摘要
采用通过型固相萃取方式净化样品,建立了乌鳢(Ophiocephalus argus Cantor)肌肉中金刚烷胺、金刚乙胺和美金刚的液相色谱-串联质谱快速分析方法。样品采用80%乙腈水溶液(含0. 1%甲酸,V/V)进行提取,使用Oasis PRi ME HLB通过型固相萃取柱净化。净化后样品采用Phenomenex Kinetex F5色谱柱分离,以乙腈和5mmol/L乙酸铵水溶液(含0. 1%甲酸,V/V)为流动相进行梯度洗脱,多反应监测正离子模式扫描,采用同位素稀释内标法定量。3种目标化合物在相关范围内线性关系良好,相关系数不低于0. 99,定量限均为0. 5μg/kg,基质加标回收率为91. 7%～104. 0%,相对标准偏差为4. 6%～8. 1%。该方法前处理操作简便,灵敏度和准确度高,成功运用于24批次养殖乌鳢样品中金刚烷胺、金刚乙胺和美金刚的同时快速测定,结果上述药物均未检出。
An analytical method was developed for the simultaneous and rapid determination of amantadine,rimantadine and memantine in Ophiocephalus argus Cantor meat by liquid chromatography-tandem mass spectrometry(LC-MS/MS)coupled with pass-through solid phase extraction(SPE).The samples were extracted with 80%acetonitrile-water(0.1%formic acid,V/V),then purified with an Oasis PRiME HLB pass-through SPE column.The samples were separated directly on a Phenomenex Kinetex F5 column using 5 mmol/L ammonium acetate(0.1%formic acid,V/V)and acetonitrile as mobile phase.Qualitative and quantitative analysis of the analytes was carried out under the multiple reaction monitoring mode with positive electrospray ionization.The samples were quantified by the internal standard methods with isotope dilution.The calibration curves were linear in the corresponding concentration ranges,with correlation coefficient≥0.99.The limit of quantification was 0.5μg/kg.The average spiked recoveries were between 91.7%and 104.0%with the relative standard deviations in the range of 4.6%-8.1%.The proposed method is sensitive,accurate,and efficient for sample pretreatment.It is applicable for the determination of amantadine,rimantadine and memantine in Ophiocephalus argus Cantor meat.Afterwards,this method was successfully applied to the simultaneous determination of amantadine,adamantine and memantine in 24 batches of cultured snakehead samples,and the results showed that none of the above mentioned drugs were detected.
作者
李诗言
王扬
周凡
柯庆青
贝亦江
王鼎南
郑重莺
吴洪喜
丁雪燕
LI Shiyan;WANG Yang;ZHOU Fan;KE Qingqing;BEI Yijiang;WANG Dingnan;ZHENG Chongying;WU Hongxi;DING Xueyan(Aquatic Products Quality Inspection Center of Zhejiang Province,Hangzhou 310023,China)
出处
《中国渔业质量与标准》
2018年第5期64-72,共9页
Chinese Fishery Quality and Standards
基金
浙江省水产品质量安全技术支撑团队项目(QS2017006
QS2017013)
关键词
高效液相色谱串联质谱法
金刚烷胺
金刚乙胺
美金刚
乌鳢
通过型固相萃取
high performance liquid chromatography-tandem mass spectrometry
amantadine
rimantadine
memantine
pass-through solid-phase extraction
Ophiocephalus argus Cantor
