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1.
磁性固相萃取(Magnetic solid-phase extraction,MSPE)是一种采用磁性材料作为吸附剂的新型样品前处理技术,发展新型的磁性材料作为吸附剂是MSPE领域的研究热点。用离子液体(Ionic liquid,IL)修饰磁性材料作为吸附剂既具有MSPE操作简单、萃取快速、基质干扰小的优点,又兼具IL结构的可设计性和易功能化的优点,在样品前处理领域引起了广泛关注。该文综述了IL修饰磁性吸附剂的制备方法(物理涂敷、化学键合和包埋法),IL-MSPE的萃取方式(传统的MSPE,混合半胶束-MSPE和分散液液微萃取-MSPE),以及IL-MSPE在有机污染物、金属离子和生物活性物质萃取分离中的应用,并对该技术的发展趋势进行了展望。  相似文献   

2.
通过水热合成法和溶胶凝胶法制备Fe_3O_4@NiSiO_3磁性纳米粒子,该纳米粒子微球具有均一的形貌、良好的磁性和分散性。将合成的Fe_3O_4@NiSiO_3磁性纳米粒子作为磁性固相萃取(MSPE)介质,并结合高效液相色谱(HPLC)建立了水样中痕量微囊藻毒素MC-LR的分析方法。在优化实验条件下,方法在0.25~146.5μg/L浓度范围内呈良好的线性关系,相关系数(r)为0.999 1,检出限为0.011μg/L。将该方法用于纯水中微囊藻毒素的分析,回收率为81.0%,对实际水样的回收率为66.7%~72.0%。表明Fe_3O_4@NiSiO_3磁性纳米粒子具有良好的选择性富集能力,可用于水中痕量微囊藻毒素的萃取。  相似文献   

3.
《色谱》2015,(5)
通过水热合成和常温合成的方法制备了介孔Fe3O4@mSiO2@Cu2+磁性复合纳米粒子(NPs),其具有均匀的尺寸大小、良好的磁性能和特异的选择性。本研究将合成的NPs用作磁性固相萃取(MSPE)介质,结合高效液相色谱(HPLC)发展了一种测定水样品中痕量微囊藻毒素MC-LR的方法。在优化MSPE和HPLC条件后,该方法在0.1~15μg/L范围内呈现良好的线性,线性相关系数(r)为0.999 4,检出限为0.025μg/L,定量限为0.082μg/L。进一步将该方法用于水样中痕量藻毒素分析,结果发现回收率达到78%。这一结果表明:制得的磁性纳米粒子具有良好的萃取性能,可有效用于水样中痕量藻毒素的测定。  相似文献   

4.
采用基于离子液体修饰的类沸石咪唑酯磁性复合纳米材料(IL@M/ZIF-8)的磁性固相萃取(MSPE)前处理技术,结合超高效液相色谱-三重四极杆串联质谱法(UPLC-MS/MS)测定环境水体中痕量微囊藻毒素MC-RR和MC-LR的浓度水平。以扫描电镜和透射电镜对合成材料进行表征,并对UPLC-MS/MS条件和MSPE技术中吸附剂用量、水样pH值、洗脱溶剂的种类、振荡时间等参数进行优化。在最佳条件下,MC-RR和MC-LR分别在0.01~5μg/L和0.05~5μg/L浓度范围内呈良好线性,线性系数(r)分别为0.999 5、0.999 3,检出限分别为1.98、3.94 ng/L,定量下限分别为6.52、12.98 ng/L。将该方法应用于实际水样的测定,加标回收率为88.5%~108%,相对标准偏差为1.5%~7.2%。该方法操作简单,灵敏度高,可用于水样中痕量微囊藻毒素的检测。  相似文献   

5.
制备了一种新型的磁性纳米吸附剂—巯基修饰的Fe3O4@Si O2,并将其用作固相萃取剂从环境水样中富集痕量Hg2+,采用原子荧光分光光度计测定富集后的Hg2+。研究了吸附剂用量、p H、平衡时间、洗脱条件及吸附剂重复使用次数对Hg2+回收率的影响。利用该磁性固相萃取方法建立了标准曲线,并用于测定实际水样中的Hg2+含量。方法的检测限为0.1 ng/L,加标回收率为95%~104%,相对标准偏差0.1%~0.6%。  相似文献   

