高效液相色谱法同时测定那格列奈中顺式异构体和<i>L</i>-异构体

高效液相色谱法同时测定那格列奈中顺式异构体和L-异构体

摘要: 称取样品25 mg，用正己烷-无水乙醇-三氟乙酸（80+20+0.1）混合溶液溶解并定容至25 mL，采用Chiralpak IG色谱柱（250 mm×4.6 mm，5 μm）分离待测物，以正己烷-无水乙醇-三氟乙酸（80+20+0.1）混合溶液为流动相，流量为0.8 mL·min^-1，采用二极管阵列检测器进行测定，检测波长为210 nm。那格列奈的顺式异构体和L-异构体的质量浓度分别在0.024~4.392，0.050~4.040 mg·L^-1内与其峰面积呈线性关系，检出限（3S/N）分别为0.008，0.015 mg·L^-1。加标回收率分别在94.1%~99.3%，100%~104%之间，测定值的相对标准偏差（n=6）小于5.0%。

Abstract: The sample (25 mg) was dissolved and the solution was diluted to 25 mL with a mixed solution of hexane-ethanol-trifluoroacetate (80+20+0.1). Chromatographic separation was achieved on a Chiralpak IG column (250 mm×4.6 mm, 5 μm), with a mixed solution of hexane-ethanol-trifluoroacetate (80+20+0.1) as mobile phase, at a fow rate of 0.8 mL·min^-1. Diode array detector was used for determination at wavelength of 210 nm. Linear relationships were found between peak areas and mass concentraions of cis-isomer and L-isomer in the ranges of 0.024-4.392, 0.050-4.040 mg·L^-1, respectively, with detecion limits (3S/N) of 0.008, 0.015 mg·L^-1 respectively. Values of recovery obtained by standard additon method were in the range of 94.1%-99.3%, 100%-104%, respectively, and RSDs (n=6) were less than 5.0%.