一种用于测定和控制龙骨葵属片剂中美鼠李碱含量的毛细管区带电泳方法。
A capillary zone electrophoresis method for the assay and quality control of mesembrine in Sceletium tablets.
作者信息
Patnala Srinivas, Kanfer Isadore
机构信息
Division of Pharmaceutics, Faculty of Pharmacy, Rhodes University, Grahamstown, South Africa.
出版信息
J Pharm Biomed Anal. 2008 Sep 29;48(2):440-6. doi: 10.1016/j.jpba.2008.01.002. Epub 2008 Jan 9.
The Sceletium plant has been reported to contain psychoactive alkaloids, specifically mesembrine, mesembrenone, mesembrenol and other related alkaloids. Sceletium is marketed through health shops and on the internet as dried plant powder and as pharmaceutical dosage forms. The objectives of this research was to develop and validate a capillary zone electrophoresis (CZE) method to identify five alkaloids and quantitatively determine the content of the important alkaloid, mesembrine in Sceletium tablets. Since reference standards of the relevant alkaloids are not commercially available for use in quality control of Sceletium products, it was necessary to isolate and characterize an appropriate analytical marker for use in the assay and additional markers for fingerprinting by CZE. The separation of the relevant alkaloids was carried out by CZE on a 50cm effective length, fused silica capillary tubing (50microm i.d.x360microm o.d.) using 50mM of sodium dihydrogen orthophosphate dihydrate at pH 1.5 as the background electrolyte and monitored at a UV wavelength of 228nm. All the marker alkaloids were found to be well resolved and were identified in the plant material and in commercially available Sceletium tablets based on the relative migration times (MTs) with respect to quinine hydrochloride that was used as an internal standard. The method was validated and used to assay the mesembrine content in Sceletium tablets. Calibration curves were found to be linear over the entire concentration range of 2.5-80microg/ml with correlation coefficients >0.995. The accuracy was found to be 92.5 and 104.5% (R.S.D.<3.5%) and the R.S.D.'s of the inter-day precision at low, medium and high tablet masses were better than 0.9, 2.2 and 2.7%, respectively. The recoveries were all within the range of 91.8 and 105.8% (R.S.D.<8.5%) and the limit of quantitation (LOQ) and limit of detection (LOD) values were found to be 2.5 and 1.5microg/ml, respectively.
据报道，南非钩枝藤属植物含有精神活性生物碱，特别是美山胺、美山酮、美山醇及其他相关生物碱。南非钩枝藤属植物以干燥植物粉末和药物剂型的形式在保健品商店和互联网上销售。本研究的目的是开发并验证一种毛细管区带电泳（CZE）方法，用于鉴定五种生物碱，并定量测定南非钩枝藤属植物片剂中重要生物碱美山胺的含量。由于相关生物碱的参考标准品在商业上无法获得，无法用于南非钩枝藤属植物产品的质量控制，因此有必要分离并鉴定一种合适的分析标记物用于该测定，并鉴定其他用于CZE指纹图谱分析的标记物。相关生物碱的分离在一根有效长度为50cm的熔融石英毛细管柱（内径50μm×外径360μm）上进行，以50mM二水合磷酸二氢钠在pH 1.5作为背景电解质，并在228nm的紫外波长下进行监测。所有标记生物碱均得到良好分离，并根据相对于用作内标的盐酸奎宁的相对迁移时间（MTs），在植物材料和市售南非钩枝藤属植物片剂中得到鉴定。该方法经过验证后用于测定南非钩枝藤属植物片剂中美山胺的含量。校准曲线在2.5 - 80μg/ml的整个浓度范围内呈线性，相关系数>0.995。准确度分别为92.5%和104.5%（相对标准偏差<3.5%），低、中、高片剂质量下日间精密度的相对标准偏差分别优于0.9%、2.2%和2.7%。回收率均在91.8%至105.8%范围内（相对标准偏差<8.5%），定量限（LOQ）和检测限（LOD）值分别为2.5μg/ml和1.5μg/ml。
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