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疯草中苦马豆素的固相萃取-亲水作用色谱检测
李金成1, 杨国栋1, 王 研,等1
西北农林科技大学 动物医学院
摘要:
【目的】建立疯草中苦马豆素的固相萃取 亲水作用色谱分析方法。【方法】以小花棘豆、毛瓣棘豆、黄花棘豆、甘肃棘豆、冰川棘豆等5种疯草为样品,经纯乙醇索氏提取和SPE固相萃取柱净化,采用Waters X-Bredge HILIC色谱柱和蒸发光散射检测器,对流动相中的有机溶剂种类及质量浓度、缓冲盐浓度和柱温等条件进行优化,检测苦马豆素含量并用质谱检测法进行验证。【结果】苦马豆素与疯草中的其他成分在异丙醇2 mmol/L乙酸铵(体积比为52∶48)流动相条件下可以得到较好地分离;苦马豆素在10~100 μg/mL的质量浓度与色谱峰面积具有良好的线性关系(r2=0.997),检出限(LOD)(信噪比=3)为6 μg/mL,定量限(LOQ)(信噪比=10)为20 μg/mL,加标回收率在80%~100%。【结论】建立的固相萃取-亲水作用色谱检测方法简单、快速、精密度和准确度高,可替代传统的阳离子交换树脂净化-衍生化法用于疯草中苦马豆素的测定。
关键词:  固相萃取  亲水色谱法  疯草  苦马豆素
DOI:
分类号:
基金项目:国家自然科学基金项目(30871901)
Determination of swainsonine in locoweeds by hydrophilic interaction chromatography combined with solid phase extraction
LI Jin-cheng,YANG Guo-dong,WANG Yan,et al
Abstract:
【Objective】This study established a hydrophilic interaction liquid chromatography combined with solid phase extraction method (SPE-HILIC) for the determination of swainsonine in locoweeds.【Method】Oxytropis glabra,O.sericopetala,O.ochrocepala,O.kansuensis,and Astragalus strictus were collected as samples of locoweeds.The samples were extracted with ethyl ethanol,purified with solid phase extraction column and analyzed by a Waters X-Bredge HILIC column,and then swainsonine was detected by evaporative light scattering detector.The extraction conditions including organic solvents and their concentrations,buffer salt concentration,and column temperature were optimized and the results were validated using mass spectrometry.【Result】Swainsonine was separated from other components in extracts of locoweeds with mobile phase of isopropanol 2 mmol/L ammonium acetate (volume ratio was 52∶48).The calibration curve was linear within the range of 10-100 μg/mL (r2=0.997),the detection limit was 6 μg/mL and the limit of quantitation was 20 μg/mL.The recovery rate was 80%-100%.【Conclusion】This study established a solid phase extraction-hydrophilic interaction chromatography method (SPE-HILIC) for detection of swainsonine.The method was simple and accurate,which can be used to determine swainsonine content in locoweeds to replace conventional cation exchange resin purification.
Key words:  solid phase extraction  hydrophilic interaction chromatographic  locoweeds  swainsonine