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

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.