Department of Pharmaceutical Analysis, College of Pharmacy, Chung-Ang University, 221 Heukseok-Dong, Dongjak-Gu, Seoul, 156-756, South Korea.
Arch Pharm Res. 2013 Mar;36(3):359-65. doi: 10.1007/s12272-013-0065-y. Epub 2013 Mar 6.
A simple, robust and reliable method for the determination of residual robenidine in chicken muscle using high performance liquid chromatography with ultraviolet (UV) detection was developed and validated according to the Codex Alimentarius Commission guidelines. Chicken muscle was extracted by acetonitrile/formic acid (98:2, v/v) and defatted with hexane. Analytes were isocratically separated on a Luna C18 column (4.6 × 150 mm, 5 μm) using 70 % methanol in water containing 0.1 % trifluoroacetic acid at a flow rate of 1.0 mL/min at 30 °C. UV detection was performed at 312 nm. The method was validated by assessing performance parameters including selectivity, linearity, limit of quantification (LOQ), precision, accuracy, recovery, stability and robustness. A calibration curve that was constructed over 0.05-0.5 μg/g showed correlation coefficients of more than 0.999. The intra- and inter-day precisions (as coefficient of variation) were 1.45-3.32 and 2.63-4.99 %, respectively. The intra- and inter-day accuracies were 99.4-105.3 and 98.3-101.6 %, respectively. The recoveries were in the range of 76.6-81.8 % and the LOQ was 0.05 μg/g. The developed method showed suitable performance for the determination of robenidine residues in chicken muscle.
建立并验证了一种采用高效液相色谱-紫外检测法(HPLC-UV)测定鸡肉中残留罗贝尼迪的简单、稳健、可靠的方法,该方法符合食品法典委员会(CAC)的指导原则。鸡肉经乙腈/甲酸(98:2,v/v)提取,正己烷脱脂。分析物在 Luna C18 柱(4.6×150mm,5μm)上以 70%甲醇-水(含 0.1%三氟乙酸)为流动相进行等度洗脱,流速为 1.0mL/min,柱温为 30°C,在 312nm 处进行紫外检测。该方法通过评估选择性、线性、定量限(LOQ)、精密度、准确度、回收率、稳定性和稳健性等性能参数进行验证。在 0.05-0.5μg/g 范围内构建的校准曲线的相关系数均大于 0.999。日内和日间精密度(以变异系数表示)分别为 1.45-3.32%和 2.63-4.99%,日内和日间准确度分别为 99.4-105.3%和 98.3-101.6%。回收率在 76.6-81.8%范围内,LOQ 为 0.05μg/g。该方法适用于鸡肉中罗贝尼迪残留量的测定。