高效液相色谱法法测定TH-302肝动脉栓塞微球的体外释放药量  

Determination of the release of TH-302 hepatic artery embolic microspheres in vitro by HPLC

作　　者：唐雪梅[1,2] 渠海贤 高越 梅兴国 喻芳邻 刘燕 王志军 施瑞珊[5] 赵悦 俞捷 李志平[2] TANG Xue-mei;QU Hai-xian;GAO Yue;MEI Xing-guo;YU Fang-ling;LIU Yan;WANG Zhi-jun;SHI Rui-shang;ZHAO Yue;YU Jie;LI Zhi-ping(Yunnan University of Traditional Chinese Medicine,Kunming 650500,China;Institute of Pharmacology and Toxicology,Academy of Military Medical Sciences,Academy of Military Sciences,Beijing 100850,China;Geneal Hospital of PLA,Beijing 100853,China;School of Chemical Engineering and Pharmacy,Wuhan Institute of Technology,Wuhan 430070,China;Changzhi Medical College,Changzhi 046000,China)

机构地区：[1]云南中医学院,昆明650500 [2]军事科学院军事医学研究院毒物药物研究所,北京100850 [3]中国人民解放军总医院,北京100853 [4]武汉工程大学化工与制药学院,武汉430070 [5]长治医学院,长治046000

出　　处：《国际药学研究杂志》2018年第4期320-324,共5页Journal of International Pharmaceutical Research

基　　金：国家自然科学基金资助项目(81671790)

摘　　要：目的建立TH-302肝动脉栓塞微球体外释放药量的测定方法。方法采用高效液相色谱法测定。色谱柱为:Venusil ASB C18(4.6 mm×150 mm,5μm);流动相为乙腈-水(30∶70,V/V);流速为1.0 ml/min;检测波长为316 nm;柱温30℃;进样体积为10μl。结果 TH-302的定量限与检测限分别为1.4和0.4μg/ml,在0.1~10μg/ml范围内呈良好的线性关系,线性方程为Y=10.867X-0.3034(R2=1.0000,n=8);各浓度的平均回收率在98.99%~101.77%之间,RSD为0.07%;稳定性实验结果表明TH-302在微球长期释放条件下不稳定。为能准确测定TH-302含量,本文建立了TH-302体外长期释放条件下不同时间实际峰面积与理论降解药量的线性关系,线性方程为:A实际=0.0523M降解-1.4166(R2=0.9919)。结论该法专属性良好,可准确、快速、灵敏地测定TH-302的含量。Objiective To establish a high performance liquid chromatography（HPLC）method for the determination of the release of TH-302 hepatic artery embolization microspheres in vitro. Methods The release of TH-302 hepatic artery embolization microspheres in vitro was determined by HPLC. The Venusil ASB C18 column（4.6 mm×150 mm,5 μm）was used. The mobile phase consisted of acetonitrile-water（70∶30,V/V）with a flow rate of 1 ml/min,and the detection wavelength was 316 nm. The column temperature was 30℃ and the injection volume was 10 μl. Results The quantification limit and detection limit were 1.4 and 0.4 μg/ml,respectively. The calibration curves were linear within the range of 0.1-10 μg/ml,and the linear equation was Y=10.867 X＋0.3034（R2=1.0000,n=8）. For concentration,the average recovery was within the range of 98.99%-101.77%（n=9）（RSD%=0.07%）. The stability results showed that TH-302 was unstable under long-term release conditions,therefore,a linear relationship between the actual degradation peak area and the theoretical degradation content of TH-302 was established to calculate the microsphere release accurately.The linear equation was Aactual= 0.0523 Mdegredation-1.4166（R2=0.9919）. Conclusion The method could be used for the determination of the release of TH-302 hepatic artery embolization microspheres,which is convenient,fast,sensitive and reproducible,with good precision,specificity and accuracy.

关 键 词：TH-302 栓塞微球 释放度测定 降解峰 体外释放 

分 类 号：R917[医药卫生—药物分析学]