Chen Xuan, Bai Xiaohong, Wang Xiao, Wang Jing, Bu Wei
Department of Pharmacy, Shanxi Medical University, Taiyuan 030001, China.
Se Pu. 2010 Dec;28(12):1144-9.
The preferred conformations of the ephedrine and pseudoephedrine in Ephedra sinica Stapf and rat urine were analyzed by the hollow fiber liquid-phase microextraction (HF-LPME) and their extraction mechanisms were illuminated. The method of the separation of the ephedrine and pseudoephedrine and the determination of their concentrations with high performance liquid chromatography (HPLC) were established. The optimal experimental conditions were as follows: the organic phase carrier was the hollow fiber of polyvinylidene fluoride (MOF-503), organic solvent was n-hexanol, the extraction time was 35 min, the stirring rate was 1200 r/min, the sample phase was the NaOH solution (5 mol/L) of the analyte, the acceptor was 0.01 mol/L H2SO4 solution. The extracts were analyzed by HPLC. Under the optimal conditions, the method is convenient and highly sensitive. In Ephedra sinica Stapf, the linear ranges of ephedrine and pseudoephedrine were 5-100 microg/L, the detection limits were 1.9 microg/L and 1.2 microg/L and the enrichment factors were 38 and 61, respectively. The average recoveries of ephedrine and pseudoephedrine were 100.6% +/- 1.2% and 103.2% +/- 3.5%, respectively. In rat urine, their linear ranges were 100 - 5 x 10(4) microg/L, the detection limits were 30 microg/L and 42 microg/L and the enrichment factors were 20 and 17, respectively. In rat urine, their average recoveries were 108.4% +/- 4.4% and 106. 1% +/- 5.4%, respectively. The obtained results indicated that the method can be successfully applied for the extraction and determination of the ephedrine and pseudoephedrine in Ephedra sinica Stapf and rat urine.
采用中空纤维液相微萃取(HF-LPME)法分析了麻黄中麻黄碱和伪麻黄碱的优势构象及其在大鼠尿液中的构象,并阐明了其萃取机理。建立了采用高效液相色谱(HPLC)分离麻黄碱和伪麻黄碱并测定其含量的方法。最佳实验条件如下:有机相载体为聚偏氟乙烯中空纤维(MOF-503),有机溶剂为正己醇,萃取时间为35分钟,搅拌速率为1200转/分钟,样品相为分析物的氢氧化钠溶液(5摩尔/升),接受相为0.01摩尔/升硫酸溶液。萃取物采用HPLC分析。在最佳条件下,该方法简便且灵敏度高。在麻黄中,麻黄碱和伪麻黄碱的线性范围为5-100微克/升,检测限分别为1.9微克/升和1.2微克/升,富集因子分别为38和61。麻黄碱和伪麻黄碱的平均回收率分别为100.6%±1.2%和103.2%±3.5%。在大鼠尿液中,它们的线性范围为100-5×10⁴微克/升,检测限分别为30微克/升和42微克/升,富集因子分别为20和17。在大鼠尿液中,它们的平均回收率分别为108.4%±4.4%和106.1%±5.4%。所得结果表明,该方法可成功应用于麻黄和大鼠尿液中麻黄碱和伪麻黄碱的萃取和测定。