QuEChERS-高效液相色谱/质谱联用法测定猪肉中氯丙那林

Determination of Clorprenaline in Pork by QuEChERS-High Performance Liquid Chromatography-Mass Spectrometry

利用QuEChERS-高效液相色谱／质谱联用法建立了猪肉中氯丙那林的定性定量分析方法。猪肉样品用乙酸乙酯和K2CO。超声提取，加入C18、PSA和中性A12O3粉离心净化样品；采用AglientXDB—C18色谱柱（150×4．6mm，3．5μm），流动相为0．1％甲酸-甲醇上机监测；采用电喷雾离子源正离子模式（ESI＋）和多反应监测模式（MRM）进行质谱分析。结果表明，氯丙那林在0．005～5／μg／L之间呈线性关系，相关系数（r）为1．0000；检出限和定量限分别为0．15btg／kg和2．50μg／kg。在2．5、5．0和10．0μg／kg添加水平下，氯丙那林的回收率（n=12）范围为70．32％～92．13％，相对标准偏差均小于10％（n=12）。该方法快捷，简单，成本低且安全有效，适用于猪肉中氯丙那林的痕量检测。

A method for simultaneous determination of Clorprenaline in pork by modified QuEChERS- high performance liquid chromatography-tendem mass spectrometry （QuEChERS-HPLC-MS） was developed. The pork were extracted with ethyl acetate and potassium carbonate, and purified with Carbon-18, PSA, and neutral alumina followed by analysis on an Aglient XDB-C18 column（150 mm× 4.6 mm, 3.5 μm）using formic acid methanol（l：999 ,V/V） as the mobile phase. The mass spectrometric acquisition was carried out by means of eleetrospary ionization in positive mode （ESI＋ ） with multiple reaction monitoring（MRM） method. The good linearities（r= 1） were achieved within the concentration ranges of 0. 005-5 μg/L,and the limit of detection（LOD） and the limit of quantifiction（LOQ） were 0.15 μg/kg and 2.50 μg/kg, respectively. The recoveries of clorprenaline at the spiked levels of 2.5, 5.0 and 10.0 μg/kg ranged from 70.32-92.13% with the relative standard deviations（RSDs） less than 10%. The results demonstrated that the proposed method is quick, easy, cheap, eμective, rugged, safe and suitable for the determination of trace clorprenaline in pork.