HPLC-MS/MS法同时测定新疆一枝蒿药材中5个成分的含量  

Simultaneous determination of 5 constituents in Artemisia rupestris L. by HPLC- MS / MS

作　　者：蔡晓翠 贺金华 顾政一 张瑞萍[2] 毛艳 

机构地区：[1]新疆维吾尔自治区药物研究所,乌鲁木齐830004 [2]天然药物活性物质与功能国家重点实验室,中国医学科学院北京协和医学院药物研究所,北京100050

出　　处：《药物分析杂志》2013年第10期1672-1676,共5页Chinese Journal of Pharmaceutical Analysis

基　　金：国家科技重大专项"重大新药创制"(课题编号:2011ZX09102-009-07)

摘　　要：目的:建立新疆一枝蒿药材中绿原酸、木犀草素、一枝蒿酮酸、紫花牡荆素及芹菜素5个指标成分的含量测定方法,比较不同产地及不同采收期新疆一枝蒿药材中5个成分的含量。方法:采用HPLC-MS/MS法,使用Agilent C18色谱柱(4.6 mm×250mm,5μm),流动相为甲醇-0.2%甲酸溶液,梯度洗脱,流速1.0 mL·min-1,柱温30℃,进样量10μL;质谱采用电喷雾离子源(ESI源),负离子模式检测,扫描方式为多反应监测(MRM)。结果:绿原酸、木犀草素、一枝蒿酮酸、紫花牡荆素及芹菜素分别在52.4～1048μg·mL-1(r=0.9996)、2.965～118.6μg·mL-1(r=0.9997)、25～700μg·mL-1(r=0.9993)、5.96～238.4μg·mL-1(r=0.9994)、1.219～243.8μg·mL-1(r=0.9992)范围内线性关系良好;平均加样回收率在97.6%～100.9%之间,RSD均小于2.5%。结论:该方法灵敏、快速、准确,专属性强,可为新疆一枝蒿药材的质量标准研究提供依据。Objective： To establish a method for simultaneous determination of 5 main bioactive constituents including chlorogenic acid,luteolin,rupestonic acid,casticin and apigenin in Artemisia rupestris L.by HPLC-MS/MS,and to compare the content differences of Artemisia rupestris L.from different areas and different harvest periods. Methods： The HPLC separation was performed on an Agilent Cl8 column（250 mm×4.6 mm,5 μm）in a gradient elute mode with methanol and water（containing 0.2% formic acid）as the mobile phase at a flow rate of 1.0 mL·min-1.MS detection was performed with multiple reaction monitoring（MRM）mode using negative electrospray ionization. Results： The linearity was achieved in the range of 52.4-1048 μg·mL-1（r=0.9996）for chlorogenic acid,2.965-118.6 μg·mL-1（r=0.9997）for luteolin,25-700 μg·mL-1（r=0.9993）for rupestonic acid,5.96-238.4 μg·mL-1（r=0.9994）for casticin,and 1.219-243.8 μg·mL-1（r=0.9992）for apigenin.The recoveries were 97.6%-100.9% with RSD less than 2.5%. Conclusion： The method is sensitive,rapid,accurate and specific and can be used for the quality control of Artemisia rupestris L.

关 键 词：新疆一枝蒿 绿原酸 木犀草素 一枝蒿酮酸 紫花牡荆素 芹菜素 不同产地不同采收期含量测定 高效液相色谱-串联质谱 

分 类 号：R917[医药卫生—药物分析学]