Li Jian, Ming Meiting, Huai Wenhui, Cai Zhimin, Sun Zhiwen, Ye Nengsheng
a Beijing Institute of Veterinary Drugs Control , Beijing , P. R. China.
b Department of Chemistry , Capital Normal University , Beijing , P. R. China.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2018 Nov;35(11):2111-2119. doi: 10.1080/19440049.2018.1512756. Epub 2018 Sep 13.
A general solid-phase extraction (SPE) method using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for the determination of moroxydine residues in pig and chicken samples has been developed. After extraction and purification of real samples, moroxydine residues were detected using a hydrophobic interaction liquid chromatography column with an optimised mobile phase composition. The extraction reagents, the kind of SPE columns and the type of eluents were optimised to achieve the maximum extraction efficiency. The matrix effects from the animal tissue influenced the quality of the quantitative data obtained. Under the optimised conditions, the moroxydine residues in pig and chicken samples spiked at three levels (1.0 μg/kg, 5.0 μg/kg and 10.0 μg/kg) were determined with good recoveries (61.5%-105.4%) and adequate relative standard deviations (3.2%-13.0%). In pig and chicken samples, the limit of detection (LOD) was 0.3 μg/kg, and the limit of quantification (LOQ) was 1.0 μg/kg. A sufficiently linear relationship in the range of 1.0 μg/kg-20.0 μg/kg was achieved with a good correlation coefficient (R ≥ 0.99).
建立了一种采用超高效液相色谱-串联质谱法（UPLC-MS/MS）测定猪和鸡样品中吗啉胍残留量的通用固相萃取（SPE）方法。对实际样品进行萃取和净化后，使用具有优化流动相组成的疏水作用液相色谱柱检测吗啉胍残留量。对萃取试剂、SPE柱类型和洗脱剂类型进行了优化，以实现最大萃取效率。动物组织的基质效应影响了所获得定量数据的质量。在优化条件下，对添加了三个水平（1.0μg/kg、5.0μg/kg和10.0μg/kg）吗啉胍的猪和鸡样品进行测定，回收率良好（61.5%-105.4%），相对标准偏差适中（3.2%-13.0%）。在猪和鸡样品中，检测限（LOD）为0.3μg/kg，定量限（LOQ）为1.0μg/kg。在1.0μg/kg-20.0μg/kg范围内实现了足够的线性关系，相关系数良好（R≥0.99）。
