高效液相色谱柱后衍生测定鸡组织中甲基盐霉素残留量

建立了鸡组织中甲基盐霉素的高效液相色谱柱后衍生化分析方法.样品经异辛烷提取,离心后上层有机相过硅胶固相萃取小柱,洗脱液浓缩后用V(甲醇)∶ V(水)=90∶ 10混合液溶解.采用Inertsil ODS-3 C18柱,以V(甲醇): V(乙酸)∶ V(水)=94∶ 3∶ 3为流动相,香草醛为衍生剂进行高效液相色谱柱后衍生分析,520 nm检测,外标法定量.方法检出限为6 μg/kg; 定量限为20 μg/kg; 添加浓度在20～1800 μg/kg范围内,平均添加回收率为76.4%～93.1%; 批内相对标准偏差(RSD)在2.6%～8.9%之间; 批间相对标准偏差(RSD)在4.7%～9.7%之间.样品浓度在0.07～10.0 mg/L范围内与峰面积呈良好的线性关系,r>0.9993.

Determination of Narasin in Chicken Tissues by High Performance Liquid Chromatography with Post-column Derivatization

A method was developed for determining residual narasin in chicken tissues by HPLC with post-column derivatization. The samples were extracted with iso-octane. Further cleanup was performed on LC-si cartridge after centrifugation. Then the eluent was dried by nitrogen and residues were dissolved in methanol, water mixture (90∶ 10 v/v). The samples were analyzed on an Inertsil ODS-3 C18 column with a mixture of methanol-acetic acid-water as the mobile phase and vanillin as the derivatization reagent. The detection wavelength was 520 nm. The samples were quantified with the external standard calibration curve method. The limit of detection and the limit of quantification for narasin in chicken tissues were 6.0 μg/kg and 20 μg/kg, respectively. The average recoveries of narasin in chicken tissues were 76.4 %-93.1 %, the intra-assay relative standard deviations were 2.6 %-8.9% and the inter-assay relative standard deviations were 4.7%-9.7% at spiked levels of 20-1800 μg/kg. There was a good linear correlation (the calibration coefficient is above 0.9993) between the peak areas and concentration of narasin in the range of 70-10000 μg/L.