固相萃取净化-高效液相色谱串联质谱法测定鱼肉制品中链霉素、双氢链霉素、卡那霉素的含量

Simultaneous Determination of Streptomycin, Dihydrostreptomycin and Kanamycin Residues in Fish Products by Solid-phase Extraction Coupled with High Performance Liquid Chromatography-tandem Mass Spectrometry

本文建立了一种简单、快速测定鱼肉制品中链霉素、双氢链霉素、卡那霉素的固相萃取净化-液相色谱串联质谱的分析方法。样品经庚烷磺酸钠和磷酸盐缓冲溶液提取,C18固相萃取柱净化后,在ACQUITYUPLC BEH HILIC C18色谱柱上以乙腈和0.1%甲酸水溶液为流动相进行梯度洗脱分离,采用HPLC-MS/MS选择反应监测(SRM)模式测定进行定性、定量分析,质谱采集模式为电喷雾正离子监测模式。结果表明:在5.0~100μg/kg范围内,峰面积与浓度线性良好,相关系数均大于0.9992;方法的检出限(LOD)为2.5μg/kg,定量限(LOQ)为5.0μg/kg,检测结果的相对标准偏差为1.16%~7.35%(n=6),平均加标回收率达到77.4%~107.3%。该方法具有较高的重现性和选择性,适用于鱼肉制品中链霉素、双氢链霉素、卡那霉素的残留分析检测。

A simple and quick analysis method was established for the determination of streptomycin, dihydrostreptomycin and kanamycinresidues in fish products by solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry. The sample was extracted with sodium heptanesulfonate and phosphate buffer, and cleaned with C18, The separation was carried out on a ACQUITYUPLC BEH HILIC C18 column with a gradient elution using acetonitrile and 0.1% formic acid, The mass spectrometer was operated in the positive ion mode using selected reaction monitoring for the qualitative and quantitative analysis. The external standard calibration curve was used for the quantification. The linear ranges were from 5.0 to 100 μg/kg with a good linear relationship（R20.9992）. The detection limit of this method was 2.5 μg/kg, and the limit of quantification was 5.0 μg/kg. The relative standard deviations ranged from 1.16%~7.35%（n=6） and the average recovery rates were from77.4%~107.3%. The method was suitable for the identification and quantification of streptomycin, dihydrostreptomycin and kanamycin residues in fish products due to high reproducibility and selectivity.