.0μg/kg,定量限(Limit of quantitation,LOQ)为3.0μg/kg,对3个添加浓度(30.0、60.0、90.0μg/kg)下的鸡胸,鸡肝,鸡蛋,猪肉,羊肉5种样品中金刚烷胺残留的检测具有较高的准确度(回收率在83.6%~94.2%之间)和重现性(RSD<4.0%,n=3)。

An accurate and sensitive method for the detection of amantadine （AM） residues in animal-derived food products was developed by combining solid-phase extraction with high performance liquid chromatogra-phy-tandem mass spectrometry （SPE-HPLC-MS/MS）. The Oasis MCX solid-phase extraction column was used for complex matrix purification and Agilent SB-C18 column （2.1 mm × 150 mm, 3.5 pm） was employed for sep-aration in liquid chromatography using a mobile phase consisting of 0.1 % formic acid and acetonitrile （80 ： 20, volume ratio）with the flow rate 0.2 mL/min. The electrospray ionization （ESI） source in the positive mode and the multiple-reaction monitoring （MRM） mode were used for the quantitative analysis with external standard method. The results showed that the calibration curves were in good linearity for the AM ranged from 0.1 pg/L to 100 pg/L with the correlation coefficients（R2）〉 0.999.The limits of detection （LODs） and the limits of quantifi-cation （LOQs） of this method were 1.0 pg/kg and 3.0 pg/kg respectively . The average recovery rates were from 83.6 % to 94.2 % with the good relative standard deviations （RSDs, RSD〈4.0 % , n=3 ） in chosen chicken mus cle, chicken liver, egg, beef and mutton samples at three standard addition levels of 30.0,60.0, and 90.0 pg/kg.