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  

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

作　　者：许海棠[1] 黄丽涵[1] 徐远金[1] 

机构地区：[1]广西大学糖业工程技术研究中心

出　　处：《色谱》2008年第5期599-602,共4页Chinese Journal of Chromatography

基　　金：广西壮族自治区科学研究基金项目(桂科能0718009-2E)

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ZorbaxSBC18色谱柱,以含0.2%甲酸的0.4mmol/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0.050～50mg/L,0.020～20mg/L,0.005～30mg/L,0.010～15mg/L和0.010～10mg/L;检出限分别为0.010,0.005,0.001,0.002和0.003mg/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。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 41,12→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.

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

分 类 号：O658[理学—分析化学]