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目的:建立伏立康唑对映体HPLC手性分离及分析方法。方法:以β-CD及其衍生物为流动相手性添加剂,探讨β-CD衍生物类型及浓度、流动相中有机相体积分数、色谱柱固定相类型等因素对伏立康唑对映体HPLC手性拆分效果的影响,在此基础上,建立伏立康唑对映体的HPLC分析方法,并进行方法学考察。结果:β-CD衍生物中,SBE-β-CD适宜作为伏立康唑对映体HPLC手性拆分添加剂,以甲醇-水(45∶55)为流动相,磷酸二氢钾浓度为15 mmol.L-1,SBE-β-CD浓度为10.0 mmol.L-1时,伏立康唑对映体在C8及C18固定相上均能得到有效拆分。在上述条件下,以Hypersil C18色谱柱(4.6 mm×150 mm,5μm)分析伏立康唑对映体,流动相流速为1.0 mL.min-1,伏立康唑对映体能实现基线分离,伏立康唑浓度在31.2～156μg.mL-1范围内,浓度与峰面积呈良好线性关系(R2=0.9998),伏立康唑加样回收率大于98%,稳定性及重现性RSD分别为0.77%,0.67%。结论:建立了一种伏立康唑对映体的手性拆分和分析方法,可为伏立康唑的分离与分析提供借鉴。
Objective: To establish HPLC chiral separation and analysis of voriconazole enantiomers. Methods: β-CD and its derivatives as mobile phase chiral additives, to explore the type and concentration of β-CD derivatives, the mobile phase volume fraction of organic phase, column stationary phase of voriconazole enantiomer HPLC chiral removal On the basis of which, the HPLC analysis method of voriconazole enantiomer was established and the methodological study was conducted. Results: Among the β-CD derivatives, SBE-β-CD was suitable as HPLC chiral resolving agent for voriconazole enantiomers. The mobile phase was methanol-water (45:55), the concentration of potassium dihydrogen phosphate was 15 mmol·L -1 and the concentration of SBE-β-CD was 10.0 mmol.L-1, the voriconazole enantiomers could be resolved effectively on both C8 and C18 stationary phases. Under the above conditions, the enantiomers of voriconazole were analyzed on a Hypersil C18 column (4.6 mm × 150 mm, 5 μm) at a mobile phase flow rate of 1.0 mL · min-1. The voriconazole enantiomers were baseline separated and voriconazole concentrations ranged from 31.2 to 156 μg .mL-1, the concentration and peak area showed a good linear relationship (R2 = 0.9998), the recovery of voriconazole was greater than 98%, the stability and reproducibility RSD were 0.77% and 0.67%, respectively. CONCLUSION: A method for the chiral separation and analysis of voriconazole enantiomers was established, which can provide reference for the isolation and analysis of voriconazole.