高效液相色谱法同时测定饲料中地西泮、安眠酮的含量

Simultaneous HPLC Determination of Diazepam and Methaqualone in Feed

①目的:用高效液相色谱仪(HPLC)同时测定饲料中地西泮、安眠酮的含量。方法:在碱性条件下,用有机溶剂提取饲料中的地西泮和安眠酮,利用硅酸镁小柱对提取液进行富集、净化,用高效液相色谱仪进行检测。HPLC测定参数:C18柱(4.00mm×250mmi.d.,5μm);流动相乙腈—25mmol·L-1乙酸铵溶液(30:70);流速1.00mL·min-1;利用二极管阵列检测器测定地西泮、安眠酮紫外光区的特征光谱进行定性,外标法在254、226nm处进行定量。②结果:样品提取液中各组分分离良好,地西泮浓度在200ng·mL-1～100μg·mL-1范围内与峰面积呈线性相关,R=0.9992;平均回收率:92.28%～114.9%;变异系数(RSD)<5%;检测限(S/N=3)4ng。安眠酮浓度在250ng·ml-1～500μg·mL-1范围内与峰面积呈线性相关,R=0.9996;平均回收率:87.5%～112.9%;变异系数(RSD)<5%;检测限(S/N=3)1.2ng;其他常用镇静安眠药物在该条件下对地西泮、安眠酮均无干扰。③结论:是一种简便、快速、准确的方法。

①Objective： determine simultaneously diazepam and methaqualone in Feed by HPLC..Methods：C18 analytic column （4.00mm×250mm i.d.,5μm）.Acetonitrile-25mmol·L^-1 ammonium acetate （30：70）as the mobile phase. The flow rate was 1.00mL·min^-1. The detection wavelength was 254nm,226nm.It was as- sayed with external standard method.②Results： Diazepam：the linear range was 200ng.ml-^-100μg·ml^-1（r= 0.9992）. The average recoveries were92.28%-114.9%; RSD〈5%. The detection limit was 4ng （S/N=3）. Methaqualone： the linear range was 250ng·mL^- 1-500μg· mL^- 1 （r=0.9996）.The average recoveries were87.5%- 112.9%; RSD〈5%. The detection limit was 1.2ng（S/N=3）. ③Conclusion： The method is rapid, accurate and reliable .