维生素H中间体手性内酯衍生化高效液相色谱检测研究  

Study on the Detection of the Intermediate Lactone of Vitamin H via Derivatization HPLC

作　　者：章良 王建军 秦飞 梁玲玲[2] 宋少奇 于绪平[2] 吴春雷[3] ZHANG Liang;WANG Jian-jun;QIN Fei;LIANG Ling-ling;SONG Shao-qi;YU Xu-ping;WU Chun-lei(Zhejiang Zhongxian Biotechnology Co.Ltd.,Shaoxing,312000,China;Zhejiang Pharmaceutical Co.Ltd.,Shaoxing,312000,China;College of Chemeal Engineering,Shaoxing University,Shaoxing 312000,China)

机构地区：[1]浙江中贤生物科技有限公司,浙江绍兴312000 [2]浙江医药股份有限公司,浙江绍兴312000 [3]绍兴文理学院,化学化工学院,浙江绍兴312000

出　　处：《安徽化工》2025年第1期149-153,共5页Anhui Chemical Industry

摘　　要：对维生素H的关键中间体(3aS,6aR)-1,3-二苄基四氢-1H-呋喃[3,4-d]咪唑-2,4-二酮(右内酯)及其制备过程中产生的对映体杂质(3aR,6aS)-1,3-二苄基四氢-1H-呋喃[3,4-d]咪唑-2,4-二酮(左内酯)混合物的分离检测做了研究。将上述左、右内脂的混合物和(1R,2R)-(-)-苏-1-(对硝基苯基)-2-胺基-1,3-丙二醇(右胺)进行衍生化反应,两者的衍生物在高效液相色谱中可以顺利分开。此外,对左右内脂的衍生化反应条件做了筛选,使得反应收率达98%。对液相条件进行了优化,两个衍生物的分离度为4.25,液相色谱条件为色谱柱:C-18(250 mm×4.6 mm,5μm);流动相:乙腈∶0.025 mol·L^(-1)磷酸二氢钾溶液(30∶70,v/v);流速为1.0 mL·min^(-1);检测波长为254 nm;柱温为30℃;进样量为10μL。该方法为维生素H中间体左、右内脂的分离检测提供了一种思路。The study on the detection between the key intermediate(3aS,6aR)-1,3-dibenzyl-tetrahydro-1H-furo[3,4-d]imidazole-2,4-dione of vitamin H anditsimpurity(3aR,6aS)-1,3-dibenzyl-tetrahydro-1H-furo[3,4-d]imidazole-2,4-dione was carried out in this paper.The mixtures of the above two lactones was then reacted with(1R,2R)-2-amino-1-(4-nitrophenyl)propane-1,3-diol in n-butanol in a yield of 98%to afford the corresponding derivatives.The HPLC sepa⁃ration degree of the two derivatives was 4.25,and the HPLC conditions were as follows:column:C-18(250 mm×4.6 mm,5μm);mobile phase:acetonitrile:0.025 mol·L^(-1) potassium dihydrogen phosphate solution(30∶70,v/v);the flow rate:1.0 mL·min^(-1);the detection wavelength:254 nm;the column temperature:30℃;the injection volume:10μL.It provides a feasible method for the detection of chiral lactone content in industrial production.

关 键 词：维生素H (3aS 6aR)-1 3-二苄基四氢-1H-呋喃[3 4-d]咪唑-2 4-二酮 衍生化法 高效液相色谱法 

分 类 号：O657[理学—分析化学]