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机构地区:[1]广东医学院广东省天然药物重点实验室,湛江524023
出 处:《药物分析杂志》2010年第4期592-595,共4页Chinese Journal of Pharmaceutical Analysis
基 金:广东省建设中医药强省科研基金资助项目(No.2060044)
摘 要:目的:建立测定大鼠血清中高良姜素的HPLC内标法。方法:SD大鼠腹腔注射给药,血清样品用乙酸乙酯萃取,以大黄素为内标;采用Shim-pack C_(18)柱(2.1 mm×250 mm,5μm),以A相:0.1%乙酸-水,B相:乙腈-甲醇-四氢呋喃(15:40:45)为流动相,梯度洗脱[0 min时,A-B(61:39);20 min时,A-B(39:61);30 min时,A-B(0:100);45 min时,A-B(0:100)],流速0.2 mL·min^(-1);检测波长为345 nm,柱温35℃。结果:高良姜素的线性范围为0.34~26.0μg·mL^(-1)(r=0.9998),最低定量限为0.34μg·mL^(-1),方法回收率为90.6%~111.9%,绝对回收率大于85%,日内和日间的RSD均小于6.3%;血清样品的稳定性符合要求。结论:所建立的大鼠血清中高良姜素的HPLC测定方法灵敏、准确、精密、稳定,适用于大鼠体内高良姜的药代动力学研究。Objective:To develop an HPLC internal standard method for the determination of galangin in rat serum. Methods:The determination was performanced on Shim -pack C18 column(2.1 mm×250 mm,5μm)with the mobile phase consisting of 0.1%acetic acid - water(A) and acetonitrile - methanol - tetrahydrofuran(15:40:45;B) with gradient elution mode at a flow rate of 0.2 mL·min^-1.The following gradient procedure was used:0 - 20 min,39%→61%B;20 - 30 min,61%→100%B;30 -45 min,100%→100%B.Detection wavelength was 345 nm, the column temperature was 35℃.The route of administration of rats was ip,serum samples were extracted with ethyl acetate,methyl parahydroxybenzoate was used as an internal standard.Results:The linear range of galangin was 0.34 to 26.0μg·mL^-1(r = 0.9998 ) with the lower limit of quantification for 0.34μg·mL^-1.The method recovery was 90.6%to 111.9%and the absolute recovery was more than 85%.The intra - day RSD and inter - day RSD were less than 6.3%.Conclusion:The developed method for the quantification of galangin in rat serum is sensitive, accurate,precise,stable,and is suitable for the pharmacokinetic studies of galangal in rats.
关 键 词:高良姜素 高良姜 药代动力学 高效液相色谱 内标法
分 类 号:R917[医药卫生—药物分析学]
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