加压毛细管电色谱-微流蒸发光散射检测器联用系统的构建及其应用  

Construction of Microflow Evaporative Light Scattering Detector Coupled with Pressurized Capillary Electrochromatography and Its Application

作　　者：高红秀[1] 周文莉[1] 王玉红 李鹏 谷雪[1] 王彦[1] 李静[1,2] 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：《分析化学》2014年第5期766-772,共7页Chinese Journal of Analytical Chemistry

基　　金：国家重大科学仪器设备开发专项项目(No.2011YQ150072);国家自然科学基金项目(Nos.21175092;.21105064);上海市自然科学基金项目(No.12ZR1413600);上海市引进技术的吸收与创新计划项目(No.JJ-YJCX-03-10-2586)资助~~

摘　　要：构建微流蒸发光散射检测器（μELSD）与加压毛细管电色谱（ pCEC）联用系统,测定中药提取物注射用血塞通（冻干）中三七皂苷R1、人参皂苷Rg1, Re, Rb1、Rd考察系统的实用性和稳定性。用C18毛细管色谱柱,通过对流动相体系、梯度洗脱条件、雾化载气流速、蒸发温度、施加电压等参数的优化,确定了注射用血塞通（冻干）5种成分含量测定的最佳测定参数。最佳测定参数如下,流动相A为15 mmol/L甲酸-三乙胺乙腈溶液（pH=7.0）,流动相B为15 mmol/L甲酸-三乙胺溶液（pH=7.0）；梯度洗脱条件：0~10 min,19%A；10~30 min,22%A；30~35 min,36%A；35~45 min,40%A。雾化载气流速2 L/min；蒸发温度120℃；施加电压＋8 kV。5种成分线性范围为8.6~146.9 ng （三七皂苷 R1）、6.9~189.7 ng （人参皂苷 Rg1）、6.8~171.4 ng（人参皂苷Re）、9.4~156.1 ng（人参皂苷Rb1）、7.5~180.5 ng（人参皂苷Rd）,5种成分回收率都在95%~105%之间。实验表明,构建的pCEC-μELSD联用系统能用于药物中有效成分的含量测定。μELSD的构建为毛细管液相色谱、毛细管电色谱和毛细管电泳分离技术提供了一种全新的检测手段。A novel separation system of microflow evaporative light scattering detector （μELSD） coupled with pressurized capillary electrochromatography （ pCEC） was built and applied to the separation and detection of notoginsenoside R1 , ginsenoside Rg1 , ginsenoside Re, ginsenoside Rb1 , ginsenoside Rd in traditional Chinese medicine extract Xuesaitong （lyophilization）. With C18 capillary column the best separation conditions were established by optimizing the mobile phase composition, gradient conditions, flow rate of atomizing gas, evaporating temperature and applied voltage. The mobile phase A was acetonitrile containing 15 mmol/L formic acid-triethylamine acetonitrile （ pH=7 . 0 ） , and the mobile phase B was 15 mmol/L formic acid-triethylamine acetonitrile （pH=7. 0）. The optimized gradient elution conditions were as follows：0-10 min, 19%A;10-30 min, 22%A;30-35 min, 36%A;35-45 min, 40%A. The flow rate of atomizing gas（ N2 ） was 2 L/min. The evaporating temperature was 120 ℃. The applied voltage was＋8 kV. A good linearity was obtained：8. 6-146. 9 ng （ notoginsenoside R1 ）, 6. 9-189. 7 ng （ ginsenoside Rg1 ）, 6. 8-171. 4 ng （ginsenoside Re）, 9. 4-156. 1 ng （ginsenoside Rb1）, 7. 5-180. 5 ng （ginsenoside Rd）. The recovery was between 95%-105%. The results show that the pCEC-μELSD system can be used for the determination of the content of active ingredients in medicines. The construction ofμELSD provides an innovative detection means for capillary liquid chromatography, pCEC and capillary electrophoresis.

关 键 词：微流蒸发光散射检测器 加压毛细管电色谱 血塞通 三七皂苷 人参皂苷 

分 类 号：O657[理学—分析化学] TP216[理学—化学]