GITC手性试剂衍生化高效液相色谱法分离测定血浆中普罗帕酮对映体  

RESOLUTION AND DETERMINATION OF PROPAFENONE ENANTIOMERS IN HUMAN DERIVATIZATION AND REVERSED-PHASE LIQUID CHROMATOGRAPHY

作　　者：张宜[1] 陈鹰[1] 裘军[2] 李高[2] 田世雄[2] 

机构地区：[1]中国人民解放军广州军区武汉总医院,武汉430070 [2]同济医科大学药学院,武汉430030

出　　处：《解放军药学学报》1999年第2期6-9,共4页Pharmaceutical Journal of Chinese People's Liberation Army

摘　　要：目的：建立分离测定血浆中普罗帕酮（ＰＰＦ） 对映体浓度的ＨＰＬＣ方法，为临床对ＰＰＦ对映体的药动学研究提供分析技术。方法：用乙酰葡萄糖异硫氰酸酯（ＧＩＴＣ） 作手性衍生化试剂，产生非对映异构体。以含０ ．０１ ％ 冰醋酸的乙腈－ 水（３∶２）为流动相。采用内标法，紫外检测波长为２１０ｎｍ 。结果：实验表明，Ｒ－ ＰＰＦ与Ｓ－ ＰＰＦ的分离度好。日内、日间的ＲＳＤ 均小于１１ ％ 。血药浓度在５０ ～５００ｎｇ·ｍｌ－１ 范围内呈线性关系，ｒ ＞ ０．９９６ 。AIM To establish a convenient and sensitive HPLC method for separation and determination of the enantiomers of propafenone(PPF) in human plasma, and to provide a scientific analytical technique for the studies of the pharmacokinetics for those Chinese oftaking PPF enantiomers.METHOD The method was based on derivatization with the chiral reagent 2,3,4,6-tetra-o-acetyl-β-D-glucopyranosyl isothiocyanate (GITC), and resolution of the resulting diastereomeric thioureas by reversed-phase HPLC, using acetonitrite-water(3∶2) containing 0.01% acetic acid as the mobile phase.The detection wavelength was 210 nm, Li-1115 was used as the internal standard.RESULTS The separation of the PPF enantiomers and I.S. was proved to be highly satisfactory. The accuracy (percentage error) was excellent.Both RSD of intra-day and inter-day were less than 11%. The assay linearity was determined over the range of 50～500ng·ml -1 in plasma(r>0.996).CONCLUSION This method possesses high accuracy and precision, and is sensitive and specific.The applicability of the assay to the pharmacokinetic studies of the enantiomers of PPF is also demonstrated.

关 键 词：GITC手性试剂 高效液相色谱法 血浆 普罗帕酮 药动学 

分 类 号：R914[医药卫生—药物化学]