Determination of tropane alkaloids by heart cutting reversed phase - Strong cation exchange two dimensional liquid chromatography
Autor: | Lvye Liu, Xiaoda Liu, Yan Jin, Zhimou Guo, Frank Steiner, Nana Du, Zhen Long, Xingguo Liu, Yan-Hai Zhang, Paul H. Gamache |
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Rok vydání: | 2017 |
Předmět: |
Resolution (mass spectrometry)
Clinical Biochemistry Analytical chemistry 02 engineering and technology Scopolia 01 natural sciences Biochemistry Analytical Chemistry Matrix (chemical analysis) chemistry.chemical_compound Alkaloids Limit of Detection Cations medicine Sample preparation Hyoscyamine Detection limit Chromatography Reverse-Phase Chromatography Chemistry Plant Extracts 010401 analytical chemistry Reproducibility of Results Tropane Cell Biology General Medicine Reversed-phase chromatography 021001 nanoscience & nanotechnology Chromatography Ion Exchange 0104 chemical sciences Linear Models 0210 nano-technology Tropane alkaloid medicine.drug Tropanes |
Zdroj: | Journal of chromatography. B, Analytical technologies in the biomedical and life sciences. 1072 |
ISSN: | 1873-376X |
Popis: | Current Chinese Pharmacopoeia (ChP) standards apply liquid extraction combined with one dimensional liquid chromatography (1DLC) method for determining alkaloids in herbal medicines. The complex pretreatments lead to a low analytical efficiency and possible component loss. In this study, a heart cutting reversed phase - strong cation exchange two dimensional liquid chromatography (RP - SCX 2DLC) approach was optimized for simultaneously quantifying tropane alkaloids (anisodine, scopolamine and hyoscyamine) in herbal medicines and herbal medicine tablets without further treatment of the filtered extract. The chromatographic conditions were systematically optimized in terms of column type, mobile phase composition and flow rate. To improve peak capacity and obtain symmetric peak shape of alkaloids, a polar group embedded C18 column combined with chaotropic salts was used in the first dimension. To remove the disturbance of non-alkaloids, achieve unique selectivity and acquire symmetric peak shape of alkaloids, an SCX column combined with phosphate buffer was used in the second dimension. Method validation was performed in terms of linearity, precision (0.54-0.82%), recovery (94.1-105.2%), limit of detection (LOD) and limit of quantification (LOQ) of the three analytes varied between 0.067-0.115mgL-1 and 0.195-0.268mgL-1, respectively. The method demonstrated superiority over 1DLC method in respect of resolution (less alkaloid co-eluted), sample preparation (no pretreatment procedure) and transfer rate (minimum component loss). The optimized RP - SCX 2DLC approach was subsequently applied to quantify target alkaloids in five herbal medicines and herbal medicine tablets from three different manufactures. The results demonstrated that the developed heart cutting RP - SCX 2DLC approach represented a new, strategically significant methodology for the quality evaluation of tropane alkaloid in related herbal medicines that involve complex chemical matrix. |
Databáze: | OpenAIRE |
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