作　　者： ; ; ; ; ; ; ; ;

机构地区： 兰州军区兰州总医院

出　　处： 《色谱》 2011年第1期26-30,共5页

摘　　要： 建立正相液相色谱-串联质谱（LC-MS/MS）分离普萘洛尔对映体的方法,并用于盐酸普萘洛尔片对映体含量测定。样品使用甲醇进行简单提取,采用Chiralcel OD-H手性柱,以正己烷-乙醇-氨水（70∶30∶0.4,v/v/v）为流动相,流速为0.4mL/min。在正离子模式下,通过电喷雾离子化（ESI＋）,采用多反应监测（MRM）方式进行检测,用于定量分析检测的离子对为m/z260.2→116.0,在20min内完成普萘洛尔对映体定量分析。盐酸普萘洛尔对映体在2.5-1 000μg/L质量浓度范围内线性关系良好,定量限为2.5μg/L;日内及日间测定的相对标准偏差小于2.64%。两种对映体的加样回收率范围分别为99.08%-102.58%和100.21%-103.16%。该方法准确、简便、可靠、有效,可用于盐酸普萘洛尔片对映体的质量控制。 A rapid and sensitive method was developed and validated using a normal phase liquid chromatography coupled with tandem mass spectrometry（LC-MS/MS） for determination of propranolol enantiomers in pharmaceuticals.Sample preparation involved a single extraction step by the addition of methanol.Separation of propranolol enantiomers was achieved on a Chiralcel OD-H chiral column using a mobile phase consisting of n-hexane-ethanol-ammonia（70∶30∶0.4,v/v/v）,and the flow rate was 0.40 mL/min for 20 min.The analyte was monitored by tandem mass spectrometry with electrospray positive ionization in multiple reaction monitoring（MRM） mode,using the transitions of m/z 260.2→116.0.Propranolol enantiomers can be completely separated.The linear range was 2.5-1 000 μg/L,and the limit of quantification（LOQ） was 2.5 μg/L.The values for within day and between day precisions and accuracies were well within the generally accepted criteria for analytical methods.The relative standard deviations（RSDs） were less than 2.64%,and the recoveries of the two enantiomers were 99.08%-102.58% and 100.21%-103.16%,respectively.The separation method is accurate,convenient,reliable,efficient,and can be subsequently used for quality control of propranolol enantiomers in pharmaceuticals.

关 键 词： 正相液相色谱 串联质谱 手性分离 测定 普萘洛尔对映体

领　　域： [理学] [理学]