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建立了胶束毛细管电动色谱在线富集技术测定药品中痕量的泼尼松的方法。在胶束扫集的基础上联用场放大进样,使泼尼松的富集倍数提高了136倍;检出限由原来的2.7mg/L降至20μg/L。胶束扫集毛细管电泳缓冲体系为120mmol/LSDS、10mmol/LNaH2PO4(pH2.5)10%乙腈(V/V)。分离电压-20kV,进样电压-20kV,进样时间70s,进水时间180s,检测波长250nm。同时讨论了SDS浓度、样品基质pH、进样电压、进水时间和进样时间对分离效果的影响。实验结果显示:在优化实验条件下,样品的检测仅需8min,泼尼松在0.05～10mg/L的范围内线性关系良好(r=0.998)。回收率在89.4%～106%之间,相对标准偏差在2.1%～2.6%之间,可用于各种中药制剂中泼尼松的含量测定。
A method of micellar capillary electrokinetic chromatography on-line enrichment for the determination of trace amounts of prednisone in pharmaceuticals was established. On the basis of micellar scanning, the field amplification was used to increase the prednisone enrichment multiple by 136-fold. The detection limit was reduced from 2.7mg / L to 20μg / L. Micellar sweep capillary electrophoresis buffer system was 120mmol / LSDS, 10mmol / L NaH2PO4 (pH2.5) 10% acetonitrile (V / V). Separation voltage -20kV, injection voltage -20kV, injection time 70s, water inlet time 180s, detection wavelength 250nm. The effects of SDS concentration, sample matrix pH, injection voltage, water inlet time and injection time on the separation efficiency were also discussed. The experimental results show that under the optimal experimental conditions, the sample is only detected for 8 min. Prednisone has a good linear relationship (r = 0.998) in the range of 0.05 ~ 10 mg / L. The recoveries ranged from 89.4% to 106% and the relative standard deviations ranged from 2.1% to 2.6%, which could be used for the determination of prednisone in various traditional Chinese medicine preparations.