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熱感賽比斯坦顆粒定性定量方法研究

發(fā)布時間:2019-08-01 15:44
【摘要】:目的:建立熱感賽比斯坦顆粒定性定量方法。方法:采用薄層色譜法對熱感賽比斯坦顆粒中罌粟殼、罌粟子、甘草、破布木果、蜀葵子、黃瓜子、i卙r子和巴旦仁進(jìn)行定性鑒別;采用高效液相色譜法測定熱感賽比斯坦顆粒中甘草苷、甘草酸銨和嗎啡的含量。甘草苷和甘草酸銨含量測定色譜條件:采用Agilent TC C18(250 mm×4.6 mm,5μm)色譜柱,以乙腈(A)-0.1%磷酸溶液(B)為流動相,梯度洗脫(0~10 min,19%A;10~15 min,19%A→25%A;15~30 min,25%A→38%A;30~42 min,38%A;42~50 min,38%A→19%A),流速1 m L·min-1,檢測波長237 nm,柱溫為30℃;嗎啡含量測定色譜條件:采用Phenomenex Luna C8(250 mm×4.6 mm,5μm)色譜柱,以乙腈-0.5%醋酸銨水溶液(含三乙胺0.8%)(13∶87)為流動相,流速1.0 m L·min-1,檢測波長286 nm,柱溫30℃。結(jié)果:TLC斑點(diǎn)清晰,分離度好,陰性無干擾。甘草苷、甘草酸銨和嗎啡質(zhì)量濃度分別在3.68~73.64、18.62~260.68和5.33~85.28μg·m L-1范圍內(nèi),與峰面積線性關(guān)系良好,r分別為0.999 8、0.999 9和0.999 8);平均回收率(n=6)分別為102.9%、102.2%和99.71%,RSD分別為0.98%、1.4%和1.7%。結(jié)論:所建方法可用于熱感賽比斯坦顆粒的質(zhì)量控制。
[Abstract]:Objective: to establish a qualitative and quantitative method for thermal sensitivity Sebstein granules. Methods: the opium poppy shell, poppy seed, Glycyrrhiza uralensis Fisch, rag wooden fruit, solium mandshurica, cucumber seed, I rzi and Padan kernel were identified qualitatively by thin layer chromatography, and the contents of glycyrrhizin, ammonium glycyrrhizinate and morphine in heat sensitive Sebistein granules were determined by high performance liquid chromatography (HPLC), and the contents of glycyrrhizin, ammonium glycyrrhizinate and morphine in heat sensitive Sebistein granules were determined by high performance liquid chromatography (HPLC). The chromatographic conditions for the determination of glycyrrhizin and ammonium glycyrrhizinate were as follows: Agilent TC C18 (250 mm 脳 4.6 mm, 5 渭 m) column, (B) as mobile phase with (A)-0.1% phosphate solution, gradient eluting (0 鈮,

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