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采用新型的硝基苯胺衍生化β-环糊精键合有序介孔SBA-15液相色谱手性固定相(NCDSP),在极性有机模式下实现了美托洛尔对映体的快速拆分。优化了流动相中甲醇含量、冰乙酸、三乙胺的比例和含量,并研究了温度对分离的影响。实验表明优化的色谱条件为:乙腈/甲醇/冰乙酸/三乙胺体积比95/5/1.5/1.5,流速为0.5 mL/min,柱温为20℃,检测波长为275 nm。在该条件下,美托洛尔对映体的离度为1.80,拆分时间较短(<15 min)。在此基础上建立了酒石酸美托洛尔药片中对映体含量的快速测定方法,两对映体的浓度在2.2~140μg/mL范围内呈良好的线性关系(r=0.9993~0.9996),平均回收率为97.6%~103.4%,检出限为0.2μg/mL,两对映体测定结果的日内和日间RSD分别小于1.4%和1.9%(n=5)。
The novel nitroaniline-derivatized β-cyclodextrin bonded ordered mesoporous SBA-15 liquid chromatography chiral stationary phase (NCDSP) was used to achieve the rapid enantioselectivity of metoprolol in polar organic mode Split. The mobile phase methanol content, glacial acetic acid, triethylamine ratio and content were optimized, and the influence of temperature on the separation was studied. The experimental conditions showed that the optimal chromatographic conditions were as follows: acetonitrile / methanol / glacial acetic acid / triethylamine volume ratio 95/5 / 1.5 / 1.5, flow rate 0.5 mL / min, column temperature 20 ℃ and detection wavelength 275 nm. Under this condition, the resolution of the metoprolol enantiomer was 1.80 and the resolution time was shorter (<15 min). On this basis, a rapid determination method for the enantiomeric contents of metoprolol tartrate tablets was established. The two enantiomers showed a good linear relationship (r = 0.9993 ~ 0.9996) in the range of 2.2 ~ 140μg / mL with an average of The recoveries ranged from 97.6% to 103.4% with a detection limit of 0.2 μg / mL. The daily and intraday RSDs of the two enantiomers were less than 1.4% and 1.9%, respectively (n = 5).