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采用自制的苯氨基甲酸酯衍生化β-环糊精键合SBA-15手性固定相,以甲醇-水作流动相,拆分了柚皮甙对映体;考察了流动相组成、柱温、检测波长等对柚皮甙拆分和测定的影响,优化的色谱条件为:流动相为甲醇-水(55:45,V/V),流速0.5 m L/min,柱温20℃,进样量10μL,检测波长为285 nm。基于上述条件,对中草药化橘红、香橼、枳壳及柚皮中的柚皮甙对映体进行了含量测定。柚皮甙每个对映异构体均在0.5~500μg/m L范围内线性关系良好(r≥0.995),检出限为0.04μg/m L(S/N=3)。以化橘红为例,柚皮甙第一个对映体的加标平均回收率为93.8%和RSD为1.2%(n=5),第二个对映体的加标平均回收率为91.3%和RSD为1.6%(n=5)。测得化橘红、香橼、枳壳和柚皮中柚皮甙两对映体的含量分别为10.42 mg/g和15.84 mg/g,15.39 mg/g和49.52 mg/g,16.53 mg/g和95.80 mg/g,18.47 mg/g和30.98 mg/g。
The enantiomers of naringin were resolved by self-made phenylcarbamate-derivatized β-cyclodextrin bonded SBA-15 chiral stationary phase and methanol-water as mobile phase. The mobile phase composition, column Temperature and detection wavelength on the separation and determination of naringin. The optimized chromatographic conditions were methanol-water (55:45, V / V), flow rate 0.5 m L / min, Injection volume 10μL, detection wavelength of 285 nm. Based on the above conditions, the enantiomers of naringin in Chinese herbal medicine orange, citron, Citrus aurantium and pomelo peel were determined. Each enantiomer of naringin had a good linearity (r ≥0.995) in the range of 0.5-500 μg / mL with a detection limit of 0.04 μg / mL (S / N = 3). Taking the orange juice as an example, the average recoveries of the first enantiomer of naringin were 93.8% and the RSD was 1.2% (n = 5). The average recoveries of the second enantiomer were 91.3% And RSD was 1.6% (n = 5). The two enantiomers were found to be 10.42 mg / g and 15.84 mg / g, 15.39 mg / g and 49.52 mg / g, 16.53 mg / g in Citrus, Citron, Citrus aurantium and pomelo peel respectively 95.80 mg / g, 18.47 mg / g and 30.98 mg / g.