微流蒸发光散射检测器与加压毛细管电色谱联用测定川贝枇杷糖浆中6种有效成分的含量  

Determination of Six Active Components in Chuanbei Pipa Syrups by Microfluidic Evaporative Light Scattering Detector Coupled to Pressurized Capillary Electrochromatography

作　　者：周文莉[1] 阚文彬 王玉红 张琳 王彦[1] 阎超[1,2] 

机构地区：[1]上海交通大学药学院,上海200240 [2]上海通微分析技术有限公司,上海201203

出　　处：《分析测试学报》2015年第3期321-327,共7页Journal of Instrumental Analysis

基　　金：国家重大科学仪器设备开发专项项目(2011YQ150072,2011YQ15007202);国家自然科学基金项目(21175092,21105064);上海市自然科学基金项目(12ZR1413600);上海市科委“科技创新行动计划”科学仪器研制项目(14142200200,13142200100)

摘　　要：建立了同时测定川贝枇杷糖浆中6种有效成分（桔梗皂苷D、贝母辛、齐墩果酸、西贝素、贝母甲素和贝母乙素）含量的微流蒸发光散射检测器（μELSD）与加压毛细管电色谱（pCEC）联用检测方法.搭建pCEC-μELSD联用平台,采用C18毛细管色谱柱（EP-150-15-3-C18）,流动相为乙腈（A）-10 mmol·L-1甲酸-三乙胺水溶液（pH 11.0） （B）,梯度洗脱,柱流速为1.02 μL·min-1,施加电压为＋ 10 kV,雾化载气流速为0.4 L·min-1,蒸发温度为40℃.川贝枇杷糖浆中6种有效成分可在10 min内得到分离检测,6种有效成分的线性范围可达4个数量级,检出限均在Pg水平,加标回收率为97.9％～ 103.0％.所建立的pCEC-μELSD联用方法精密度、重复性和稳定性良好,且简便、快速、可靠,可用于川贝枇杷糖浆中6种有效成分的含量测定.Microfluidic evaporative light scattering detector（txELSD） coupled to pressurized capillary electrochromatography （pCEC） was applied in the separation and detection of six active components, e.g. platycodin D, peimisine, oleanolic acid, imperialine, peimine and peiminine in Chuanbei Pi- pa Syrups. The simultaneous analysis of six active components by pCEC - IxELSD was performed on a Cls capillary column（EP- 150- 15 -3 -Cls ） with mobile phase A： acetonitrile and mobile phase B： 10 mmol L-1 formic acid- triethylamine aqueous solution（ pH i i. 0） by gradient elution. The optimal conditions were as follows： column flow rate： 1.02 μL min-1, applied voltage： ＋ 10 kV, nebulizing gas flow rate： 0.4 L min-1 and evaporative temperature： 40 ℃. Six active components in Chuanbei Pipa Syrups were successfully separated in 10 min with the excellent linearity of four orders of magnitude. The limit of detection （LOD） could reach up to the level of pg, and the recoveries were between 97.9% and 103.0%. The precision, repeatability and stability indicated a good re- producibility for the determination. The results also demonstrated the feasibility and practicality of pCEC - μELSD platform. The method could be used for the determination of the active ingredients in Chuanbei Pipa Syrups.

关 键 词：微流蒸发光散射检测器 加压毛细管电色谱 贝母生物碱类 桔梗皂苷D 齐墩果酸 

分 类 号：O657.8[理学—分析化学] TQ460.72[理学—化学]