摘要
本文报道用高效液相色谱法同时测定血清中氢化泼尼松和氢化可的松浓度,血清样品经醋酸乙酯1次提取浓集后进样,采用YQG-80国产硅胶分析柱,以二氯甲烷─甲醇(97:3)为流动相,地塞米松作内标,在254nm波长下测定洗提液,按内标法定量,并对提取及色谱条件等进行了探讨。本法具有快速、简便、灵敏、准确等特点,适用于使用相关药物或未用药病人血中氢化泼尼松、氢化可的松浓度的同时或单独测定。
A sensitive and specific method for the simultaneous measuremnet of both prednisolone (PL) and hydrocortisone (HC) in serum using dexamethasone (DX) as the internal standard was reported.High-performance liquid chrornatograph Model 344 (Beckman. USA) with a 254nm wavelength UV detector and YQG-80 silica column(5μm,250mm×4. 6mm)was used.Serum sample(0.5ml) was extracted with 2.5ml ethyl acetate and the organic layer was evaporated to dryness under an air stream in a 37℃ water bath,The residue was dissoved in 30μl mobile phase and 20μl injected. The mobile phase of methylene chloride and methanol ( 97: 3) was pumped at 2.0ml/min through the column.The detector was operated at 0. 002AUFS. The retention time for PL, HC and DX was 10.36,7. 63 and 6. 30min, respectively.Standard curve was linear in the concentration range of 0.03125 to 1. 0μ mol/L for both PL and HC.The detection limits in serum was 0.02μ mol/L for PL and 0. 012μ mol/L for HC.Extraction recovery was 81%~89%,within-day RSD was less than 4.5%.inter-day RSD was less than 8.5% for both PL and HC.
出处
《药物分析杂志》
CAS
CSCD
北大核心
1995年第4期9-12,共4页
Chinese Journal of Pharmaceutical Analysis