首页> 外文期刊>RSC Advances >Zeolite based solid-phase extraction coupled with UPLC-Q-TOF-MS for rapid analysis of acetylcholinesterase binders from crude extract of Corydalis yanhusuo
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Zeolite based solid-phase extraction coupled with UPLC-Q-TOF-MS for rapid analysis of acetylcholinesterase binders from crude extract of Corydalis yanhusuo

机译:基于沸石的固相萃取与UPLC-Q-TOF-MS耦合,用于从Corydalis yanhusuo的粗提物迅速分析乙酰胆碱酯酶粘合剂

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摘要

A very convenient, sensitive and precise solid-phase extraction approach was established for extract and analysis of acetylcholinesterase binders from crude extract of Corydalis yanhusuo. This approach was based on the retention of binders by acetylcholinesterase immobilized zeolite. The retained acetylcholinesterase binders were eluted and analyzed by ultra-high performance liquid chromatography and quadrupole-time-of-flight mass spectrometry. The powder X-ray diffraction (XRD), transmission electron microscopy (TEM), and Fourier transform infrared (FT-IR) spectroscopy techniques were employed for the characterization of acetylcholinesterase immobilized zeolite. Some experimental conditions such as incubation temperature, time, buffer pH and ion strength, which may affect binding capability, were investigated by using coptisine as a model inhibitor. The optimal incubation conditions were as follows: wash times: 4, wash solvent: 50% methanol-water, incubation time: 20 min, temperature: 37 degrees C, ion strength: 10 mM, pH: 7.4. The proposed approach was successfully applied for the extraction of acetylcholinesterase binders from crude extract of Corydalis yanhusuo. These binders were further validated by acetylcholinesterase inhibitory assay. Fourteen acetylcholinesterase inhibitors were identified, and ten of which, including dehydrocorydaline, allocryptopine, corydaline, dehydroglaucine, protopine, tetrahydrocoptisine, tetrahydropalmatine, corynoline, tetrahydrocolumbamne and tetrahydroberberine, were reported for the first time. In addition, the merits and shortcomings of zeolite based solid-phase extraction approach were compared with that of magnetic nanoparticles based solidphase extraction approach.
机译:建立了一种非常方便,敏感和精确的固相提取方法,用于从Corydalis yanhusuo的粗提物中提取和分析乙酰胆碱酯酶粘合剂。这种方法是基于乙酰胆碱酯酶固定的沸石的粘合剂的保留。洗脱保留的乙酰胆碱酯酶粘合剂并通过超高效液相色谱法和四极 - 飞行时间质谱法分析。粉末X射线衍射(XRD),透射电子显微镜(TEM)和傅里叶变换红外(FT-IR)光谱技术用于表征乙酰胆碱酯酶固定的沸石。通过使用Coptisine作为模型抑制剂,研究了一些实验条件,例如孵育温度,时间,缓冲pH和离子强度,这可能影响结合能力。最佳培养条件如下:洗涤时间:4,洗涤溶剂:50%甲醇 - 水,孵育时间:20分钟,温度:37℃,离子强度:10mm,pH:7.4。成功地应用了所提出的方法,用于从Corydalis yanhusuo的粗提取物中提取乙酰胆碱酯酶粘合剂。通过乙酰胆碱酯酶抑制试验进一步验证这些粘合剂。鉴定了十四乙酰胆碱酯酶抑制剂,其中10个包括脱氢胶质肽,羟基胺,烯丙胺,脱氢辛酸氨基,脱氢喹,四氢丙氨酸,四氢丙氨酸,植物甾胺,四氢丙氨酸,四氢甲酰氨基和四氢铀霉素。此外,基于沸石的固相提取方法的优点和缺点与基于磁性纳米粒子的固相提取方法进行了比较。

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  • 来源
    《RSC Advances》 |2016年第100期|共11页
  • 作者单位

    Nanjing Univ Chinese Med Sch Pharm Xianlin Campus 138 Xianlin Ave Nanjing 210023 Jiangsu Peoples R China;

    Nanjing Univ Chinese Med Sch Pharm Xianlin Campus 138 Xianlin Ave Nanjing 210023 Jiangsu Peoples R China;

    Nanjing Univ Chinese Med Sch Pharm Xianlin Campus 138 Xianlin Ave Nanjing 210023 Jiangsu Peoples R China;

    Nanjing Univ Chinese Med Sch Pharm Xianlin Campus 138 Xianlin Ave Nanjing 210023 Jiangsu Peoples R China;

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  • 正文语种 eng
  • 中图分类 化学;
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