Advances in Sample Preparation最新文献_第6页

Synthesis and modification of MIL-101-NH2-based metal organic frameworks for preparation of SPME fibers using sol-gel methodology 溶胶-凝胶法制备SPME纤维用mil -101- nh2基金属有机骨架的合成与改性

Advances in Sample Preparation Pub Date : 2023-08-01 DOI: 10.1016/j.sampre.2023.100075

Hasan Javanmardi , Mahsa Doosti , Alireza Abbasi , Habib Bagheri

{"title":"Synthesis and modification of MIL-101-NH2-based metal organic frameworks for preparation of SPME fibers using sol-gel methodology","authors":"Hasan Javanmardi , Mahsa Doosti , Alireza Abbasi , Habib Bagheri","doi":"10.1016/j.sampre.2023.100075","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100075","url":null,"abstract":"<div>Implementation of metal-organic frameworks (MOFs) in the separation science is attractive for many researchers, nowadays. In this study, three MOFs were synthesized and employed as extractive coating fibers. The MIL-101-NH2-based coatings were implemented in immersed solid phase microextraction (ISPME) of organophosphorus pesticides (OPPs) from real-life samples. The three different kinds of fiber coatings included MIL-101-NH2 and its acyl and ethyl modified structures as particles and 3-aminopropyl triethoxysilane (APTES) sol-gel precursor as binder. Each single MOF was coated on a stainless steel substrate via sol-gel technique. The uniform and tunable pore structure, high surface area, and capability to functionalization of MIL-101-NH2, make it susceptible for isolation of a wide range of analytes from small to large molecules. Extraction performance of the synthesized fiber coatings with different functionalities was examined on some model OPPs, followed by gas chromatography-mass spectrometry (GC–MS). The highest extraction efficiency was achieved by the acyl-modified (MIL-101-NH<img>COCH3) fiber coating. The effects of various parameters affecting the extraction and desorption efficiency such as desorption time, desorption temperature, ionic strength, stirring rate, extraction time and temperature for the selected fiber were investigated and optimized. All the synthesized fiber coatings showed sufficient affinity while the acyl modified extractive phase was found to be very sensitive for determination of OPPs with reliable figures of merit such as acceptable linear dynamic ranges (1–1000 & 5–1000 ng.kg−1, here two linear dynamic ranges (LDR) are reported due to the variation of LDR ranges from one analyte to another), low limits of detection (0.2–1 ng.kg−1), suitable intra–day (RSD% <13%) and inter–day relative standard deviation (RSD% <15%).</div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"7 ","pages":"Article 100075"},"PeriodicalIF":0.0,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49750838","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 1

Quality by design approach with design of experiment for sample preparation techniques 样品制备技术的质量设计方法和实验设计

Advances in Sample Preparation Pub Date : 2023-08-01 DOI: 10.1016/j.sampre.2023.100079

Saniye Özcan , Serkan Levent , Nafiz Öncü Can

引用次数: 0

Supramolecular solvents for multi-target and matrix-independent sample preparation 用于多靶点和基质无关样品制备的超分子溶剂

Advances in Sample Preparation Pub Date : 2023-08-01 DOI: 10.1016/j.sampre.2023.100085

Ana Ballesteros-Gómez, Soledad Rubio

引用次数: 1

Green sample preparation 2023 绿色样品制备2023

Advances in Sample Preparation Pub Date : 2023-08-01 DOI: 10.1016/j.sampre.2023.100087

Francisco Pena-Pereira , Verónica Pino , Marek Tobiszewski , Lorena Vidal

引用次数: 0

Application of a homemade silica-based mixed-mode ion-exchange sorbent for the determination of drugs in environmental water samples 自制硅基混合模式离子交换吸附剂在环境水样中药物测定中的应用

Advances in Sample Preparation Pub Date : 2023-08-01 DOI: 10.1016/j.sampre.2023.100074

Alberto Moral , Pol Clivillé-Cabré , Francesc Borrull , Kenneth G. Furton , Abuzar Kabir , Rosa Maria Marcé , Núria Fontanals

