Enrichment of trace bioactive constituents and metabolites from complex biological samples is challenging.This study presented a one-pot synthesis of magnetic polydopamine nanoparticles(Fe3O4@-SiO2@PDA NPs)with multip...Enrichment of trace bioactive constituents and metabolites from complex biological samples is challenging.This study presented a one-pot synthesis of magnetic polydopamine nanoparticles(Fe3O4@-SiO2@PDA NPs)with multiple recognition sites for the magnetic dispersive solid-phase extraction(MDSPE)of ginsenosides from rat plasma treated with white ginseng.The extracted ginsenosides were characterized by combining an ultra-high-performance liquid chromatography coupled to a highresolution mass spectrometry with supplemental UNIFI libraries.Response surface methodology was statistically used to optimize the extraction procedure of the ginsenosides.The reusability of Fe3O4@-SiO2@PDA NPs was also examined and the results showed that the recovery rate exceeded 80%after recycling 6 times.Furthermore,the proposed method showed greater enrichment efficiency and could rapidly determine and characterize 23 ginsenoside prototypes and metabolites from plasma.In comparison,conventional methanol method can only detect 8 ginsenosides from the same plasma samples.The proposed approach can provide methodological reference for the trace determination and characterization of different bioactive ingredients and metabolites of traditional Chinese medicines and food.展开更多
A rapid and sensitive method for analyzing trace b-blockers in complex biological samples,which involved magnetic solid-phase extraction(MSPE)coupled with Fourier transform ion cyclotron resonance mass spectrometry(FT...A rapid and sensitive method for analyzing trace b-blockers in complex biological samples,which involved magnetic solid-phase extraction(MSPE)coupled with Fourier transform ion cyclotron resonance mass spectrometry(FTICR-MS),was developed.Novel nanosilver-functionalized magnetic nanoparticles with an interlayer of poly(3,4-dihydroxyphenylalanine)(polyDOPA@Ag-MNPs)were synthesized and used as MSPE adsorbents to extract trace b-blockers from biological samples.After extraction,the analytes loaded on the polyDOPA@Ag-MNPs were desorbed using an organic solvent and analyzed by FTICR-MS.The method was rapid and sensitive,with a total detection procedure of less than 10 min as well as limits of detection and quantification in the ranges of 3.5-6.8 pg/mL and 11.7-22.8 pg/mL,respectively.The accuracy of the method was also desirable,with recoveries ranging from 80.9%to 91.0%following the detection of analytes in human blood samples.All the experimental results demonstrated that the developed MSPE-FTICR-MS method was suitable for the rapid and sensitive analysis of trace b-blockers in complex biological samples.展开更多
In this work, a metal-organic framework derived nanoporous carbon (MOF-5-C) was fabricated and modified with Fe3O4 magnetic nanoparticles. The resulting magnetic MOF-5-derived porous carbon (Fe304@MOF-5-C) was the...In this work, a metal-organic framework derived nanoporous carbon (MOF-5-C) was fabricated and modified with Fe3O4 magnetic nanoparticles. The resulting magnetic MOF-5-derived porous carbon (Fe304@MOF-5-C) was then used for the magnetic solid-phase extraction of chlorophenols (CPs) from mushroom samples prior to high performance liquid chromatography-ultraviolet detection. Scanning electron microscopy, transmission electron microscopy, X-ray diffraction, and N2 adsorption were used to characterize the adsorbent. After experimental optimization, the amount of the adsorbent was chosen as 8.0 mg, extraction time as 10 min, sample volume as 50 mL, desorption solvent as 0.4 mL (0.2 mL × 2) of alkaline methanol, and sample pH as 6. Under the above optimized conditions, good linearity for the analytes was obtained in the range of 0.8-100.0 ng g 1 with the correlation coefficients between 0.9923 and 0.9963. The limits of detection (SIN= 3) were in the range of 0.25-0.30 ng g-1, and the relative standard deviations were below 6.8%. The result showed that the Fe304@MOF-5-C has an excellent adsorption capacity for the analytes.展开更多
In the present work,a novel amino-functionalized hexaalkylguanidinium chloride ionic liquid was prepared and grafted on the surface of magnetic materials through polyethyleneimine to enrich polycyclic aromatic hydroca...In the present work,a novel amino-functionalized hexaalkylguanidinium chloride ionic liquid was prepared and grafted on the surface of magnetic materials through polyethyleneimine to enrich polycyclic aromatic hydrocarbons in water in combination with HPLC equipped with an ultraviolet detector.The effect of several parameters on the extraction efficiency was investigated,including the desorption solvent,the amounts of sorbents,the extraction time,the desorption time and the salt amount.Under the optimized conditions,the method validation exhibited good linearity with correlation coefficients above 0.994 in the range of 0.2-300 ng/mL and low limits of detection and quantification of 0.05 and 0.2 ng/mL,respectively.Besides,relative recoveries were in the range of 80-120%,and the intra-day and inter-day repeatability were good with the relative standard deviations of less than 20%.Finally,the guanidinium ionic liquid modified magnetic materials were applied for the extraction of polycyclic aromatic hydrocarbons from real water samples to demonstrate the utility,and the results show that the proposed method has good prospect for effective enrichment and determination of pollutants in water.展开更多
