新型电膜萃取技术结合液相色谱串联质谱法测定畜肉食品中的沙丁胺醇

    Determination of salbutamol in livestock meat foods by electro-membrane extraction coupled with liquid chromatography-tandem mass spectrometry

    • 摘要: 针对不同畜肉食品中沙丁胺醇残留量低、基质干扰严重的问题,建立了一种采用新型电膜萃取技术结合液相色谱串联质谱测定畜肉食品中沙丁胺醇的分析方法。使用乙腈提取试样,采用电膜萃取技术进行选择性分离、净化和富集,在液相色谱串联质谱仪上选择多反应监测正离子模式检测,外标法定量。结果表明:施加80 V的外加电压、选择二-(2-乙基己基)磷酸酯和2-硝基苯辛醚体积比为2:8的混合溶剂作为有机溶剂、20 mmol/L甲酸溶液作为接收相,萃取时间30 min,可使沙丁胺醇的回收率最佳;该方法具有较宽的线性范围(1~1000 ng/mL),相关系数R2>0.9996,方法的检出限(S/N=3)和定量限(S/N=10)分别为0.05 µg/kg和0.17 µg/kg;对牛肉、羊肉、猪肉、猪肝4种不同样品进行加标测定,平均回收率和相对标准偏差(n=6)分别为83.5%~110%和3.3%~9.8%。本方法具有样品净化能力强、传质速率快、选择性好、操作简单等特点,适用于多种畜肉食品中沙丁胺醇的高灵敏准确测定。

       

      Abstract: To solve the problems of low salbutamol residue concentrations and severe matrix interference in various livestock meat foods, an analytical method has been developed for the determination of salbutamol in livestock meat food using a novel electromembrane extraction (EME) technique combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted using acetonitrile, followed by selective separation, purification, and enrichment using EME. Salbutamol detection was performed in positive ion mode with multiple reaction monitoring on an LC-MS/MS instrument, and quantification was conducted using the external standard method. In EME, salbutamol was first converted into its ionic form by adjusting the pH of the solution. Two L-shaped platinum electrodes were put into the sample solution and acceptor solution as the cathode and anode, respectively. The other ends of both L-shaped platinum electrodes were connected to the electrophoresis power supply. Upon activation of the power supply and stirring device, salbutamol in the sample phase migrate directionally through supported liquid membrane (SLM) into the acceptor phase. The results indicated that optimal extraction recovery of salbutamol was achieved under the conditions of an applied voltage of 80 V, a mixed solvent with ratio of di-(2-ethylhexyl) phosphate to 2-nitrophenyl octyl ether of 2:8 as the organic solvent, 20 mmol/L formic acid solution as the acceptor phase, and an extraction time of 30 min. This method exhibited a wide linear range of 1-1000 ng/mL with a correlation coefficient (R2) > 0.9996. The limits of detection (LOD, S/N=3) and the limits of quantification (LOQ, S/N=10) were 0.05 µg/kg and 0.17 µg/kg, respectively. Spike recovery experiments conducted on four different samples-beef, lamb, pork, and pork liver-yielded average recoveries ranging from 83.5% to 110% with relative standard deviations (RSDs, n=6) of 3.3% to 9.8%. This method is characterized by strong sample purification capabilities, rapid mass transfer rates, high sensitivity, and simple operation, making it suitable for highly sensitive and accurate determination of salbutamol in various livestock meat food.

       

    /

    返回文章
    返回