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文摘
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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2.51 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 |
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其他语种文摘
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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 |
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来源
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色谱
,2011,29(1):26-30 【核心库】
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DOI
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10.3724/sp.j.1123.2011.00026
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关键词
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正相液相色谱-串联质谱
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手性分离
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测定
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普萘洛尔对映体
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地址
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兰州军区兰州总医院全军临床药理基地, 甘肃, 兰州, 730050
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语种
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中文 |
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文献类型
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研究性论文 |
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ISSN
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1000-8713 |
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学科
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化学 |
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基金
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国家自然科学基金项目
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甘肃省科技支撑计划项目
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文献收藏号
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CSCD:4121316
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