【摘要】 建立了液相微萃取/后萃取-高效液相色谱法测定中药苦参、复方苦参注射液中氧化苦参碱和苦参碱含量的方法。利用自制的微萃取装置,选择异丙醇为萃取有机溶剂,2.00 mL NaOH(pH9)为供相,HCl(pH4)为接受相,聚丙烯腈纤维的长度为10 cm,搅拌速度为1500 r/min,萃取时间为30 min。萃取完成后,经高效液相色谱仪分析,测得氧化苦参碱和苦参碱线性范围分别为11~437 mg/L和10~433 mg/L;检出限均为1.0mg/L;相对标准偏差分别小于9.4%和6.7%。复方苦参注射液中氧化苦参碱和苦参碱的平均回收率分别为83.0%~116.1%和108.8%~117.8%;苦参药材中氧化苦参碱的平均回收率为104.3%~114.7%。本方法有机溶剂用量少,可有效去除复杂机体的干扰,测得结果满意。更多还原

【Abstract】 Liquid phase microextraction with back extraction(LPME/BE) based on porous hollow fibres coupled with high performance liquid chromatography was developed for the determination of oxymatrine and matrine in Sophora flavescens Ait.and injection preparation.The optimal experimental conditions,the polyacrylonitrile fiber was cut into 10 cm pieces,ispropyl alcohol as organic solvent,2.00 mL pH 9 NaOH as the donor phase,pH 4 HCl as the acceptor phase,1500 r/min of the stirring rate and 30 min of the extraction time,were selected.Under the optimal conditions,high extract efficiency was obtained.The linear ranges of oxymatrine and matrine were from 11 to 437 mg/L and from 10 to 433 mg/L respectively with the correlation coefficient(r) better than 0.999.The relative standard deviation was lower than 9.4% and 6.7%,respectively.The average relative recoveries of oxymatrine and matrine in injection preparation were 83.0%-116.1% and 108.8%-117.8%,respectively.The average relative recovery of oxymatrine in Sophora flavescens Ait.was 104.3%-114.7%.The limit of detection was 1.0 mg/L for oxymatrine,1.0 mg/L for matrine.This method was applied to eliminate the interference of matrices,improved the selectivities.It shows the possibility for the simultaneous determination of oxymatrine and matrine in Sophora flavescens Ait.and injection preparation.更多还原