首页|超高效液相色谱-串联质谱测定淡水鱼中三卡因和丁香酚

超高效液相色谱-串联质谱测定淡水鱼中三卡因和丁香酚

扫码查看
目的:建立淡水鱼中三卡因和丁香酚的超高效液相色谱-串联质谱测定方法.方法:试样提取离心经HRM固相萃取柱净化后过聚四氟乙烯滤膜,超高效液相色谱-串联质谱法测定.色谱柱为ACQUITY UPLC BEH C8柱(2.1 mm× 100 mm,1.7 μm),以水-甲醇为流动相,并采用等度洗脱模式.质谱分析选择电喷雾离子源(正负离子扫描)和多反应监测模式.结果:三卡因线性范围为0.1~20 µg/kg,丁香酚线性范围为1.0~200 μg/kg,相关系数(r)均大于0.999.三卡因的方法检出限为0.1 μg/kg,定量限为0.3 μg/kg;丁香酚的方法检出限为1.0 µg/kg,定量限为3.0 μg/kg.在低、中、高3组水平下,加标回收率为87.9%~114%,相对标准偏差为1.47%~8.46%.结论:采用液质串联同位素内标法同时测定三卡因和丁香酚,该方法灵敏度高、准确度好,且线性良好、分离度高,适用于淡水鱼中三卡因和丁香酚的同时检测.
Determination of Tricaine Methanesulfonate and Eugenol in Freshwater Fish by Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry
Objective:To establish an analytical method for the determination of tricaine methanesulfonate and eugenol in freshwater fish using ultra-high performance liquid chromatography tandem-mass spectrometry.Methods:The sample was extracted from the centrifuge and purified by HRM solid-phase extraction column,then passed through a polytetrafluoroethylene membrane,and determined by ultra-high performance liquid chromatography tandem mass spectrometry.The chromatographic column was an ACQUITY UPLC BEH C8 column(2.1 mm×100 mm,1.7 μm),using water-methanol as the mobile phase and adopting the isocratic elution mode,the electrospray ion source(positive and negative ion scanning)mode and multiple reaction monitoring(MRM)mode were selected for mass spectrometry analysis.Results:The linear range of tricaine was 0.1-20 ng/mL,and that of eugenol was 1.0-200 ng/mL,with correlation coefficients(r)greater than 0.999.The limit of detection(LOD)for tricaine was 0.1 μg/kg and the limit of quantification(LOQ)was 0.3 μg/kg,the LOD for eugenol was 1.0 μg/kg and the LOQ was 3.0 μg/kg.The recovery rates at low,medium,and high spiked levels ranged from 87.9%to 114%,with relative standard deviations(RSD)between 1.47%and 8.46%.Conclusion:The isotope-labeled internal standard method using liquid chromatography-tandem mass spectrometry was successfully applied to simultaneously determine tricaine and eugenol in freshwater fish.This method is highly sensitive,accurate,exhibits good linearity and separation,and is suitable for the simultaneous detection of tricaine and eugenol in freshwater fish.

ultra-high performance liquid chromatography tandem mass spectrometrytricaine methanesulfonateeugenolfreshwater fish

黄顺利、洪艺

展开 >

重庆市渝北区疾病预防控制中心,重庆 401120

超高效液相色谱-串联质谱 三卡因 丁香酚 淡水鱼

2024

食品科技
北京市粮食科学研究所

食品科技

CSTPCD北大核心
影响因子:0.622
ISSN:1005-9989
年,卷(期):2024.49(11)