冷鲜肉中β-受体激动剂测定方法的比对及优化研究
目的 对盐酸克伦特罗、莱克多巴胺、沙丁胺醇的现有检测方法进行比对, 并经优化得到一种基于超高效液相色谱-串联质谱(ultra high performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)的检测方法。方法 对2种现行检测标准和QuEChERS方法进行方法确认比对, 并基于标准方法原理进行逐步优化。通过酶解、无机提取、调pH、有机提取、固相萃取、浓缩过程进行前处理, 并通过UPLC-MS/MS对冷鲜肉中盐酸克伦特罗、莱克多巴胺和沙丁胺醇进行分析。结果 该优化方法定量限在0.08~0.17 μg/kg区间, 3个浓度的加标回收率在81.4%~94.6%区间, 相对标准偏差(relative standard deviation, RSD)小于8.1% (n=5). 结论 该方法相比标准方法, 前处理时间缩短一半以上, 仪器分析效率也有所提高; 相比于QuEChERS方法具有更低的定量限和更稳定的回收率。
Objective To compare the available methods for determination of clenbuterol hydrochloride, ractopamine and salbutamol, and obtain an optimized detection method based on high performance liquid chromatography tandem mass spectrometry (UPLC–MS/MS). Methods Two kinds of available standard methods and QuEChERS methods were employed for validation and comparison, following optimization step by step based on the principle of standard method. Clenbuterol hydrochloride, lake dopamine and salbutamol in chilled meat were analyzed by pretreatment including enzyme hydrolysis, inorganic extraction, pH adjustment, organic extraction, solid phase extraction, concentration, and detected by UPLC-MS/MS. Results The limit of quantitation of method were 0.08-0.17 μg/kg. The recoveries at 3 spiked levels were 81.4%-94.6%, and the relative standard deviations (RSDs) were less than 8.1% (n=5). Conclusion Compared with the standard method, the pretreatment time of this method is more than half, and the efficiency of instrumental analysis is improved. Compared with QuEChERS method, it has lower limit of quantitation and more stable recovery rate.
标题：冷鲜肉中β-受体激动剂测定方法的比对及优化研究
英文标题：Comparison and optimization of methods for determination of β-receptor agonists in chilled meat
作者：
周一冉 山东农业大学食品科学与工程学院;济宁市食品药检验检测中心
张琳 济宁市食品药检验检测中心
郭海涵 山东农业大学食品科学与工程学院
王明林 山东农业大学食品科学与工程学院
中文关键词:冷鲜肉,盐酸克伦特罗,莱克多巴胺,沙丁胺醇,
英文关键词:chilled meat,clenbuterol hydrochloride,ractopamine,salbutamol,
发表日期：2019-03-29
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