The analysis of endogenous glycoproteins and glycopeptides in human body fluids is of great importance for screening and discovering disease biomarkers with clinical significance.However,the presence of interfering su...The analysis of endogenous glycoproteins and glycopeptides in human body fluids is of great importance for screening and discovering disease biomarkers with clinical significance.However,the presence of interfering substances makes the direct quantitative detection of low-abundance glycoproteins and glycopeptides in human body fluids one of the great challenges in analytical chemistry.Magnetic solid phase extraction(MSPE)has the advantages of easy preparation,low cost and good magnetic responsiveness.Magnetic adsorbents are the core of MSPE technology,and magnetic adsorbents based on different functional materials are widely used in the quantitative analysis of glycoproteins and glycopeptides in human body fluids,making it possible to analyze glycoproteins and glycopeptides with low abundance as well as multiple types,which provides a technical platform for screening and evaluating glycoproteins and glycopeptides in body fluids as disease biomarkers.In this paper,we focus on the recent advances in the application of MSPE technology and magnetic adsorbents for the separation and enrichment of glycoproteins and glycopeptides in human body fluids,and the future trends and application prospects in this field are also presented.展开更多
通过简单的搅拌共混方式制备了磁性氨基功能化的金属有机骨架化合物(MOFs)材料,得到的复合材料磁性和热稳定性良好,比表面积大,被用于不同极性防腐剂(苯甲酸、山梨酸、对羟基苯甲酸丙酯和对羟基苯甲酸丁酯)的萃取。优化磁固相萃取及解...通过简单的搅拌共混方式制备了磁性氨基功能化的金属有机骨架化合物(MOFs)材料,得到的复合材料磁性和热稳定性良好,比表面积大,被用于不同极性防腐剂(苯甲酸、山梨酸、对羟基苯甲酸丙酯和对羟基苯甲酸丁酯)的萃取。优化磁固相萃取及解吸条件后,将解吸液引入高效液相色谱-紫外检测分析仪器,采用Purospher~? STAR LP C18色谱柱(250 mm×4.6 mm, 5μm)分离,以甲醇-10 mmol/L醋酸铵水溶液(50∶50, v/v)为流动相进行梯度洗脱。结果表明,目标防腐剂的检出限为0.51~1.89μg/L;苏打水、维生素饮料和方便面面饼中目标防腐剂的加标回收率为72.2%~109%。该方法简单快速,准确可靠,适用于饮料和食品中不同极性防腐剂的分析,为食品安全及质量监控提供了有效的技术有段。展开更多
基金This work was supported by grants from the National Natural Science Foundation of China Key Program(NO.81530094)General Program(NO.81573574,81873193)the Science and Technology Development Project of Jilin Province(20190201283JC).
文摘Enrichment of trace bioactive constituents and metabolites from complex biological samples is challenging.This study presented a one-pot synthesis of magnetic polydopamine nanoparticles(Fe3O4@-SiO2@PDA NPs)with multiple recognition sites for the magnetic dispersive solid-phase extraction(MDSPE)of ginsenosides from rat plasma treated with white ginseng.The extracted ginsenosides were characterized by combining an ultra-high-performance liquid chromatography coupled to a highresolution mass spectrometry with supplemental UNIFI libraries.Response surface methodology was statistically used to optimize the extraction procedure of the ginsenosides.The reusability of Fe3O4@-SiO2@PDA NPs was also examined and the results showed that the recovery rate exceeded 80%after recycling 6 times.Furthermore,the proposed method showed greater enrichment efficiency and could rapidly determine and characterize 23 ginsenoside prototypes and metabolites from plasma.In comparison,conventional methanol method can only detect 8 ginsenosides from the same plasma samples.The proposed approach can provide methodological reference for the trace determination and characterization of different bioactive ingredients and metabolites of traditional Chinese medicines and food.
基金supported by the National Natural Science Foundation of China(Grant Nos.:21976168,22127810,and 22004113)Key Research and Development Program of Guangdong Province(Grant No.:2020B1111350002)+1 种基金Guangdong Basic and Applied Basic Research Foundation(Grant No.:2019A1515110420)GDAS0 Project of Science and Technology Development(Grant No.:2021GDASYL-20210103034).
文摘A rapid and sensitive method for analyzing trace b-blockers in complex biological samples,which involved magnetic solid-phase extraction(MSPE)coupled with Fourier transform ion cyclotron resonance mass spectrometry(FTICR-MS),was developed.Novel nanosilver-functionalized magnetic nanoparticles with an interlayer of poly(3,4-dihydroxyphenylalanine)(polyDOPA@Ag-MNPs)were synthesized and used as MSPE adsorbents to extract trace b-blockers from biological samples.After extraction,the analytes loaded on the polyDOPA@Ag-MNPs were desorbed using an organic solvent and analyzed by FTICR-MS.The method was rapid and sensitive,with a total detection procedure of less than 10 min as well as limits of detection and quantification in the ranges of 3.5-6.8 pg/mL and 11.7-22.8 pg/mL,respectively.The accuracy of the method was also desirable,with recoveries ranging from 80.9%to 91.0%following the detection of analytes in human blood samples.All the experimental results demonstrated that the developed MSPE-FTICR-MS method was suitable for the rapid and sensitive analysis of trace b-blockers in complex biological samples.
