同位素稀释液相色谱-串联质谱法测定鸡蛋中金刚烷胺类药物残留量  

Simultaneous Determination of Amantadine,Rimantadine and Memantine Residues in Eggs by Liquid Chromatography with Tandem Mass Spectrometry

作　　者：吴银良 赵健 叶宇飞 朱勇 孙亚米 

机构地区：[1]宁波市农业科学研究院,浙江宁波315040

出　　处：《分析测试学报》2014年第8期905-910,共6页Journal of Instrumental Analysis

基　　金：宁波市农业重大攻关资助项目(2013C11003)

摘　　要：建立了鸡蛋中金刚烷胺、金刚乙胺和美金刚残留量的分散固相萃取液相色谱-串联质谱测定方法.方法在优化流动相组成和柱温条件后,对同分异构体金刚乙胺和美金刚获得了满意的分离效果.鸡蛋样品经乙酸乙腈提取后,用PSA和C18填料进行分散固相萃取净化,净化液经氮气吹干后用0.1％甲酸-甲醇（90＞10）溶解,过滤膜后进行LC-MS/MS分析.采用Acquity BEH C18色谱柱分离,用0.1％甲酸溶液-甲醇作为流动相进行梯度洗脱,电喷雾正离子（ESI＋）模式电离,多反应监测（MRM）模式检测,同位素稀释内标法定量.结果显示3种药物在0.10 ～ 10.0 μg/L质量浓度范围内具有良好的线性关系,线性系数均大于0.999;在鸡蛋中的方法检出限均为0.15 μg/kg,定量下限均为0.50 μg/kg.3种药物在鸡蛋中的加标浓度为0.50,0.75,1.0 μg/kg时,平均回收率为96.2％ ～ 105.9％,批内相对标准偏差（RSD）为2.7％～4.5％,批间RSD为4.1％ ～5.3％.该方法能满足鸡蛋中金刚烷胺、金刚乙胺和美金刚残留量分析的要求.A method was developed for the determination of residual amantadine,rimantadine and memantine in eggs by dispersive solid phase extraction and liquid chromatography with tandem mass spectrometry.The satisfactory separation was obtained after optimizing composition of mobile phase and column temperatures for rimantadine and memantine isomers.The samples were extracted with acetic acid acetonitrile,then purified by dispersive solid phase extraction method with PSA and C18 sorbent.After purification,the extract was dried under nitrogen,and the residues were dissolved in 0.1％ formic acid-methanol（90 ∶ 10） and filtered through a 0.22 μm filter.The target compounds were analyzed by LC-MS/MS on an Acquity BEH C18 column using a mixture of 0.1％ formic acid-methanol as mobile phase with gradient elution.The mass spectrometer was operated under multiple reaction monitoring（MRM） mode in positive mode.The samples were quantified by the isotope dilution and internal standard methods.Good linearities were obtained for amantadine,rimantadine and memantine at a concentration range of 0.10-10.0 μg/L with correlation coefficients more than 0.999.The limits of detection for three drugs were all 0.15 μg/kg,and the limits of quantitation were 0.50μg/kg.The recoveries of three drugs in eggs at three spiked levels（0.50,0.75 and 1.0 μg/kg） were in the range of 96.2％-105.9％,with intra-assay relative standard deviations of 2.7％-4.5％ and inter-assay relative standard deviations of 4.1％-5.3％.The results demonstrated that the method was suitable for the determination of amantadine,rimantadine and memantine in eggs.

关 键 词：金刚烷胺 金刚乙胺 美金刚 液相色谱-串联质谱法 鸡蛋 残留 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]