3-脱氧葡萄糖醛酮代谢产物——3-脱氧果糖的HPLC检测方法初步建立  

Preliminary HPLC Method for the Determination of 3-Deoxyfructose,a Metabolite of 3-Deoxyglucuronide

作　　者：李涵艺 江国荣[1,3] 许恒 季亚男[1,2] 张露蓉 LI Han-yi;JIANG Guo-rong;XU Heng;JI Ya-nan;ZHANG Lu-rong(Laboratory of Clinical Pharmacy of Traditional Chinese Medicine,Suzhou Hospital of Traditional Chinese Medicine,Nanjing University of Chinese Medicine,Suzhou 215009,China;Nanjing University of Chinese Medicine,Nanjing 210023,China;Laboratory of Clinical Pharmacy of Traditional Chinese Medicine,Suzhou Institute of Wu Men Medical School,Suzhou 215009,China)

机构地区：[1]南京中医药大学附属苏州市中医医院中药临床药学实验室,江苏苏州215009 [2]南京中医药大学,江苏南京210023 [3]苏州市吴门医派研究院中药临床药学实验室,江苏苏州215009

出　　处：《纤维素科学与技术》2023年第1期16-22,共7页Journal of Cellulose Science and Technology

基　　金：国家自然科学基金资助项目(81973740)。

摘　　要：建立了3-脱氧果糖(3-DF)初步检测的高效液相色谱(HPLC)方法。先使用气相色谱―质谱联用(GC-MS)对合成的3-DF标样进行鉴定。再采用C18反相色谱柱,流动相为乙腈-水(10%∶90%~90%∶10%)梯度洗脱60min,紫外检测波长352nm,应用2,4-二硝基苯肼柱前衍生法,以薄层色谱―高效液相色谱联用(TLC-HPLC)对3-DF衍生物峰进行定位,并完善衍生条件,进行方法学考察。结果表明:合成样品为3-DF;衍生条件以衍生液中1∶3添加乙酸乙酯效果最佳;3-DF衍生物峰出峰时间为15.972 min,呈尖峰,分离度良好,线性范围为0.5~8 mg/mL,方法精密度RSD为2.4%,重复性RSD为4.4%,稳定性RSD为2.4%。本检测方法稳定、可靠,可初步用于3-DF定性及相对定量。A high performance liquid chromatography(HPLC)method for the preliminary determination of 3-deoxyfructose(3-DF)was established.3-DF samples were identified using gas chromatography mass spectrometry(GC-MS).A C18 reverse phase chromatographic column was used,and the mobile phase was acetonitrile water(10%∶90%~90%∶10%)gradient elution for 60 minutes.The UV detection wavelength was 352 nm.A pre column derivatization method of 2,4-dinitrophenylhydrazine was used to localize the peaks of 3-dF derivatives using thin layer chromatography coupled with high performance liquid chromatography(TLC-HPLC),and the derivatization conditions were optimized for methodological investigation.The results showed that the synthesized sample was 3-DF.The best derivatization conditions were 1∶3 addition of ethyl acetate to the derivatization solution.The peak time of the 3-DF derivative was 15.972 minutes,showing a sharp peak.The resolution was good,with a linear range of 0.5~8 mg/mL,a method precision RSD of 2.4%,a repeatability RSD of 4.4%,and a stability RSD of 2.4%.This detection method was stable and reliable,and could be initially used for qualitative and relative quantitative analysis of 3-DF.

关 键 词：3-脱氧果糖 3-脱氧葡萄糖醛酮 2 4-二硝基苯肼 高效液相色谱 气相色谱―质谱联用 薄层色谱―高效液相色谱联用 

分 类 号：O657.72[理学—分析化学] TQ460.1[理学—化学]