{"title":"Application of a homemade silica-based mixed-mode ion-exchange sorbent for the determination of drugs in environmental water samples","authors":"Alberto Moral , Pol Clivillé-Cabré , Francesc Borrull , Kenneth G. Furton , Abuzar Kabir , Rosa Maria Marcé , Núria Fontanals","doi":"10.1016/j.sampre.2023.100074","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100074","url":null,"abstract":"<div>Two homemade silica-based mixed-mode ion-exchange sorbents with strong moieties were compared for the solid-phase extraction (SPE) of a group of pharmaceuticals, drugs of abuse and metabolites. The difference between sorbents was the presence of graphene microparticles embedded in the network and the best results were obtained with the sorbent that did not contain graphene.The optimum SPE protocol of the non-graphene sorbent was: loading pH at 3, different loading volumes depending on the type of sample, 2 mL of MeOH as washing solvent.The optimized method was validated for the analysis of water samples of environmental interest (river water, effluent wastewater and influent wastewater). Apparent recoveries ranged from 22 to 68%, matrix effect values were lower than ±20 for most compounds, and method detection limits ranged from 1 to 28 ng/L and method quantification limits from 2 to 56 ng/L. Precision was obtained as percentual relative standard deviation (RSD%, n=4) and the repeatability and reproducibility between days were always lower than 18%.The sorbent was used to determine the analytes in environmental water samples, where most compounds were found in the range from 2 to 180 ng/L in river samples, from 3 to 2547 ng/L in effluent wastewater samples and from 24 to 8086 ng/L in influent wastewater samples.</div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"7 ","pages":"Article 100074"},"PeriodicalIF":0.0,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49750575","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 2

Synergistic combination of natural deep eutectic solvent and chemical vapor generation for trace determination of As, Cd, Hg and Pb in drug samples by inductively coupled plasma optical emission spectrometry 电感耦合等离子体发射光谱法测定药物样品中痕量As、Cd、Hg和Pb

Advances in Sample Preparation Pub Date : 2023-08-01 DOI: 10.1016/j.sampre.2023.100084

Sergio J. Abellán-Martín , Jorge Pérez , Fernanda C. Pinheiro , Joaquim A. Nóbrega , Miguel Ángel Aguirre , Lorena Vidal , Antonio Canals

{"title":"Synergistic combination of natural deep eutectic solvent and chemical vapor generation for trace determination of As, Cd, Hg and Pb in drug samples by inductively coupled plasma optical emission spectrometry","authors":"Sergio J. Abellán-Martín , Jorge Pérez , Fernanda C. Pinheiro , Joaquim A. Nóbrega , Miguel Ángel Aguirre , Lorena Vidal , Antonio Canals","doi":"10.1016/j.sampre.2023.100084","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100084","url":null,"abstract":"<div>A new and environmentally friendly analytical method for simultaneous determination of As, Cd, Hg and Pb in drug samples by inductively coupled plasma optical emission spectrometry (ICP OES) has been developed. In order to increase the sensitivity of the analysis, a multinebulizer has been used for chemical vapor generation (CVG) after a dispersive liquid-liquid microextraction (DLLME) procedure using a natural deep eutectic solvent (NADES) as extractant solvent. The factors affecting analyte extraction and on-line chemical vapor generation have been optimized by multivariate analysis. Under optimized conditions, DLLME-CVG-ICP OES improved limit of quantitation (LOQ) values on average 50-fold higher compared with direct ICP OES analysis and afforded an increase of the sensitivity (i.e., enrichment factor) on average 25-times higher than those obtained with CVG-ICP OES analysis. According to the United States Pharmacopoeia (USP) Chapter 232, it means LOQ values are on average 4.3-times lower than their respective 0.3J values for the target-elements from class 1. Trueness has been evaluated by recovery experiments following USP recommendations for two oral drug samples in solid dosage form (i.e., commercial dosage tablets). In addition, the greenness of the developed method has been evaluated using the AGREEprep metrics, showing an excellent green character since it includes the miniaturization of the sample preparation procedure using a reduced volume (i.e., few microliters) of a non-hazardous extractant solvent for multielemental analysis.</div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"7 ","pages":"Article 100084"},"PeriodicalIF":0.0,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49750702","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 1

Green fat removal in the analysis of polychlorinated biphenyls in biotic samples 生物样品中多氯联苯分析中的绿色脂肪去除

Advances in Sample Preparation Pub Date : 2023-08-01 DOI: 10.1016/j.sampre.2023.100081

