畜禽肉食品中金刚烷胺金刚乙胺残留量的超高效液相色谱串联质谱法测定  

Determination on amantadine and rimantadine residues in livestock and poultry food by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：林瑶[1] LIN Yao(Fuzhou City Center for Disease Control and Prevention,Fuzhou,Fujian,50005,China)

机构地区：[1]福州市疾病预防控制中心,福建350005

出　　处：《预防医学论坛》2022年第6期438-441,共4页Preventive Medicine Tribune

摘　　要：目的 建立畜禽食品中金刚烷胺、金刚乙胺残留量的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。方法 金刚烷胺、金刚乙胺分别以金刚烷胺-D15、金刚乙胺-D4为内标,用0.5%三氯乙酸-乙腈(50∶50)提取样品中的金刚烷胺、金刚乙胺,提取液通过Oasis MCX柱净化,采用Waters HSS T3色谱柱(2.1 mm×100 mm, 1.8 μm)分离,柱温为45℃,以甲醇-含0.2%甲酸的水溶液为流动相,流速为0.4 mL/min,梯度洗脱,质谱检测,正离子模式。结果 方法线性范围为0.2~20 μg/L,两种化合物在测定的浓度范围内,线性关系良好,相关系数>0.999 9,检出限为0.1 μg/kg;用3种浓度做加标回收,金刚烷胺回收率为82.44%~92.31%,金刚乙胺回收率为87.13%~95.42%,相对标准偏差为2.62%~6.74%。结论 本法前处理操作简单、快速、灵敏,检测结果准确度高,能满足畜禽食品中金刚烷胺、金刚乙胺残留量的日常检测要求。Objective To establish a method for the determination of amantadine and rimantadine residues in livestock and poultry food by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods Amantadine and rimantadine were extracted with 0.5% trichloroacetic acid-acetonitrile(50∶50) using amantadine-D15 and rimantadine D4 as internal standard.The extraction solution was purified by Oasis MCX column.The separation was performed on a Waters HSS T3 column(2.1 x 100 mm, 1.8 μm) at 45 ℃ with gradient elution using methanol-aqueous solution containing 0.2% formic acid as mobile phase at a flow rate of 0.4 mL/min.Mass spectrometry, positive ion mode. Results The linear range of the method was 0.2 μg/L to 20 μg/L.The linear relationship between the two concentrations was good, the correlation coefficient was > 0.999 9,and the detection limit was 0.1 μg/kg.The recoveries of amantadine and rimantadine were 82.44%-92.31% and 87.13%-95.42%,respectively, with 3 kinds of spiked concentrations.The relative standard deviations(RSD) were 2.62%-6.74%. Conclusion The method is simple, rapid, sensitive and accurate, which can meet the requirements of daily determination of amantadine and rimantadine residues in livestock and poultry food.

关 键 词：超高效液相色谱串联质谱法 金刚烷胺 金刚乙胺 残留 

分 类 号：R155.5[医药卫生—营养与食品卫生学]