Andrisano V, Bonazzi D, Cavrini V
J Pharm Biomed Anal. 1995 Apr;13(4-5):597-605. doi: 10.1016/0731-7085(95)01300-a.
A reversed-phase HPLC method is proposed for the separation of five liquorice triterpenoids, 18 beta glycyrrhetic acid (beta GA), 18 alpha glycyrrhetic acid (alpha GA), 24-hydroxy-18 beta-glycyrrhetic acid (24-OH-beta GA), alpha and beta liquiritic acid (alpha and beta LA), with potentially different biological activities. The method has been developed by studying the influence of the type of stationary phase, pH, amine modifier and organic modifier on the resolution of the five compounds. The optimized chromatographic conditions were then successfully applied to the analysis of alpha- and beta-GA in pharmaceutical preparations (toothpaste and creams) on a reversed-phase Phenomenex Ultracarb 5 ODS (30) column (150 x 4.6 mm i.d.), using as the mobile phase acetonitrile-THF-0.010 M dioctylammonium phosphate buffer (pH 6.5) (25:20:55, v/v/v) at a flow-rate of 0.8 ml min-1. SPE methods with diolic and C18 sorbents were developed to isolate and concentrate the analytes and to enhance the sensitivity for the determination of alpha-GA as an impurity in the beta-GA preparations. The method was found to be reliable and suitable for the quality control of beta-GA preparations.
本文提出了一种反相高效液相色谱法，用于分离五种具有潜在不同生物活性的甘草三萜类化合物，即18β-甘草次酸（βGA）、18α-甘草次酸（αGA）、24-羟基-18β-甘草次酸（24-OH-βGA）、α和β甘草酸（α和βLA）。通过研究固定相类型、pH值、胺改性剂和有机改性剂对这五种化合物分离度的影响，开发了该方法。然后，将优化后的色谱条件成功应用于在反相Phenomenex Ultracarb 5 ODS(30)柱(150×4.6 mm内径)上对药物制剂(牙膏和乳膏)中α-和β-GA的分析，流动相为乙腈-四氢呋喃-0.010 M磷酸二辛铵缓冲液(pH 6.5)(25:20:55，v/v/v)，流速为0.8 ml min-1。开发了使用二醇型和C18吸附剂的固相萃取方法，用于分离和富集分析物，并提高对β-GA制剂中作为杂质的α-GA测定的灵敏度。该方法被认为可靠且适用于β-GA制剂的质量控制。
