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高效液相色谱手性流动相添加剂法测定富马酸(RR)-戊乙奎醚中3个光学异构体杂质的含量
引用本文:周逸芝,刘训红,许虎,傅兴圣,陈菲,张奉苏.高效液相色谱手性流动相添加剂法测定富马酸(RR)-戊乙奎醚中3个光学异构体杂质的含量[J].中国药学杂志,2013,48(2):139-142.
作者姓名:周逸芝  刘训红  许虎  傅兴圣  陈菲  张奉苏
作者单位:南京中医药大学
基金项目:江苏省科技厅“科技基础实施建设计划”专项(BM2009903);江苏高校优势学科建设工程资助项目(ysxk-2010)
摘    要: 目的 建立拆分富马酸(RR)-戊乙奎醚与其3个光学异构体的高效液相色谱分离方法,控制光学纯度。方法 选用C18(4.6 mm×250 mm,5 μm)色谱柱,以乙腈-0.05 mol·L-1磷酸二氢钾(含0.6%三乙胺和0.015 mol·L-1β-环糊精,pH为2.3)为流动相,柱温25 ℃,检测波长206 nm,流速1.0 mL·min-1。结果 3个光学异构体的检测灵敏度为9.0 ng,本方法可检出限量为0.09%的光学异构体杂质。结论 本法可有效分离富马酸(RR)-戊乙奎醚及其3个光学异构体,可用于控制本品光学纯度。

关 键 词:富马酸(R  R)-戊乙奎醚  光学异构体  高效液相色谱法  手性拆分
收稿时间:2012-06-13;

Simultaneous Determination of Five Index Components in Glycyrrhizae Radix et Rhizoma and Longchai Decoction by HPLC
ZHOU Yi-zhi,LIU Xun-hong,XU Hu,FU Xing-sheng,CHEN Fei,ZHANG Feng-su.Simultaneous Determination of Five Index Components in Glycyrrhizae Radix et Rhizoma and Longchai Decoction by HPLC[J].Chinese Pharmaceutical Journal,2013,48(2):139-142.
Authors:ZHOU Yi-zhi  LIU Xun-hong  XU Hu  FU Xing-sheng  CHEN Fei  ZHANG Feng-su
Institution:(Nanjing University of Chinese Medicine,Nangjing 210046,China)
Abstract:OBJECTIVE To establish a determination method of five index components to control the quality of Glycyrrhizae Radix et Rhizoma and Longchai Decoction. METHODS An ODS C18 column (4.6 mm×250 mm, 5 μm) was adopted; the mobile phase consisted of acetonitrile-0.05% phosphoric acid with gradient elution at the flow rate of 1 mL·min-1;the detection wavelength was 237 nm,and the column temperature was 30 ℃.RESULTS The five index components achieved baseline separation, and the negative sample showed no interference. The linear ranges were 0.156 8-1.568 μg for liquiritin (r=0.999 7), 0.157 1-1.571 μg for isoliquiritin (r=0.999 8), 0.155 8-1.558 μg for liquiritigenin (r=0.999 6), 0.187 1-1.871 μg for glycyrrhizic(r=0.996 9) and 0.158 1-1.58 1 μg for isoliquiritigenin (r=0.999 5), respectively. The average recoveries were 101.47%(RSD=1.272%), 101.09%(RSD=1.937%), 101.14%(RSD=2.388%), 100.38%(RSD=1.448%)and 100.86%(RSD=1.759%), respectively (n=5). CONCLUSION This method has good resolution and high precision, and can be used for the quality control of Glycyrrhizae Radix et Rhizoma and Longchai decoction.
Keywords:Longchai decoction  Glycyrrhizae Radix et Rhizoma  liquiritin  isoliquiritin  liquiritigenin  glycyrrhizic  isoliquiritigenin
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