高效液相色谱-手性配位基交换流动相法拆分甲状腺片中甲状腺素对映体  被引量:4

Determination of D - and L - Thyroxine Enantiomers in Thyroid Tablets with Normal HPLC - Chiral Complexes Exchange Mobile Phase

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作  者:王荣[1] 贾正平[2] 谢景文[2] 胡晓丽[2] 李永民[1] 陈立仁[1] 邬静[3] 

机构地区:[1]中国科学院兰州化学物理研究所,兰州730000 [2]兰州军区兰州总医院药材科,兰州730050 [3]兰州军区联勤部药品仪器检验所,兰州730050

出  处:《药物分析杂志》2002年第4期267-269,共3页Chinese Journal of Pharmaceutical Analysis

基  金:全军"十五"医药科研资助项目(01Q013)

摘  要:目的:运用正相高效液相色谱-手性配位基交换流动相法,建立甲状腺片中甲状腺素对映体(L-,D-T_4)的拆分方法。方法:通过流动相中添加L-脯氨酸、醋酸铜及三乙胺对甲状腺片中甲状腺素对联体进行测定。最佳色谱条件为流动相:乙腈-水(35:65),每升流动相水中(未加乙腈)含有0.1mmol·L^(-1)醋酸铜(Ⅱ),0.2 mmol·L^(-1)L-脯氨酸和0.5mmol·L^(-1)三乙胺;pH为5.42;柱温:40℃;流速:1.0mL·min^(-1);色谱柱:Hypersil SiO_25μm(4.6mm×250mm);紫外测定波长:225nm。结果:在所建立的色谱条件下甲状腺素L-,D-2种异构体得到基线分离,并测定了甲状腺片中的L-,D-T_4的含量,结果显示同一厂家不同批号甲状腺片中L-,D-T_4含量不同。结论:所建立的方法简便、快速、准确、成本低,可作为样品的检测及药品质量控制方法。Objective: To established a HPLC assay method for the separation and the determination of L - and D - thyroxine enantiomers (L - , and D - T4 ) in thyroid tablets. Method: A normai phase - chiral mobile phase chromatography method has been developed that the method includes extraction of thyroxine from tablet and separation of thyroxine enantiomers on HPLC silica eolumn with chiral eluent containing L - proline, cupric acetate and triethylamine (TEA). Results: The sensitivity of the method was 0. 1 μg ·mL-1. The precision of interday and intarday, linearity, extraction recovery, and stability of T4 enantiomers in thyroxine tablets was determined for the validation of the method. Baseline enantioseparations of compounds containing D - and L - T4 was achieved. We determined the L - , D - T4 concentration of the different lot number of same factor in thyroid tablets. The result showed the different L - , D - T4 concentration in the different lot number thyroid tablets. Conclusiori: The im-proved method is rapid, accurate and reproducible. It is suitable for the quality control of the thyroxine enantiomers in tablets.

关 键 词:高效液相色谱 手性配位基交换流动相分析 甲状腺片 甲状腺素对映体 药品质量控制 

分 类 号:R927.1[医药卫生—药学]

 

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