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HPLC analysis of oxindole alkaloids in Uncaria tomentosa: sample preparation and analysis optimisation by factorial design.

机译:绒毛钩藤中羟吲哚生物碱的HPLC分析:样品制备和因子设计优化分析。

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Introduction - Uncaria tomentosa ("cat's claw") is widely used for the treatment of some infectious and inflammatory diseases. Oxindole alkaloids are regarded as the most important components responsible for the biological activities attributed to the plant. Their analysis require efficient sample preparation and suitable reference standards but few are commercially available. Objective - To develop and validate a HPLC analytical method for oxindole alkaloids in Uncaria tomentosa with emphasis on sample preparation. Method - Factorial experimental designs were used for the optimisation of both sample preparation and chromatographic separation. The optimised sample preparation involved extraction with aqueous ethanol, and the granulometry of the powdered plant material significantly influenced extraction yields. Mitraphylline was used as a calibration reference for the determination of total alkaloids. Results - The method was fully validated and showed good selectivity, linearity (r2=96%) and precision (RSD <2.4%). Detection and quantification limits for mitraphylline were 0.8 and 2.4 ppm, respectively. Conclusion - The optimised chromatographic method, using organic buffer in the mobile phase, provided baseline separation of tetracyclic and pentacyclic alkaloids in the samples. Calibration using mitraphylline provided more accurate estimates of total alkaloid content when compared to other available reference alkaloids.Digital Object Identifier http://dx.doi.org/10.1002/pca.1335
机译:简介-猫毛(Uncaria tomentosa)(猫爪)被广泛用于治疗某些传染性和炎性疾病。羟吲哚生物碱被认为是归因于植物的生物活性的最重要成分。他们的分析需要有效的样品制备和合适的参考标准,但市售品很少。目的-建立并验证高效液相色谱分析方法,用于 Uncaria tomentosa 中的羟吲哚生物碱,重点是样品制备。方法-采用析因实验设计来优化样品制备和色谱分离。优化的样品前处理包括用乙醇水溶液萃取,粉状植物材料的粒度显着影响萃取产量。米曲茶碱用作测定总生物碱的校准参考。结果-该方法经过充分验证,并显示出良好的选择性,线性( r 2 = 96%)和精度(RSD <2.4%) 。米曲茶碱的检出限和定量限分别为0.8和2.4 ppm。结论-在流动相中使用有机缓冲液的优化色谱方法提供了样品中四环和五环生物碱的基线分离。与其他可用的参考生物碱相比,使用米茶碱进行校准可提供更准确的总生物碱含量估算。数字对象标识符http://dx.doi.org/10.1002/pca.1335

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