HPLC法检测氟雷拉纳对映异构体的比例

Ratio of enantiomer in fluralaner by HPLC

目的:建立氟雷拉纳对映异构体比例的高效液相色谱测定方法。方法:采用CHIRALPAK AD-H手性色谱柱(250 mm×4.6 mm,5μm);以正己烷-无水乙醇(60∶40)为流动相,流速1.0 mL·min^(-1),检测波长265 nm,柱温室温,进样量20μL。结果:在本文色谱条件下,测定的3批样品,R-氟雷拉纳与S-氟雷拉纳峰面积的比例均为1∶1,R-氟雷拉纳与S-氟雷拉纳质量浓度分别在80.288~187.338μg·mL^(-1)(r=0.9997)和81.902~191.104μg·mL^(-1)(r=0.9999)范围内与峰面积呈良好的线性关系,平均回收率分别为100.6%和100.8%。结论:本方法准确度高,重复性好,可用于氟雷拉纳外消旋体中对映异构体的比例测定方法。

Objective:To establish an HPLC method for the ratio of the enantiomer in fluralaner.Methods:The chromatographic separation was performed on chiral chromatography column CHIRALPAK AD-H(250 mm×4.6 mm,5μm).The mobile phase consisted of n-hexane-anhydrous ethanol(60∶40)and the flow rate was 1.0 mL·min^(-1).The detection wavelength was 265 nm and the column temperature was room temperature.Results:Under this chromatographic condition,three batches of samples were determined,the proportions of R-fluralaner and S-fluralaner were 1∶1.The calibration curves of R-fluralaner and S-fluralaner good linearities at the range of 80.288-187.338μg·mL^(-1)(r=0.9997)and 81.902-191.104μg·mL^(-1)(r=0.9999),respectively.The average recoveries were 100.6%and 100.8%.Conclusion:The method is accurate,reproducible and can be used for the ratio of enantiomers in fluralaner racemate.