6.
李迪  张瑞琪  王铁峰  苏萍  杨屹 《色谱》2019,37(3):259-264
采用溶胶-凝胶法制备表面修饰了十八烷基三甲基溴化铵的磁性粒子作为萃取剂,研制了一种在线磁性固相萃取(on-line MSPE)装置,建立了on-line MSPE与高效液相色谱联用测定水样中两种磺酰脲类农药(氯磺隆、苄嘧磺隆)的方法。实验优化了在线磁性固相萃取条件并进行方法学考察,证明该方法具有良好的线性关系(两种目标物的线性相关系数均≥ 0.9997)和较低的检出限(两种目标物的检出限分别为0.32和1.12 μg/L)。将此法用于3种环境水样中两种磺酰脲类农药的检测,水样中均检出氯磺隆,均未检出苄嘧磺隆。两种目标物加标回收率为70.0%~113.4%。该方法高效、简便,在分离富集环境水样中磺酰脲类农药方面有一定的应用前景。  相似文献   

7.
合成了一种由Fe3 O4磁性纳米粒子(MNPs)和多壁碳纳米管(MWCNTs)组成的复合纳米材料,用于水样中16种邻苯二甲酸酯类化合物(PAEs)的磁固相萃取(MSPE),并结合气相色谱-质谱(GC - MS)法进行定量分析.合成的纳米材料用傅立叶变换红外光谱表征.为提高萃取效率,优化了解析溶剂的种类和用量、解析时间、...  相似文献   

8.
以1-(2-吡咯偶氮)-2-萘酚(PAN)为络合剂络合水样中的痕量铜,以磁性石墨烯(G)纳米材料为固相萃取吸附剂,建立了测定水样中痕量铜的磁性固相萃取/火焰原子吸收分光光度法。此方法将磁性石墨烯比表面积大、吸附性能好的优点与Fe3O4纳米粒子的磁性相结合,采用的磁性固相萃取避免了传统固相萃取中离心和过滤等繁琐的操作步骤。对影响G-Fe3O4萃取效率的实验因素进行了优化。在优化实验条件下,对铜离子的富集倍数为80.4倍,线性范围为0.5~100μg/L,相关系数(r)为0.998 1,检出限为0.067μg/L,相对标准偏差为2.1%~5.2%。此方法成功地应用于矿泉水、自来水、公园湖水中铜离子含量的测定,其加标回收率为94%~103%。结果表明,该磁性石墨烯纳米材料G-Fe3O4对水样品中铜的PAN络合物具有较高的富集能力。  相似文献   

9.
魏丹  张菊  国明 《分析测试学报》2022,41(2):187-195
通过制备磁性大孔有机共聚物材料(Fe3O4@SiO2@PLS)和磁性金属有机骨架材料(Fe3O4@ZIF-8),将两种材料同时作为磁性吸附剂,建立了混合吸附剂磁性固相萃取/高效液相色谱-串联质谱(MSPE/HPLC-MS/MS)测定水中4种磺胺类和8种喹诺酮类抗生素残留的分析方法.通过扫描电子显微镜(SEM)、傅里叶变换红外光谱(FT-IR)和X-射线衍射仪(XRD)对两种磁性材料进行表面形貌和结构表征,结果显示,亲水亲脂大孔有机共聚物(PLS)包覆于磁性纳米粒子Fe3O4表面,且Fe3O4成功附着于正六边形金属有机骨架材料(ZIF-8)晶体表面,可以满足磁性固相萃取的要求.通过优化吸附剂用量、萃取方式、吸附时间、样品pH值、洗脱剂种类及洗脱时间,在最优的实验条件下,12种目标物的线性范围为0.5~10μg/L,相关系数(r2)为0.9961~0.9998,检出限(S/N=3)为0.01~0.14μg/L,定量下限(S/N=10)为0.04~0.45μg/L.所建方法成功用于水中12种目标抗生素的检测,在3个加标水平下的回收率为75.0%~107%,相对标准偏差(RSD)为0.50%~5.5%.该方法适用于水中痕量磺胺类和喹诺酮类抗生素残留的分析.  相似文献   

10.
利用水热法合成了Fe_3O_4纳米粒子,并通过巯基-烯点击化学法合成了Fe_3O_4@DA-IL。通过FT-IR、XRD、SEM、TEM等手段对Fe_3O_4@DA-IL进行表征,并以该复合材料为MSPE的吸附剂用于螺旋藻中的PAHs的富集。实验还优化了吸附剂用量、萃取时间、洗脱剂种类以及洗脱次数,在最佳条件下,方法定量限为0.031~0.49μg/L,回收率为78.4%~107.1%。  相似文献   

