高效液相色谱法测定药品中的二硫苏糖醇和氧化型二硫苏糖醇  

Determination of Dithiothreitol and Oxidized Dithiothreitol in Medicine Using High Performance Liquid Chromatography

作　　者：罗宁[1] 刘平怀[1] 吴晓娜 陈晨[1] 张玲[1] 何沂飞[1] 李昂[1] 

机构地区：[1]海南大学材料与化工学院,热带作物种质资源保护与开发利用教育部重点实验室,海南海口570228

出　　处：《分析科学学报》2016年第4期537-540,共4页Journal of Analytical Science

基　　金：国家科技支撑计划(No.2011BAD14B01);海南省中药现代化科技专项(No.ZY201327);国家科技型中小企业技术创新基金(No.13C26244604892);海南省产学一体化项目(No.CXY20150034)

摘　　要：建立了高效液相色谱法同时测定药品中二硫苏糖醇(DTT)和氧化型二硫苏糖醇(DTTox)含量。采用Waters X-Bridge C18柱(250×4.6mm,5μm)分离,流动相为体积比为30∶70的甲醇-水(含0.02%三氟乙酸),检测波长为210nm。结果表明,DTT和DTTox在选定质量浓度范围内呈良好的线性关系(r>0.999),DTT和DTTox的检出限(S/N=3)为0.02μg/mL,定量限(S/N=10)为0.07μg/mL。平均加标回收率分别为99.32%、99.49%,相对标准偏差分别为2.34%、2.23%。该方法简单、准确,灵敏度高,重复性好,适用于药品中DTT和DTTox的检测。A method was developed for the simultaneous determination of dithiothreitol （DTT） and oxidized dithiothreitol（DTTox） in medicine by high performance liquid chromatography（HPLC）. The mobile phase consisted of methanol-water （30：70,V/V） with 0.02% trifluoroacetic acid. The chromatographic conditions were as follows：flow rate, 1. 0 mL/min; the detection wavelength, 210 nm; the column temperature, 40 ℃; the injection volume, 100 μL. Under these conditions, good linear relationships between the mass concentration and the peak areas of DTT and DTTox were observed in the selected mass range（r〉0. 999）. The limits of detection（LODs,S/N=3） and limits of quantitation（LOQs,S/N=10） were determined as 0.02 μg/mL and 0.07 μg/mL,respectively. The average recoveries were 99.32% for DTT and 99.49% for DTTox,and RSDs were 2.34%（n=6） for DTT and 2.23%（n=6） for DTTox. The results showed that the developed method was sensitive, accurate and reproducible. It is suitable for the analysis of DTT and DTTox in medicine.

关 键 词：高效液相色谱 二硫苏糖醇 氧化型二硫苏糖醇 

分 类 号：O657.72[理学—分析化学]