色谱

色谱

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高效液相色谱-质谱法同时测定清热解毒口服液中的5种有效成分

许海棠1,黄丽涵1,徐远金1,2   

  1. 1.Center for Sugar Technology Research, Guangxi University, Nanning 530004, China; 2.Guangxi Key Laboratory of Subtropical Bioresource Conservation and Utilization, Nanning 530004, China
  • 收稿日期:2008-10-27 修回日期:2008-10-27 出版日期:2008-10-27 发布日期:1983-09-25
  • 通讯作者: 徐远金
  • 基金资助:
    广西壮族自治区科学研究基金项目(桂科能0718009-2E)

Simultaneous determination of five effective components in Qingrejiedu oral liquid using high performance liquid chromatography-mass spectrometry

XU Haitang1, HUANG Lihan1, XU Yuanjin1,2   

  1. 1.Center for Sugar Technology Research, Guangxi University, Nanning 530004, China; 2.Guangxi Key Laboratory of Subtropical Bioresource Conservation and Utilization, Nanning 530004, China
  • Received:2008-10-27 Revised:2008-10-27 Online:2008-10-27 Published:1983-09-25
  • Contact: XU Yuanjin

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摘要： 建立了同时测定清热解毒口服液中的绿原酸、栀子苷、黄芩苷、连翘苷和靛玉红5种有效成分的高效液相色谱-电喷雾电离质谱（HPLC-ESI/MS）分析方法。采用Zorbax SB C18色谱柱,以含0.2%甲酸的0.4 mmol/L醋酸钠(A相)、乙腈(B相)为流动相进行梯度洗脱,在ESI正离子模式下,采用选择离子监测方法进行测定,用峰面积进行定量。结果表明,绿原酸、栀子苷、黄芩苷、连翘苷和靛玉红的线性范围分别为0.050～50 mg/L,0.020～20 mg/L,0.005～30 mg/L,0.010～15 mg/L和0.010～10 mg/L;检出限分别为0.010，0.005，0.001，0.002和0.003 mg/L。5种成分的加样回收率为97.0%～101.7%,相对标准偏差小于2.2%。该法快捷、准确、重复性好,可用于清热解毒口服液中的5种有效成分含量的同时测定。

关键词: 靛玉红, 高效液相色谱-质谱法, 黄芩苷, 连翘苷, 绿原酸, 清热解毒口服液 , 栀子苷

Abstract: A high performance liquid chromatography-electrospray ionization mass spectrometry (HPLC-ESI/MS) method for the simultaneous determination of five effective components in Qingrejiedu oral liquid was developed. The HPLC separation was performed on a Zorbax SB C18 column (250 mm×3.0 mm, 5 μm) using 0.4 mmol/L sodium acetate solution containing 0.2% formic acid (A) and acetonitrile (B) as the mobile phase with gradient elution (0 min, 10% B; 06 min, 10%B30%B; 615 min, 30%B39%B; 1516 min, 39%B80%B) at a flow rate of 0.35 mL/min. The analytes were detected by ESI(+)-MS under selected ion monitoring mode (09.7 min, m/z 377; 9.712 min, m/z 411; 1214.7 min, m/z 447; 14.718 min, m/z 557; 1825 min, m/z 263). The linear ranges were 0.050-50 mg/L, 0.020-20 mg/L, 0.005-30 mg/L, 0.010-15 mg/L and 0.010-10 mg/L with detection limits of 0.010, 0.005, 0.001, 0.002 and 0.003 mg/L for chlorogenic acid, geniposide, baicalin, forsythin and indirubin, respectively. The average recoveries ranged from 97.0% to 101.7%. The relative standard deviations were less than 2.2%. This method is rapid, accurate, and suitable for the quality control of the five effective components in Qingrejiedu oral liquid.

Key words: baicalin, chlorogenic acid, forsythin, geniposide, indirubin, Qingrejiedu oral liquid , high performance liquid chromatography-mass spectrometry (HPLC-MS)