摘要
目的建立美西律对映体在人血清白蛋白中的测定方法。方法采用手性衍生化试剂2,3,4,6-四-O-乙酰基-β-D-吡喃葡萄糖异硫氰酸酯(GITC)对美西律进行柱前手性衍生化。衍生产物以乙腈-0.01mol·L^-1磷酸二氢钾(pH4.5)缓冲液(1∶1)为流动相,用C18色谱柱分离,以R-艾司洛尔为内标,流速为1.0mL·min^-1,检测波长为250nm。结果实验表明,R-美西律与S-美西律的分离度良好。日内、日间RSD均小于15%。美西律对映体在0.1-40.0mg·L^-1内呈线性关系,r=0.9995。结论该方法结果准确,重现性好,灵敏度高,可用于美西律对映体的蛋白结合研究。
OBJECTIVE To develope enantiomeric separation method for mexiletine enantiomers in human serum albumin. METHODS The mexiletine enantiomers were separated on a C18 column after chiral derivatization with 2,3,4,6-tetra-O-acetyl- β-D- glucopyranosyl isothiocyanate (GITC). The mobile phase consisted of acetonitrile-0.01 mol ·L^-1 potassium dihydrogen phosphate buffer ( pH 4. 5 ) ( 1 : 1 ) at the flow rate of 1.0 mL· min ^- 1. R-esmolol was used as the internal standard. The UV detection wavelength was set at 250 nm. RESULTS The mexiletine enantiomers and internal standard were separated on base-line. The intra-day and interday variations were less than 15%. The assay linearity was determined over the range of 0. 1 -40. 0 mg ·L^-1 ,r =0. 999 5. CONCLUSION The method established is accurate, precision, sensitive and specific. The validated method has been used for protein binding studies of mexiletine enantiomers.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2007年第11期860-862,共3页
Chinese Pharmaceutical Journal
基金
国家杰出青年基金资助项目(30225047)