离子液体[BMIM]BF_4对甘草酸及其衍生物色谱行为的影响

Effect of Ionic Liquid [BMIM]BF_4 on Chromatographic Behavior of Glycyrrhizin and Its Derivatives

将离子液体1-丁基-3-甲基咪唑四氟硼酸盐（[BMIM]BF。）加入到高效液相色谱流动相中，研究其对甘草酸（GL）及其衍生物甘草次酸（GA）和单葡萄糖醛酸基甘草次酸（GAMG）色谱行为的影响。结果显示，加入离子液体后的流动相能够明显改善色谱峰形、减少峰拖尾、增大峰面积和峰高、提高检测灵敏度，并缩短GL，GA及GAMG3种化合物的同时检测时间，提高检测效率。优化色谱条件为：InertSustain C18（4．6mm×250mmi．d．，5μm）反相色谱柱为分离柱，柱温40℃；甲醇-1．0mmol／L[BMIM]BF4（体积比81：19，乙酸调至pH3．0）为流动相，流速0．7mL／min，进样体积20μL，检测波长251nm。GL，GA及GAMG在5．00—100mg／L范围内线性关系良好（r≥0．9998），检出限分别为0．02，0．04，0．09mg／L；加标回收率分别为100．1％，98．0％，98．2％，RSD为0．18％～0．43％。同时测定GL生物转化体系中3种组分，结果满意。

Effect of 1-butyl-3-methylimidazolium tetrafluoroborate （ [ BMIM ] BF4 ） on the chromato- graphic behavior of glycyrrhizin（GL） and its derivatives was studied by adding ionic liquids in mobible phase of reverse phase high performance liquid chromatography （HPLC）. The result showed that the addition of ILs had a superior effect on the determination of GL, glycyrrhetinic acid （GA） and glycyrrhetinic acid monoglucuronide （GAMG） by improving chromatographic peak shape, reducing tailing, increasing peak area and peak height, and enhancing detection sensitivity. In addition, the simultaneous detection time of three substances was greatly shortened, and the detection efficiency was obviously improved. The optimum chromatographic conditions were as follows： separation col- umn： InertSustain Cls （4. 6 mm - 250 mm i. d. , 5 μm） ; column temprerature： 40 ℃ ; mobile phase： methanol -1.0 mmol/L [ BMIM] BF4 aqueous solution（81 ： 19, adjusted pH 3.0 with acetic acid）; flow rate： 0.7 mL/min; injection volume： 20 IxL; detection wavelength： 251 nm. The calibration curves showed good linearities over the concentration range of 5.00 - 100 mg/L for three compounds with correlation coefficients not less than 0. 999 8. The detection limits （S/N = 3 ） of GL, GA and GAMG were 0. 02, 0. 04 and 0. 09 mg/L, with spiked recoveries of 100. 1% , 98.0~/6 and 98.2%, respectively. The relative standard deviations （RSD） were in the range of 0. 18% - 0. 43%. The method was used to determine the above three components in GL bioconversion system with satisfactory result.