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基于MOF-5(Zn)-FeO纳米复合材料的磁性固相微萃取结合高效液相色谱-紫外检测法用于秋水仙提取物根及血浆样品中秋水仙碱的高效富集

MOF-5(Zn)-FeO nanocomposite based magnetic solid-phase microextraction followed by HPLC-UV for efficient enrichment of colchicine in root of colchicium extracts and plasma samples.

作者信息

Bahrani Sonia, Ghaedi Mehrorang, Dashtian Kheibar, Ostovan Abbas, Mansoorkhani Mohammad Javad Khoshnood, Salehi Amin

机构信息

Departmentof chemistry, Yasouj University, Yasouj, 75918-74831, Iran.

Departmentof chemistry, Yasouj University, Yasouj, 75918-74831, Iran.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Nov 1;1067:45-52. doi: 10.1016/j.jchromb.2017.09.044. Epub 2017 Sep 29.

Abstract

In present work, facile method is developed for determination of colchicine in human plasma sample, autumn and spring root of colchicium extracts by ultrasound assisted dispersive magnetic solid phase microextraction followed by HPLC-UV method (UAD-MSPME-HPLC-UV). Magnetic (FeO-nanoparticles) metal organic framework-5, (MOF-5(Zn)-FeONPs) was synthesized by dispersing MOF-5 and Fe(NO).9HO in ethylene glycol (as capping agent) and NaOH (pH adjustment agent) by hydrothermal method. The prepared sorbent was characterized via XRD and SEM analysis and applied as magnetic solid phase in UAD-MSPME-HPLC-UV method. In this method, colchicine molecules were sorbed on MOF-5(Zn)-FeONPs sorbent by various mechanisms like ion exchange, hydrogen bonding and electrostatic, ᴨ-ᴨ, hard-hard and dipole-ion interaction followed by exposing sonication waves as incremental mass transfer agent and then the sorbent was separated from the sample matrix by an external magnetic fields. Subsequently, accumulated colchicine were eluted by small volume of desorption organic solvent. Influence of operational variables such as MOF-5(Zn)-FeONPs mass, volume of extracting solvent and sonication time on response property (recovery) were studied and optimized by central composite design (CCD) combined with desirability function (DF) approach. Under optimum condition, the method has wide linear calibration rang (0.5-1700ngmL) with reasonable detection limit (0.13ngmL) and R=0.9971. Finally, the UAD-MSPME-HPLC-UV method was successfully applied for determination of colchicine autumn and spring root of colchicium extracts and plasma samples.

摘要

在本研究中,开发了一种简便的方法,通过超声辅助分散磁性固相微萃取结合高效液相色谱 - 紫外检测法(UAD - MSPME - HPLC - UV)测定人血浆样品、秋水仙提取物和春根提取物中的秋水仙碱。通过水热法将金属有机骨架 - 5(MOF - 5(Zn))和Fe(NO₃)₃·9H₂O分散在乙二醇(作为封端剂)和NaOH(pH调节剂)中来合成磁性(Fe₃O₄ - 纳米颗粒)金属有机骨架 - 5(MOF - 5(Zn) - Fe₃O₄NPs)。通过X射线衍射(XRD)和扫描电子显微镜(SEM)分析对制备的吸附剂进行表征,并将其用作UAD - MSPME - HPLC - UV方法中的磁性固相。在该方法中,秋水仙碱分子通过离子交换、氢键、静电作用、π - π、硬 - 硬和偶极 - 离子相互作用等多种机制吸附在MOF - 5(Zn) - Fe₃O₄NPs吸附剂上,随后通过施加超声作为增量传质剂,然后通过外部磁场将吸附剂与样品基质分离。随后,用少量解吸有机溶剂洗脱富集的秋水仙碱。采用中心复合设计(CCD)结合期望函数(DF)方法研究并优化了诸如MOF - 5(Zn) - Fe₃O₄NPs质量、萃取溶剂体积和超声时间等操作变量对响应特性(回收率)的影响。在最佳条件下,该方法具有宽线性校准范围(0.5 - 1700 ng/mL)、合理的检测限(0.13 ng/mL)且R² = 0.9971。最后,UAD - MSPME - HPLC - UV方法成功应用于测定秋水仙提取物和春根提取物以及血浆样品中的秋水仙碱。

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