柱前衍生化高效液相色谱法测定2-去氧葡萄糖的含量  

Determination of 2-deoxyglucose by high performance liquid chromatography with precolumn derivatization

作　　者：洪碧红[1,2] 黄文文[1] 尤小云[1] 谢全灵[1] 刘俊朋[1] 易瑞灶[1] 

机构地区：[1]国家海洋局第三海洋研究所,福建厦门361005 [2]厦门大学材料学院,福建厦门361005

出　　处：《中国海洋药物》2011年第5期44-48,共5页Chinese Journal of Marine Drugs

基　　金：海洋公益性行业科研专项经费资助(No.201005020);福建省科技重大专项经费资助(No.2010NZ0001-2);厦门市海洋与渔业局科技计划项目经费资助(厦海渔合[2009]9号)

摘　　要：目的建立柱前衍生化高效液相色谱法测定2-去氧葡萄糖（2-DG）含量的方法。方法采用1-苯基-3-甲基-5-吡唑酮（PMP）为柱前衍生化试剂,将2-DG在碱性条件下衍生化后直接进样测定。分离柱为HypersilODS2色谱柱（4.6 mm×250 mm,5μm）,流动相为100 mmol·L-1醋酸铵缓冲液（pH 5.5）-乙腈（78∶22）,流速1.0 mL·min-1,波长249 nm。结果 2-DG在19.68~393.6μg·mL-1浓度范围内与峰面积具有良好的线性关系（r=0.9997）;其定量限（S/N=10）和最低检出限（S/N=3）分别为7.8和3.1 ng;平均回收率为101.21%,RSD 0.63%。结论该方法简便实用、检测灵敏度高、测定结果准确,适用于2-DG的质量控制。Objective An effective precolumn derivatization HPLC method was developed to determine 2-deoxyglucose（2-DG）.Methods The 2-DG after being derived with 1-phenyl-3-methyl-5-pyrazolone（PMP） in alkaline medium was injected directly for determination.The determination of 2-DG was performed on a Hypersil ODS2 column（250 mm×4.6 mm,5 μm） with a mobile phase of 100 mmol·L-1 ammonium acetate buffer（pH 5.5） to acetonitrile（v/v=78∶22）.The flow rate was 1.0 mL·min-1and the detection wavelength was set at 249 nm.Results A good linearity was observed in the concentration range from 19.68-393.6 μg·mL-1,and the correlation coefficient was 0.9997.The lowest detection and quantitative limits were 3.1and 7.8 ng,respectively.The average recovery was 101.21%,RSD 0.63%.Conclusion This method has good accuracy and repeatability and it can be used for the quality control of 2-DG.

关 键 词：2-去氧葡萄糖 柱前衍生化 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]