摘要
建立了鳗鲡肌肉中13种禁用β-受体激动剂残留的UPLC-MS/MS检测方法。鳗鲡肌肉样品采用0. 2 mol/L乙酸铵溶液提取,β-葡萄糖醛苷酶/芳基硫酸酯酶酶解,5%的三氯乙酸溶液沉淀蛋白,HLB固相萃取柱净化富集,目标化合物选用C_(18)色谱柱利用乙酸铵和乙腈梯度分离,UPLC-MS/MS在电喷雾离子源(ESI)正离子模式下以选择反应监测(SRM)模式定量分析。结果表明,13种β-受体激动剂在2. 5~100 ng/mL范围内线性关系良好,相关系数均大于0. 9938,在3个不同浓度(0. 5,1. 0,10μg/kg)水平下的基质加标,平均回收率在77. 0%~122. 0%之间,RSD为0. 59%~14%。方法检出限和定量限分别为0. 1μg/kg和0. 5μg/kg。方法适用于对鳗鲡中13种禁用β-受体激动剂残留的定性和定量分析。
A determination strategy of 13 banned β-agonists residues in eel muscle was established by ultra-high performance liquid chromatography triple-quadrupole mass spectrometry( UPLC-MS/MS).The samples were first pretreated by using β-glucoronidase/arylsulfatase to perform enzymatic hydrolysis,the product was then extracted by 0. 2 mol/L ammonium acetate solution. Subsequently,trichloroacetic acid( TCA) was added to remove proteins,and hydrophilic lipophilic balance( HLB)solid-phase extraction column cartridge was employed to purify and enrich the targets. The target compounds were separated through C_(18) chromatographic column,and quantified by UPLC-MS/MS which operated in positive selected reaction monitoring( SRM) mode. The method showed good linear in the range of 2. 5-100 ng/m L for the 13 β-agonists,with correlation coefficients( R~2) above0. 9938. The average recoveries at three spiked levels( 0. 5,1,10 μg/kg) ranged from 77. 0% to122. 0%,and the relative standard deviations( RSDs) ranged from 0. 59% to 14%. The limits of detection( LOD) and quantitation( LOQ) were 0. 1 μg/kg and 0. 5 μg/kg,respectively. This method was successfully applied to the simultaneous determination of 13 β-agonists residues in eel muscle.
引文
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