基金Financial support from the National Natural Science Foundation of China (Nos. 31471643, 31571925)the Innovation Research Program of the Department of Education of Hebei for Hebei Provincial Universities (No. LJRC009)
文摘In this work, a metal-organic framework derived nanoporous carbon (MOF-5-C) was fabricated and modified with Fe3O4 magnetic nanoparticles. The resulting magnetic MOF-5-derived porous carbon (Fe304@MOF-5-C) was then used for the magnetic solid-phase extraction of chlorophenols (CPs) from mushroom samples prior to high performance liquid chromatography-ultraviolet detection. Scanning electron microscopy, transmission electron microscopy, X-ray diffraction, and N2 adsorption were used to characterize the adsorbent. After experimental optimization, the amount of the adsorbent was chosen as 8.0 mg, extraction time as 10 min, sample volume as 50 mL, desorption solvent as 0.4 mL (0.2 mL × 2) of alkaline methanol, and sample pH as 6. Under the above optimized conditions, good linearity for the analytes was obtained in the range of 0.8-100.0 ng g 1 with the correlation coefficients between 0.9923 and 0.9963. The limits of detection (SIN= 3) were in the range of 0.25-0.30 ng g-1, and the relative standard deviations were below 6.8%. The result showed that the Fe304@MOF-5-C has an excellent adsorption capacity for the analytes.
基金The work was financially supported by the Fundamental Research Funds for the Central Universities(DUT18RC(4)058).
文摘In the present work,a novel amino-functionalized hexaalkylguanidinium chloride ionic liquid was prepared and grafted on the surface of magnetic materials through polyethyleneimine to enrich polycyclic aromatic hydrocarbons in water in combination with HPLC equipped with an ultraviolet detector.The effect of several parameters on the extraction efficiency was investigated,including the desorption solvent,the amounts of sorbents,the extraction time,the desorption time and the salt amount.Under the optimized conditions,the method validation exhibited good linearity with correlation coefficients above 0.994 in the range of 0.2-300 ng/mL and low limits of detection and quantification of 0.05 and 0.2 ng/mL,respectively.Besides,relative recoveries were in the range of 80-120%,and the intra-day and inter-day repeatability were good with the relative standard deviations of less than 20%.Finally,the guanidinium ionic liquid modified magnetic materials were applied for the extraction of polycyclic aromatic hydrocarbons from real water samples to demonstrate the utility,and the results show that the proposed method has good prospect for effective enrichment and determination of pollutants in water.
基金supported by the Natural Science Foundation of Jilin Provincial Science&Technology Department(No.20190201079JC)。
文摘The analysis of endogenous glycoproteins and glycopeptides in human body fluids is of great importance for screening and discovering disease biomarkers with clinical significance.However,the presence of interfering substances makes the direct quantitative detection of low-abundance glycoproteins and glycopeptides in human body fluids one of the great challenges in analytical chemistry.Magnetic solid phase extraction(MSPE)has the advantages of easy preparation,low cost and good magnetic responsiveness.Magnetic adsorbents are the core of MSPE technology,and magnetic adsorbents based on different functional materials are widely used in the quantitative analysis of glycoproteins and glycopeptides in human body fluids,making it possible to analyze glycoproteins and glycopeptides with low abundance as well as multiple types,which provides a technical platform for screening and evaluating glycoproteins and glycopeptides in body fluids as disease biomarkers.In this paper,we focus on the recent advances in the application of MSPE technology and magnetic adsorbents for the separation and enrichment of glycoproteins and glycopeptides in human body fluids,and the future trends and application prospects in this field are also presented.
文摘通过简单的搅拌共混方式制备了磁性氨基功能化的金属有机骨架化合物(MOFs)材料,得到的复合材料磁性和热稳定性良好,比表面积大,被用于不同极性防腐剂(苯甲酸、山梨酸、对羟基苯甲酸丙酯和对羟基苯甲酸丁酯)的萃取。优化磁固相萃取及解吸条件后,将解吸液引入高效液相色谱-紫外检测分析仪器,采用Purospher~? STAR LP C18色谱柱(250 mm×4.6 mm, 5μm)分离,以甲醇-10 mmol/L醋酸铵水溶液(50∶50, v/v)为流动相进行梯度洗脱。结果表明,目标防腐剂的检出限为0.51~1.89μg/L;苏打水、维生素饮料和方便面面饼中目标防腐剂的加标回收率为72.2%~109%。该方法简单快速,准确可靠,适用于饮料和食品中不同极性防腐剂的分析,为食品安全及质量监控提供了有效的技术有段。