摘要
采用柱前手性衍生化方法，氯仿为提取溶剂，以Ｎ三氟乙酰基脯氨酰氯［（Ｓ）（－）Ｎ（Ｔｒｉｆｌｕｏｒｏａｃｅｔｙｌ）ｐｒｏｌｙｌｃｈｌｏｒｉｄｅ，ＳＴＦＰＣ］为手性衍生化试剂，三乙胺为催化剂，将安非他明转变成相应的酰胺类非对映异构体对，用常规非手性毛细管柱气相色谱，程序升温法分离了大鼠肝微粒体中Ｒ和Ｓ安非他明，在５～２５０μｇ／ｍＬ范围内线性良好，线性方程分别为：Ｒ（－）安非他明：Ｙ＝６９２＋６２１８Ｘ，ｒ＝０９９８；Ｓ（＋）安非他明：Ｙ＝６４７＋５６０５Ｘ，ｒ＝０９９７９。方法回收率±Ｓ：左旋安非他明（７６４９％±６５５）～（７８５７％±３８９）；右旋安非他明为（７３１５％±４１９）～（７５７８％±１９７）。方法检测限为１２５ｎｇ，定量限为１２５ｎｇ（ＲＳＤ＜１１％）。重现性和精密度均良好，相对标准偏差小于４８％。通过测定安非他明在大鼠肝微粒体中一相代谢时间反应曲线，表明安非他明在大鼠肝微粒体中经历了立体选择性代谢。
A chiral assay for amphetamine enantiomers in rat liver microsomal incubate is based on pre-column chiral derivatization with (S) N trifluoroacetyl prolylchloride(S TFPC),followed by capillary chromatographic separation of the diastereomeric amide derivatives and detection by flame ionization detector.The method is capable of detecting low level of R (-) or S (+) amphetamine.The assay is linear from 5 to 250 μg/mL for each enantiomer.The limit of detection is 12 5 ng and the limit of quantitation is 12 5 ng(RSD<11 %) for each enantiomer.The analytical method affords the average recoveries of (76 49 %±6 55)～(78 57 %±3 89) for R (-) amphetamine and (73 15 %±4 19)～(75 78 %±1 97) for S (+) amphetamine.The method allowed study of the metabolic depletion of R (-) and S (+) amphetamine in rat liver microsomal incubates.The time-dependent concentration of amphetamine enantiomers in rat liver microsome was determined and the stereoselectivity of amphetamine phase I metabolism was observed.
出处
《药物分析杂志》
CAS
CSCD
北大核心
1998年第5期291-295,共5页
Chinese Journal of Pharmaceutical Analysis
基金
国家自然科学基金
关键词
安非他明
对映体
手性衍生化
气相色谱
肝
amphetamine enantiomer,chiral derivatization reagent,stereoselective analysis,gas chromatography
