柱前衍生化反相高效液相色谱法测定去水卫矛醇的含量  

Determination of Dianhydrogalactitol by Pre-column Derivatization and RP-HPLC

作　　者：王杏利 孙丽涵 张雷 吴华晶 张峻颖[2] 吴春勇[1,3] WANG Xingli;SUN Lihan;ZHANG Lei;WU Huajing;ZHANG Junying;WU Chunyong(Key Laboratory of Drug Quality Control and Pharmacovigilance, Ministry of Education, China Pharmaceutical University, Nanjing 210009, China;Department of Pharmaceutics of Traditional Chinese Medicine, China Pharmaceutical University, Nanjing 211198, China;Department of Pharmaceutical Analysis, China Pharmaceutical University, Nanjing 210009, China;Shandong Institute for Food and Drug Control, Jinan 250101, China)

机构地区：[1]中国药科大学药物质量与安全预警教育部重点实验室,南京210009 [2]中国药科大学中药制剂系,南京211198 [3]中国药科大学药物分析系,南京210009 [4]山东省食品药品检验研究院,济南250101

出　　处：《医药导报》2019年第5期641-645,共5页Herald of Medicine

基　　金：国家自然科学基金资助项目(81473357;81673681);中央高校基本科研业务费资助项目(2015PT062);江苏高校优势学科建设工程资助项目

摘　　要：目的建立测定去水卫矛醇含量的柱前衍生化反相高效液相色谱法(RP-HPLC)。方法去水卫矛醇经二乙基二硫代氨基甲酸钠衍生化后进行RP-HPLC分析,采用Welch Ultimate XB-CN色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈-水(50∶50),流速为1.0 m L·min^(-1),检测波长为278 nm。结果 40℃下衍生化反应可在30 min内完成,去水卫矛醇衍生物在10 h内稳定。去水卫矛醇在0.100～20.0μg獉m L^(-1)范围内线性关系良好(r=0.999 8)。检测限(LOD)和定量限(LOQ)分别为30和100 ng·m L^(-1)。方法专属性、准确度和精密度均符合要求。结论该方法快速、准确、灵敏,具有良好的专属性和重复性,可用于去水卫矛醇的质量控制。Objective To establish a reversed-phase high performance liquid chromatographic (RP-HPLC) method with pre-column derivatization for determination of dianhydrogalactitol. Methods After dianhydrogalactitol was derivatized with sodium diethyldithiocarbamate, the RP-HPLC separation was performed on a Welch Ultimate XB-CN column (250 mm× 4.6 mm ,5 μm) with the mixture of acetonitrile-water (50 : 50) as the mobile phase. The flow rate was 1.0 mL·min^-1 and the detection wavelength was set at 278 nm. Results The derivatization reaction could be finished within 30 min at 40 ℃ and the derivative was stable within 10 h. The calibration curve was linear over the range of 0.100-20.0 μg·mL^-1 ( r =0.999 8). The limit of detection (LOD) and limit of quantification (LOQ) was 30 and 100 ng·mL ^-1 , respectively. The method showed good specificity, accuracy and precision. Conclusion The proposed method was fast, accurate and sensitive with high specific and repeatability. The study provides a new approach for the quality control of dianhydrogalactitol.

关 键 词：去水卫矛醇 柱前衍生化 色谱法 反相高效液相 含量测定 

分 类 号：R971[医药卫生—药品] R927.2[医药卫生—药学]