Departamento de Química Inorgánica y Analítica, ESCET, Universidad Rey Juan Carlos, 28933 Móstoles, Madrid, Spain.
J Pharm Biomed Anal. 2012 Mar 25;62:33-41. doi: 10.1016/j.jpba.2011.12.029. Epub 2012 Jan 4.
The enantioselectivities of β-blockers (propranolol, metoprolol, atenolol and pindolol) on four different types of chiral stationary phases (CSPs): Chiralpak AD-H, Lux Cellulose-1, Chirobiotic T and Sumichiral OA-4900 were compared using polar organic (PO) elution mode and normal phase (NP) elution mode. Method optimizations were demonstrated by modifying parameters such as organic modifier composition (ethanol, 2-propanol and acetonitrile) and basic mobile phase additives (triethylamine, diethylamine, ethanolamine, and buthylamine). In normal phase elution mode with Lux Cellulose-1, the four pairs of enantiomers can be separated in the same run in gradient elution mode. Additionally, a simple chiral HPLC-DAD method using a newly commercialized polysaccharide-based CSP by Phenomenex (Lux Cellulose-1) in NP elution mode for enantioselective determination of propranolol in water samples by highly selective molecularly imprinted polymers extraction was validated. The optimized conditions were a mobile phase composed by n-hexane/ethanol/DEA (70/30/0.3, v/v/v) at a flow rate of 1.0 mL min(-1) and 25 °C. The method is selective, precise and accurate and was found to be linear in the range of 0.125-50 μg mL(-1) (R(2)>0.999) with a method detection limit (MLD) of 0.4 μg mL(-1) for both enantiomers. Recoveries achieved with both enantiomers ranged from 97 to 109%.
比较了β受体阻滞剂（普萘洛尔、美托洛尔、阿替洛尔和吲哚洛尔）在四种不同手性固定相（CSP）上的对映选择性：Chiralpak AD-H、Lux Cellulose-1、Chirobiotic T 和 Sumichiral OA-4900，使用极性有机（PO）洗脱模式和正相（NP）洗脱模式。通过修改有机改性剂组成（乙醇、2-丙醇和乙腈）和碱性流动相添加剂（三乙胺、二乙胺、乙醇胺和丁胺）等参数，展示了方法优化。在 Lux Cellulose-1 的正相洗脱模式下，四对对映异构体可以在梯度洗脱模式下在同一运行中分离。此外，还验证了一种使用 Phenomenex 新商业化的多糖基 CSP（Lux Cellulose-1）的简单手性 HPLC-DAD 方法，用于通过高度选择性的分子印迹聚合物萃取在 NP 洗脱模式下对水样品中的普萘洛尔进行对映选择性测定。优化条件为正己烷/乙醇/DEA（70/30/0.3，v/v/v）组成的流动相，流速为 1.0 mL min(-1)，温度为 25°C。该方法具有选择性、精确性和准确性，在 0.125-50 μg mL(-1)（R(2)>0.999）范围内呈线性，两种对映异构体的方法检测限（MLD）均为 0.4 μg mL(-1)。两种对映异构体的回收率均在 97%至 109%之间。
