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出 处:《分析试验室》2014年第5期582-585,共4页Chinese Journal of Analysis Laboratory
摘 要:采用磺丁基醚-β-环糊精(SBE-β-CD)为手性流动相添加剂,建立了反相高效液相色谱手性流动相添加剂法拆分分离佐匹克隆对映体的方法。在普通C增色谱柱(250mm×4.6mm×5.0μm)上,考察了水相pH、磺丁基醚-β-环糊精浓度、磷酸盐缓冲液浓度、甲醇含量、柱温等对佐匹克隆对映体拆分效果的影响。确定最适用的色谱条件:流动相为水相(5mmol/LNaH2PO4,含磺丁基醚-β-环糊精5mmo/L,以H3P04调pH为3):甲醇=78:22(v/v),检测波长305nm,流速为1mL/min,柱温为30℃,此条件下佐匹克隆对映体的保留时间分别为23.0和25.6min,分离度为1.81。两对对映体质量浓度在0.04~0.36g/L范围内线性关系良好(r≥0.9990),保留时间的RSD分别为0.73%和0.80%,峰面积的RSD分别为1.2%和1.1%。Some β-cyclodextrin derivatives are very excellent mobile phase additives for high pressure liquid chromatography and capillary electrophoresis. A RP- HPLC method is established to separate zopiclone enantiomers using Sulfobutyl ether-β-cyclodextrin (SBE-β-CD) as a chiral mobile phase additive in this paper. The influences of water phase pH , the concentration of sulfobutyl ether-β-cyclodextrin and NaH2PO4, the proportion of methanol content and column temperature on the resolution of enantiomers were investigated on a C18 column(250mm × 4.6mm × 5.0um). The optimal conditions of separation of zopielone enantiomers were achieved at 30℃ on the reversed - phase Cls column with a mobile phase of 5 mmo/L NaH2PO4 ( containing 5 mmo/L sulfobutyl ether-β-cyclodextrin, pH3.0) - Methanol = 78:22 (V/V) at the flow rate of 1.0 ml/min and the detection wavelength of 305 nm,the retention time of zopiclone enantiomers are 23.0 min ( RSD =0.73% ) and 25.6 min ( RSD = 0.80% ) respectively and the resolution is 1.81 under the optimal conditions. Good linearities of zopielone enantiomers were obtained in the range of 0.04 -0.36 g/L (r≥0.9990) with RSDs of 0. 73%, 0.80% for retention time and RSD of 1.2% , 1.1% for peak area, respectively.
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