摘要
目的 采用固相萃取-高效液相色谱（SPE-HPLC）联用技术建立珍菊降压片中盐酸可乐定的含量测定方法。方法 以Cleanert SCX-SPE阳离子固相萃取小柱对样品进行前处理，色谱柱为Agilent ZORBAX SB-C18（4.6 mm×250 mm，5 μm），流动相为乙腈-0.05%磷酸溶液（10∶90），流速1.0 ml/min，柱温30℃，检测波长为220 nm。结果 珍菊降压片中盐酸可乐定含量测定的回归方程为y=2.9662x＋0.0485（r=0.99999），在1.234～123.4 ng 的测定范围内线性关系良好；低、中、高3个剂量的平均回收率为98.56%，RSD为0.68%，方法的重复性、中间精密度和准确度良好，符合含量测定对方法的要求。结论 该方法有效地消除了阴性干扰，专属性、灵敏度、重现性和准确度良好，为珍菊降压片中盐酸可乐定的检测提供了可靠的技术手段。
Objective To establish a method for the content determination of clonidine hydrochloride in Zhenju Jiangya（ZJ） tablets by solid phase extraction and high performance liquid chromatography（SPE-HPLC）. Methods Samples were pretreated by Cleanert SCX-SPE cation solid phase extraction column and analyzed by HPLC consisting of a Agilent ZORBAX SB-C18 column （4.6 mm×250 mm, 5 μm） and a mixture of acetonitrile -0.05 % H3PO4（10∶90） solution as the mobile phase. The column temperature was 30℃,flow rate was 1.0 ml/min and wavelength was 220 nm. Results The determination of clonidine hydrochloride in ZJ tablets had the regression equation as y=2.9662x＋0.0485（r=0.99999）, which showed good linearity in the range of 1.234-123.4 ng. The average recovery of high, medium and low doses was 98.56% and RSD of recovery was 0.68%. This method had good repeatability, intermediate precision and accuracy, and met the requirement of content determination method. Conclusion This method can effectively eliminate the negative interference with good specificity, sensitivity, reproducibility and accuracy, and can be used as a reliable technical method to analyze clonidine hydrochloride in ZJ tablets.
出处
《国际药学研究杂志》
CAS
CSCD
2014年第1期114-117,共4页
Journal of International Pharmaceutical Research
基金
上海市科学技术委员会中药现代化专项(09DZ1977300)
关键词
珍菊降压片
盐酸可乐定
固相萃取
高效液相色谱法
含量测定
Zhenju Jiangya tablets
clonidine hydrochloride
solid phase extraction
high performance liquid chromatography
content determination
