摘要
建立了一种超高效合相色谱法(Ultra performance convergence chromatography,UPC^2)分离和测定盐酸兰地洛尔中立体异构体的方法。本方法选用Daicel CHIRALPAK IF手性色谱柱(150 mm×4.6 mm,3μm),以CO_2为流动相,甲醇-正丁醇-乙腈(1∶1∶1,V/V)+0.5%氨水为助溶剂,梯度洗脱,流速为2.8 m L/min,检测波长为223 nm。在建立的UPC^2条件下,盐酸兰地洛尔的R,R-异构体、R,S-异构体和S,R-异构体的检出限分别为0.3、0.4和0.3 mg/L;线性范围分别为2~300 mg/L、5~300 mg/L和2~300 mg/L;加标回收率分别为103.4%,91.8%和101.7%;进样精密度分别为0.06%,0.09%和0.08%(n=6)。本方法能够满足盐酸兰地洛尔样品中3个立体异构体检查的相关要求。
A new method for chiral separation and purity inspection of landiolol hydrochloride and its stereoisomers was developed by ultra-performance convergence chromatography（ UPC^2）. The mobile phase was the mixture of supercritical CO2 and methanol / n-butyl alcohol / acetonitrile（ 1 ∶ 1 ∶ 1,V / V） plus 0. 5%NH3·H2O. The separation was carried out on the Daicel CHIRALPAK IF column（ 150 mm × 4. 6 mm,3 μm） with a flow rate of 2. 8 m L / min at 50℃ using 223 nm as detection wavelength. Under the optimized experimental conditions,for R,R-stereoisomer,R,S-stereoisomer and S,R-stereoisomer,the detection limits（ LOD,S /N = 3） were 0.3,0.4 and 0.3 mg /L,the linear ranges were 2-300 mg /L,5- 300 mg /L and 2-300 mg / L,the recoveries of spike samples were 103.4% ± 2.5%,91.8% ± 2.5% and 101.7% ± 1.5%,and the injection repeatabilities were 0.06%,0.09% and 0.08%（ n = 6）,respectively. The experimental results demonstrate that the UPC^2-based method can be used for the analysis and determination of landiolol hydrochloride and its stereoisomers.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2016年第9期1348-1353,共6页
Chinese Journal of Analytical Chemistry
基金
科技重大专项重大新药创制项目(No.2015ZX09303001)资助~~
关键词
超高效合相色谱法
盐酸兰地洛尔
立体异构体
手性拆分
Ultra performance convergence chromatography
Landiolol hydrochloride
Stereoisomers
Chiral separation
