论文部分内容阅读
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 establish a method for the resolution of thyroxine enantiomers (L- and D-T_4) in thyroid gland by normal-phase high performance liquid chromatography-chiral ligand exchange mobile phase. Methods: The thyroxine conjugates in thyroid tablets were determined by adding L-proline, copper acetate and triethylamine in the mobile phase. The best chromatographic conditions were as follows: acetonitrile-water (35:65), 0.1 mmol·L -1 copper acetate (Ⅱ), 0.2 mmol·L -1 1) L-proline and 0.5 mmol·L -1 triethylamine; pH 5.42; column temperature 40 ℃; flow rate 1.0 mL · min -1; column: Hypersil SiO 25μm 4.6 mm × 250mm); UV detection wavelength: 225nm. Results: Under the chromatographic conditions established, L-, D-2 isomers of thyroxine were baseline separated and the content of L- and D-T_4 in the thyroid gland was determined. The results showed that in different thyroid glands of the same manufacturer L-, D-T_4 content is different. Conclusion: The established method is simple, rapid, accurate and low cost and can be used as a sample testing and drug quality control methods.