LC_MS_MS法同时测定不同产地半枝莲中野黄芩苷和芹菜素含量

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1、药物分析杂志ChinJPharmAnal2009,29(9)1451LC-MS/MS法同时测定不同产地半枝莲中野黄芩苷和芹菜素含量*焦燕,王英锋,刘锁兰(首都师范大学分析测试中心,北京100048)摘要目的:采用液相色谱-二级质谱联用法(LC-MS/MS)对不同产地半枝莲药材中的野黄芩苷和芹菜素进行含量测定。-1方法:采用DiscoveryC18柱(250mm
4
6mm,5
m),流动相为乙腈-0
1%醋酸,梯度洗脱,流速1mLmin,测定波长335-nm,采用电喷雾负模式电离(ESI),选定的母离子和子离子分别为野黄芩苷m/z461/285,芹菜素m/z269/117。

2、结果:野黄芩-1-1苷浓度在2
6~72
7mgL,芹菜素浓度在2
3~63
8mgL范围内线性关系良好;所测12个产地半枝莲中,野黄芩苷和芹菜素的含量范围分别为0
03%~0
39%和0
02%~0
30%;平均回收率(n=5)分别为99
1%和97
3%,RSD分别为1
4%和0
7%。结论:本方法简单准确,适合于半枝莲中野黄芩苷和芹菜素的含量测定。关键词:半枝莲;野黄芩苷;芹菜素;液相色谱-二级质谱联用法中图分类号:R917文献标识码:A文章编号:0254-1793(2009)09-1451-03LC-MS/MSsimultaneousdeterminationof

3、scutellarinandapigeninofHerbaScutellariaeBarbataeproducedindifferentdistricts*JIAOYan,WANGYing-feng,LIUSuo-lan(AnalysisandTestingCenterofCapitalNormalUniversity,Beijing100048,China)AbstractObjective:TodetectandquantificatescutellarinandapigenininHerbaScutellariaeBarbataeofdifferentdistrict

4、sbyLC-MS/MS
Methods:DeterminationofLCsystemconsistedofaDiscoveryC18column(250mm
4
6mm,5
m)withacetonitrileandwater(0
1%aceticacid)inlineargradientcondition.Theflowratewas1mL-1minandthewavelengthofdetectionwas335nm.ThemassspectrometerwasoperatedunderthenegativeionmodewiththeESIsource.Thetra

5、nsitionofm/z461/285andm/z269/117wasusedtoqualifyscutellarinandapigenin,respectively.Results:Thelinearrangesofcalibrationcurveofscutellarinandapigeninwere2
6-72
7mg-1-1Land2
3-63
8mgL,respectively.ByusingtheestablishedLC-MS/MSmethods,12samplesofHerbaScutellariaeBarbataeindifferentdistrict

6、swereanalyzed.Theresultsshowedthatthecontentsofscutellarinandapigeninwere0
03%-0
39%and0
02%-0
30%,respectively.Theaveragerecoveries(n=5)ofscutellarinandapigeninwere99
1%and97
3%,andtheRSDswere1
4%and0
7%,respectively.Conclusion:Theproposedmethodissimpleandtheresultisaccurate.Itcanbeusedfo

7、rdeterminationofscutellarinandapigenininHerbaScutellariaeBarbatae.Keywords:HerbaScutellariaeBarbatae;scutellarin;apigenin;LC-MS/MS[1]半枝莲为唇形科植物半枝莲(Scutellariabarbata分。目前对这2种物质的含量测定多采用高效液D.Don)的干燥全草,有清热解毒、化瘀利尿的功效。相色谱法,因为这2种物质极性的差别,尚未有用1[2]半枝莲的主要成分为黄酮类化合物,如