液相色谱-串联质谱法测定动物组织中金刚烷胺和金刚乙胺的残留量

Simultaneous Determination of Amantadine and Rimantadine Residue in Animal Tissues by LC-MS/MS

采用液相色谱-电喷雾串联质谱(LC-ESI-MS/MS),在多反应监测(MRM)模式下建立了动物组织中金刚烷胺和金刚乙胺的检测方法。试样中的金刚烷胺和金刚乙胺经V(乙腈)∶V(1.0%三氯乙酸)=50∶50的混合溶液超声提取,混合阳离子交换柱净化,氮气吹干后,用1mL V(甲醇)∶V(0.2%甲酸)=10∶90的溶液溶解残渣,液相色谱-串联质谱法测定,色谱保留时间和质谱碎片离子丰度比定性,外标法定量。该方法测得在鸡肉、鸡肝、猪肉、猪肝等动物组织中,金刚烷胺和金刚乙胺的检出限(LOD)均为0.4μg/kg,定量限(LOQ)均为1.0μg/kg;在0.5～100.0μg/L线性范围内,相关系数r2均大于0.999。添加回收率实验表明,以上4种动物组织中添加水平为1.0～100μg/kg时,金刚烷胺和金刚乙胺的平均回收率在70.7%～92.3%之间,相对标准偏差为1.7%～11.7%。

A rapid determination method for amantadine and rimantadine in animal tissues was established using liquid chromatography-electrospray tandem mass spectrometry （LC-ESI-MS/MS）in the multiple reaction monitoring （MRM） mode. The samples were ex- tracted with acetonitrile-1.0% trichloroacetic acid（50 ： 50,V/V） solution in ultrasonic, fol- lowed by a cleanup procedure with mixed cation exchange SPE. The eluate was dried under nitrogen blow, then dissolved in 1 mL methanol-0.2G formic acid（10 ：90, V/V） solution and the aliquot was detected by LC-MS/MS. The chromatographic retention time and mass fragment ion abundance ratio were taken for qualitative confirmation, and external standard method was employed for quantification. The limit of detection （LOD） is 0.4 μg/kg, and the limit of quantification （LOQ） is 1.0 μg/kg in chicken, chicken liver, pork and pork liver. The correlation coefficent is greater than 0. 999（r2〉0. 999） of the four animal tissues are obtained within 0.5--100.0 9g/L linear ranges. Recoveries are in a range of 70.7%-- 92.3% with the relative standard deviations （RSDs） varied from 1.7% to 11.7% at spiked levels of 5.0--100 μg/kg, respectively.