11.
A new method based on the combination of magnetic solid phase extraction (MSPE) and spectrofluorimetric determination was developed for isolation and preconcentration of fluoxetine form aquatic and biological samples using sodium dodecyl sulfate (SDS) coated Fe(3)O(4) nanoparticles (NPs) as a sorbent. The unique properties of Fe(3)O(4) NPs including high surface area and strong magnetism were utilized effectively in the MSPE process. Effect of different parameters influencing the extraction efficiency of fluoxetine including the amount of Fe(3)O(4) and SDS, pH value, sample volume, extraction time, desorption solvent and time were optimized. Under optimized condition, the method was successfully applied to the extraction of fluoxetine from water and urine samples and absolute recovery amount of 85%, detection limit of 20 μg L(-1) and a relative standard deviation (RSD) of 1.4% were obtained. The method linear response was over a range of 50-1000 μg L(-1) with R(2)=0.9968. The relative recovery in different aquatic and urine matrices were investigated and values of 80% to 104% were obtained. The whole procedure showed to be conveniently fast, efficient and economical for extraction of fluoxetine from environmental and biological samples.  相似文献   

12.
杨华成  咸春颖 《化学研究》2012,23(3):64-67,71
以对叔丁基苯酚为原料,经逐步反应在对叔丁基杯[4]芳烃的下缘引入含卤素的基团,得到了一系列含卤素的杯[4]芳烃衍生物(记为1,2,3,4);利用核磁共振谱和气相色谱-质谱证实了目标产物的结构;并评价了产物对水中的Cr3+、Cu2+、Ag+的萃取性能.结果表明:杯[4]芳烃衍生物2、3和4分别对Cr3+、Cu2+和Ag+具有较好的萃取效果.  相似文献   

13.
A new method based on the combination of magnetic solid phase extraction (MSPE) and spectrofluorimetric determination was developed for isolation and preconcentration of fluoxetine form aquatic and biological samples using sodium dodecyl sulfate (SDS) coated Fe3O4 nanoparticles (NPs) as a sorbent. The unique properties of Fe3O4 NPs including high surface area and strong magnetism were utilized effectively in the MSPE process. Effect of different parameters influencing the extraction efficiency of fluoxetine including the amount of Fe3O4 and SDS, pH value, sample volume, extraction time, desorption solvent and time were optimized. Under optimized condition, the method was successfully applied to the extraction of fluoxetine from water and urine samples and absolute recovery amount of 85%, detection limit of 20 μg L−1 and a relative standard deviation (RSD) of 1.4% were obtained. The method linear response was over a range of 50–1000 μg L−1 with R2 = 0.9968. The relative recovery in different aquatic and urine matrices were investigated and values of 80% to 104% were obtained. The whole procedure showed to be conveniently fast, efficient and economical for extraction of fluoxetine from environmental and biological samples.  相似文献   

14.
In the present study, multi-walled carbon nanotube oxide was immobilized on the pyrrole magnetic nanoparticles. Application of the synthesized material was investigated for the magnetic solid-phase extraction (MSPE) of polycyclic aromatic hydrocarbons (PAHs), from the environmental samples. Determinations of the analytes were performed with gas chromatography–mass spectrometry. The structure and morphology of Fe3O4@PPy–MWCNT were characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, thermal gravimetric analysis, and vibrating sample magnetometer. Performance of MSPE is mainly affected by extraction time, sorbent amount, sample solution volume, and eluent type and volume. In this study, the best possible performance of MSPE has been achieved using a combination of central composite design and Bayesian regularized artificial neural network technique. Under the optimum extraction conditions, linear range between 0.5 and 250 µg L?1 (R 2 > 0.994), preconcentration factors from 232 to 403 and limits of detection ranging from 0.1 to 0.3 µg L?1 were obtained. Relative standard deviations for intra-day and inter-day precision were 3.3–5.1% and 3.7–5.6%, respectively. In addition, feasibility of the method was demonstrated by extraction and determination of PAHs from some real samples containing tap water, hookah water as well as soil samples, and relative recovery in the range of 85.4–106.8% was obtained. This MSPE method provides several advantages, such as high extraction efficiency, minimum sorbent for extraction of the analytes from high sample volumes, convenient extraction procedure, and short analysis times.  相似文献   

