摘要
采用Chiralpak AD-H(4.6μm×250 mm,5μm)手性色谱柱,建立了氟苯尼考对映体的正相高效液相色谱拆分方法。考察了流动相中碱性添加剂、醇类改性剂种类及浓度对分离度、保留时间、理论塔板数、拖尾因子的影响。结果表明:以正己烷-异丙醇-甲醇(70∶15∶15)为流动相,流速为1 mL/min,柱温为30℃,检测波长为224 nm条件下,氟苯尼考与其光学异构体获得满意的分离效果。氟苯尼考在0.05~0.5g/L质量浓度范围内与其峰面积呈良好的线性关系,相关系数r为0.999 7;氟苯尼考的检出限为0.1μg/L;日内精密度RSD小于1.8%,日间精密度RSD小于2.3%;加标回收率为109%~112%,RSD不大于3.0%。该方法快速、方便,可用于工业生产中氟苯尼考光学纯度的控制。
A high performance liquid chromatographic (HPLC) method for the separation of florfeni- col enantiomers using a Chiralpak AD - H (4. 6 μm ×250 mm, 5 μm) was established. The influ- ences of the base additive, the kinds and concentrations of alcohol additives on the chiral separation of florfenicol including resolution, retention time, theoretical plate and tailing factor were investiga- ted. The results indicated that florfenicol was separated well from its optical isomer with n-hexane : isopropyl alcohol : methanol(70 : 15 : 15) as mobile phase at a flow rate of 1 mL . min-1 and a col- umn temperature of 30 ℃. The UV detection wavelength was set at 224 nm. The calibration curve for florfenicol was linear in the concentration range of 0. 05 - 0. 5 g . L- 1 with correlation coefficient of 0. 999 7. The limit of detection (LOD) was 0. 1 μg , L- 1. The intra-day relative standard deviations (RSD) were less than 1.8% and the inter-day RSDs were less than 2. 3%. The average spiked re- coveries were in the range of 109% - 112% with RSDs not more than 3.0%. The method was relia- ble and simple, and was suitable for the lality control of florfenicol in industrial production.
出处
《分析测试学报》
CAS
CSCD
北大核心
2013年第4期459-462,467,共5页
Journal of Instrumental Analysis
基金
国家高技术研究发展计划(863计划)(2011AA10A214)
关键词
氟苯尼考对映体
高效液相色谱
手性拆分
光学纯度
florfenicol enantiomers
high performance liquid chromatography(HPLC)
chiral sepa-ration
optical purity