高效液相色谱法检测德拉昔布咀嚼片含量方法的建立  

Establishment of the HPLC Method for Determination of Deracoxib Chewable Tablets

作　　者：于泓潇 李思鸿 肖天石 张艺馨 杨雨齐 李佳瑞 杨洪亮 张秀英[1] YU Hong-xiao;LI Si-hong;XIAO Tian-shi;ZHANG Yi-xin;YANG Yu-qi;LI Jia-rui;YANG Hong-liang;ZHANG Xiu-ying(College of Veterinary Medicine,Northeast Agricultural University,Harbin 150030,China)

机构地区：[1]东北农业大学动物医学学院,黑龙江哈尔滨150030

出　　处：《中国兽医杂志》2021年第1期92-96,共5页Chinese Journal of Veterinary Medicine

摘　　要：为建立检测德拉昔布咀嚼片含量的方法,本试验采用高效液相色谱法对德拉昔布咀嚼片和Deramaxx咀嚼片进行含量测定。样品经粉碎与甲醇溶解,超声处理20 min,0.22μm滤膜滤过后进样测定。色谱条件:色谱柱Wasters C18(4.6 mm×250 mm,5μm);流动相为磷酸盐缓冲液(pH=4.5)∶乙腈(52∶48,v/v);检测波长252 nm;流速1 mL/min;柱温30℃。结果显示,德拉昔布标准品以甲醇为溶剂,进样浓度在0.5~8μg/mL,建立标准曲线,样品浓度与峰面积的线性关系良好(r^(2)=0.9992)。仪器精密度为0.56%,日内差异为0.94%,日间差异为1.85%,溶液稳定性为0.57%,平均加样回收率为(99.68±0.53)%。表明所建立的高效液相色谱含量检测方法简便、准确、专属性强,可用于德拉昔布咀嚼片含量的测定。To establish a method to determine the content of deracoxib chewable tablets,this study determined the contents of deracoxib chewable tablets and deramaxx chewable tablets by high performance liquid chromatography(HPLC).The samples were crushed,and then dissolved by methanol.After the ultrasonic treatment for^(2)0 min,the solution was filtrated by 0.22μm filter membrane then analyzed by HPLC.The chromatographic conditions were as follows:the HPLC column was Wasters C18(4.6 mm×250 mm,5μm);the mobile phase was phosphate buffer(pH=4.5)∶acetonitrile(52∶48)at a flow rate 1 mL/min;the detection wavelength was 252 nm;the column temperature was kept at 30℃.Results showed that the deracoxib standards were dissolved by methanol,the linear range of the calibration curve for deracoxib was 0.5-8μg/mL,and the linear relationship between sample concentration and peak area was good(r^(2)=0.9992).The instrument precision was 0.56%,inter-day coefficient of variation was 0.94%and intra-day coefficient of variation was 1.85%,the solvent stability was 0.57%,and the average recovery was(99.68±0.53)%.The results indicate that the method is simple and accurate with high sensitivity and specificity,which could be used to determine the content of deracoxib chewable tablets.

关 键 词：德拉昔布咀嚼片 高效液相色谱法 方法学研究 

分 类 号：S859.1[农业科学—临床兽医学]