中藥製劑中摻加類固醇之固相萃取與高效液相層析研究   全文下載

Solid-phase Extraction and High Performance Liquid Chromatographic Determination of Steroids Adulterated in Traditional Chinese Medicines

本研究以矽膠固相萃取法萃取摻加於中藥製劑中之八種類固醇betamethasone、cortisoneacetate、dexamethasone、hydrocortisoneacetate、methylprednisolone、prednisolone, prednisone及triamcinolone，再以高效液相層析法作定量分析比較，評估個別之回收率。本實驗採用逆相層析管柱，沖提液為乙?與水（3:7），檢測波長為240 nm，內部標準品為fludrocortisone acetate作分析。八種類固醇檢量線之相關係數（r）為0.9983至0.9996，均呈現良好線性關係。八種類固醇之同日問及異日間試驗之相對標準差，分別為0.7-4.的及1.0-4.4%，顯示再現性佳。固相萃取條件之探討包括萃取溶媒之組成、中藥製劑萃取液之濃度及不同廠牌之固相萃取管等，均加以比較以建立最佳之萃取條件。"

A systematic evaluation and comparison of the recoveries of eight steroids from spiked traditional Chinese medicine (TCM) extract using silica gel solid-phase extraction (SPE) are reported. The eight steroids, betamethasone, cortisone acetate, dexamethasone, hydrocortisone acetate, methylprednisolone, prednisolone, prednisone and triamcinolone, adulterated in TCM were assayed simultaneously by high performance liquid chromatography on a reverse phase column. This chromatographic method was carried out using isocratic elution with acetonitrile and water (3:7). Fludrocortisone acetate was used as an internal standard and detection was at 240 nm. Calibration curves of the eight adulterants were constructed in the range 6-96µg/mL. Their correlation coefficients ranged from 0.9983 to 0.9996. The relative standard deviations of the eight steroids for intraday and interday analyses were 0.7-4.1% and 1.0- 4.4%, respectively. Optimized experimental conditions including solvent composition, TCM extract concentration and different brands of SPE cartridge were also investigated. 本研究以矽膠固相萃取法萃取摻加於中藥製劑中之八種類固醇betamethasone、cortisoneacetate、dexamethasone、hydrocortisoneacetate、methylprednisolone、prednisolone, prednisone及triamcinolone，再以高效液相層析法作定量分析比較，評估個別之回收率。本實驗採用逆相層析管柱，沖提液為乙腈與水（3:7），檢測波長為240 nm，內部標準品為fludrocortisone acetate作分析。八種類固醇檢量線之相關係數（r）為0.9983至0.9996，均呈現良好線性關係。八種類固醇之同日問及異日間試驗之相對標準差，分別為0.7-4.的及1.0-4.4%，顯示再現性佳。固相萃取條件之探討包括萃取溶媒之組成、中藥製劑萃取液之濃度及不同廠牌之固相萃取管等，均加以比較以建立最佳之萃取條件。