Department Pharmaceutical Analysis, Institution Shenyang Pharmaceutical University, Shenyang, P. R. China.
Chirality. 2019 Nov;31(11):968-978. doi: 10.1002/chir.23125. Epub 2019 Aug 22.
The present work firstly described the enantioseparation and determination of flumequine enantiomers in milk, yogurt, chicken, beef, egg, and honey samples by chiral liquid chromatography-tandem mass spectrometry. The enantioseparation was performed under reversed-phase conditions on a Chiralpak IC column at 20°C. The effects of chiral stationary phase, mobile phase components, and column temperature on the separation of flumequine enantiomers have been studied in detail. Target compounds were extracted from six different matrices with individual extraction procedure followed by cleanup using Cleanert C18 solid phase extraction cartridge. Good linearity (R >0.9913) was obtained over the concentration range of 0.125 to 12.5 ng g for each enantiomer in matrix-matched standard calibration curves. The limits of detection and limits of quantification of two flumequine enantiomers were 0.015-0.024 and 0.045-0.063 ng g , respectively. The average recoveries of the targeted compounds varied from 82.3 to 110.5%, with relative standard deviation less than 11.7%. The method was successfully applied to the determination of flumequine enantiomers in multiple food matrices, providing a reliable method for evaluating the potential risk in animal productions.
本工作首次描述了手性液相色谱-串联质谱法在手性拆分和测定牛奶、酸奶、鸡肉、牛肉、鸡蛋和蜂蜜样品中的氟甲喹对映异构体中的应用。在反相条件下，于 20°C 下在 Chiralpak IC 柱上进行对映异构体分离。详细研究了手性固定相、流动相组成和柱温对氟甲喹对映异构体分离的影响。目标化合物通过单独的提取程序从六种不同的基质中提取，然后使用 Cleanert C18 固相萃取小柱进行净化。在基质匹配标准校准曲线中，每个对映异构体的浓度范围为 0.125 至 12.5ng/g 时，均获得了良好的线性（R>0.9913）。两种氟甲喹对映异构体的检测限和定量限分别为 0.015-0.024 和 0.045-0.063ng/g。目标化合物的平均回收率在 82.3%至 110.5%之间，相对标准偏差小于 11.7%。该方法成功应用于多种食品基质中氟甲喹对映异构体的测定，为评估动物生产中的潜在风险提供了可靠的方法。
