QuEChERS-超高效液相色谱–质谱/质谱法测定鸡肉中三种喹诺酮类药物的不确定度评定

Uncertainty Evaluation for the Determination of Β-Agonists in Chicken by QuEChERS and Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

按照日本岛津公司QuEChERS方法包提供的方法,对采用高效液相色谱–质谱/质谱测定鸡肉中氧氟沙星、环丙沙星和恩诺沙星残留量的不确定度进行评价。对检测过程中各因素进行考虑,发现上述方法测定鸡肉中的3种喹诺酮类药物时,当氧氟沙星、环丙沙星和恩诺沙星浓度分别为0.999、0.998、0.984 μg/kg时,扩展不确定度分别为0.168、0.156、0.170 μg/kg (k = 2)。评定结果表明,影响检测结果的主要因素为标准溶液配制和标准曲线拟合过程,其次为测量重复性和回收率。

This study aimed to evaluate the uncertainty of measurement in the determination of Ofloxacin, Ciprofloxacin and Enrofloxacin in chicken by QuEChERS and ultra performance liquid chromatog-raphy-tandem mass spectrometry. All factors in the testing process are considered, and then it is found that when the above method is used to determine the Quinolones in chicken, as the concen-tration of Ofloxacin, Ciprofloxacin and Enrofloxacin in chicken was 0.999, 0.998, 0.984 μg/kg, the expanded uncertainty was 0.168, 0.156, 0.170 μg/kg (k = 2), respectively. The preparation of standard solution and curve fitting were found to be the main sources of uncertainty, and the next were measurement repeatability and recovery rate.