15.
A simple and sensitive method was developed for preconcentration and determination of bisphenol A (BPA) in environmental samples by high performance liquid chromatography (HPLC). The hydrophilic silicon-dioxide- and nylon66-functionalised magnetic material (Fe3O4@SiO2@nylon66) was used as a sorbent for magnetic solid-phase extraction (MSPE). With the anhydrous microemulsion reaction, the Fe3O4@SiO2@nylon66 had shown great characteristics such as good magnetic responsivity, water dispersibility and stability. Based on the materials, various extraction parameters including pH, extraction time, elution time, the number of sorbents, sample volume and elution times were optimised. The whole extraction procedure could be accomplished within 20 min and the materials could be used more than 10 times after regeneration. Under the optimised conditions, different types of water samples (Tap water, river water, sea water and underground water) were successfully analysed to verify the applicability of the proposed method. The recoveries of different samples ranged from 88.54% to 104.46%. An enrichment factor of 250 was achieved with 0.05 μg/L detection limit. Thus, the developed MSPE is a potential technique that can be used for water samples preconcentration or combined with other analytical methods for determination of BPA.  相似文献   

16.
A novel magnetic solid-phase extraction (MSPE) sorbent, magnetite/silica/poly (methacrylic acid–co-ethylene glycol dimethacrylate) (Fe3O4/SiO2/P(MAA-co-EGDMA)), was developed. This MSPE material was prepared by distillation–precipitation polymerization of MAA and EGDMA in the presence of Fe3O4/SiO2 microspheres with the surface containing abundant reactive double bonds. The resultant sorbent material was characterized by elemental analysis, electron microscopy, X-ray diffraction and Fourier-transformed infrared spectroscopy. In this work, eleven sulfonamides (SAs) were selected as model analytes to validate the extraction performance of this new MSPE sorbent. Noticeably, the extraction can be carried out quickly, the extraction time for the SAs onto Fe3O4/SiO2/P(MAA-co-EGDMA) sorbent can be clearly shortened to 0.5 min. The desorption solution of SAs was analyzed by LC–MS/MS, and the results showed that the recoveries of these compounds were in the range of 87.6–115.6%, with relative standard deviations ranging between 0.9% and 10.8%; the limit of detection were in the range of 0.5–49.5 ng/L.  相似文献   

17.
This work demonstrates the application of silica supported Fe3O4 nanoparticles as sorbent phase for magnetic solid-phase extraction (MSPE) and magnetic on-line in-tube solid-phase microextraction (Magnetic-IT-SPME) combined with capillary liquid chromatography–diode array detection (CapLC-DAD) to determine organophosphorous compounds (OPs) at trace level. In MSPE, magnetism is used as separation tool while in Magnetic-IT-SPME, the application of an external magnetic field gave rise to a significant improvement of the adsorption of OPs on the sorbent phase. Extraction efficiency, analysis time, reproducibility and sensitivity have been compared. This work showed that Magnetic-IT-SPME can be extended to OPs with successful results in terms of simplicity, speed, extraction efficiency and limit of detection. Finally, wastewater samples were analysed to determine OPs at nanograms per litre.  相似文献   

18.
王盼  马继平  李爽  程嘉雯  邹宗岳 《色谱》2022,40(11):988-997
杀菌剂在环境中长期富集后会引起土壤和植物病害,并能借助雨水或灌溉渗透到深层土壤和地下水中,威胁水体环境和人体健康。因此针对水中杀菌剂开发简单快速、高效灵敏的分析方法至关重要。该研究通过原位合成法制备了磁性共价有机骨架材料Fe3O4@TpBD,将其作为萃取吸附剂,富集环境水体中苯并咪唑杀菌剂(噻菌灵、麦穗宁、多菌灵)和有机硫杀菌剂(稻瘟灵)。利用Fe3O4@TpBD与杀菌剂之间的π-π共轭、氢键和静电作用进行吸附,结合超高效液相色谱-串联质谱法(UHPLC-MS/MS)进行检测,建立了测定水中4种痕量杀菌剂的分析方法。通过透射电子显微镜、X射线衍射及傅里叶变换红外光谱等方式对Fe3O4@TpBD进行表征,以证明材料的成功合成。对萃取条件进行一系列的优化(Fe3O4@TpBD的磁性比例及用量、水样pH、吸附时间、洗脱液的种类及体积、洗脱时间、NaCl含量),确定了最佳萃取条件。4种杀菌剂在3~1200 ng/L的范围内线性关系良好,线性相关系数均大于0.998,方法的检出限和定量限分别为0.06~0.28 ng/L和0.20~0.92 ng/L。在15、150和600 ng/L 3个加标水平下进行加标回收试验,日内和日间精密度分别为2.8%~10.0%和4.4%~15.7%。将该方法用于实际水样的检测,4种杀菌剂的加标回收率为77.1%~119.1%,在水库水中检测出多菌灵,含量为27.5 ng/L。该方法灵敏度高,准确度和精密度良好,操作简单,耗时短。  相似文献   

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