J. Bintanel-Cenis, L. Herrero, B. Gómara, L. Ramos

{"title":"Green fat removal in the analysis of polychlorinated biphenyls in biotic samples","authors":"J. Bintanel-Cenis, L. Herrero, B. Gómara, L. Ramos","doi":"10.1016/j.sampre.2023.100081","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100081","url":null,"abstract":"<div>A green analytical method based on the use of a deep eutectic solvent (DES) has been proposed for fat removal in the analysis of polychlorinated biphenyl (PCBs) in biotic samples. Using priority PCB congeners as model compounds, a novel sample preparation approach fully avoiding the use of mineral acids has been developed. Once optimized, the procedure allowed fat removal to be accomplished by 30min treatment with [chlorine chloride]:[oxalic acid dihydrated] 1:1 molar ratio at 60°C, with 3s vortexing every 5min to facilitate the homogenization of the slurry. Then, the target PCBs were recovered from the slurry by 20min extraction with 4mL of n-hexane. This DES-based method was combined with gas chromatography-quadrupole mass spectrometry (GC-qMS) for final PCB determination. The complete analytical method provided satisfactory recoveries of the target compounds (above 87% for all analytes), using as a small amount of sample as 0.150g. The repeatability of the complete procedure, expressed as relative standard deviation, was less than 5%, and the intermediate precision better than 14%. Final validation of the proposed methodology included the satisfactory comparison of the concentrations calculated for the endogenous PCBs in selected fatty foodstuffs with lipid contents under 18% (w/w fresh weight, fw) with those found when the same samples were analyzed by a more conventional and accepted reference procedure. The limits of detection were in all cases lower than 30 pg/g fw (as calculated for real samples), demonstrating the feasibility of the proposed procedure for accurate determination of the target compounds in biotic samples.</div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"7 ","pages":"Article 100081"},"PeriodicalIF":0.0,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49758870","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 1

Capillary electrophoresis instrumentation for determination of viscosity of deep eutectic solvents 测定深共晶溶剂粘度的毛细管电泳仪器

Advances in Sample Preparation Pub Date : 2023-08-01 DOI: 10.1016/j.sampre.2023.100086

Angel Puerta, Paula Tejedor-Matellanes, Inmaculada Luque-Jurado, Cristian Gonzalez-Jimenez, Ana Cristina Soria, Mercedes de Frutos

{"title":"Capillary electrophoresis instrumentation for determination of viscosity of deep eutectic solvents","authors":"Angel Puerta, Paula Tejedor-Matellanes, Inmaculada Luque-Jurado, Cristian Gonzalez-Jimenez, Ana Cristina Soria, Mercedes de Frutos","doi":"10.1016/j.sampre.2023.100086","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100086","url":null,"abstract":"<div>Deep eutectic solvents (DES), and especially natural deep eutectic solvents (NADES), are advantageous alternatives over non-environmentally friendly organic solvents traditionally employed for sample preparation in analytical chemistry. Moreover, the use of DES has recently experienced remarkable growth to fulfill the green analytical chemistry principles. One of their most influential characteristics, which should be determined for each new DES, is viscosity. Manual or automatic viscometers are usually employed to this aim, but their use is sometimes hampered by characteristics of DES such as their variable water content or their wide viscosity range. In this study a proof-of-concept of the feasibility of employing a capillary electrophoresis (CE) instrument to determine this physicochemical property is shown. No change in the commercial instrument is required, and advantages such as applying controlled pressure and temperature, online UV detection at several wavelengths, use of extremely low volumes of solvents and viscosity markers, automation, etc., allow the easy and affordable adaptation of this method to different DES. As example of application, CE methods were used for viscosity measurement of ten different DES, including hydrophilic (based on either choline chloride or betaine) and hydrophobic ones (based on thymol), within two orders of magnitude (6 to 500 mPa⋅s). Agreement between the experimental results obtained with the CE instrument and data gathered by a commercial viscometer adequate for solvents without water or with published data (when available), is shown. Contribution of using DES to the green analytical chemistry principles is reinforced by the characterization for the first time of these solvents with the more sustainable and high applicability CE method here proposed.</div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"7 ","pages":"Article 100086"},"PeriodicalIF":0.0,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49767317","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 1

Dispersive magnetic solid-phase extraction for synthetic PDE-5 inhibitors determination by high-performance liquid chromatography with tandem mass spectrometry 色散磁固相萃取合成PDE-5抑制剂的高效液相色谱串联质谱测定

Advances in Sample Preparation Pub Date : 2023-08-01 DOI: 10.1016/j.sampre.2023.100071

Ainhoa Oller-Ruiz , Natalia Campillo , José Fenoll , Manuel Hernández-Córdoba , Pilar Viñas

{"title":"Dispersive magnetic solid-phase extraction for synthetic PDE-5 inhibitors determination by high-performance liquid chromatography with tandem mass spectrometry","authors":"Ainhoa Oller-Ruiz , Natalia Campillo , José Fenoll , Manuel Hernández-Córdoba , Pilar Viñas","doi":"10.1016/j.sampre.2023.100071","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100071","url":null,"abstract":"<div>A dispersive magnetic solid-phase extraction (DMPSE) procedure has been developed to preconcentrate four synthetic phosphodiesterase type 5 (PDE-5) inhibitors (sildenafil, desmethylsildenafil, vardenafil and tadalafil) from different samples (human hair, energy drinks, lubricating gels and dietary supplements). The target compounds were isolated from the solid samples by solid-liquid extraction in basic aqueous medium and the extract was submitted to DMSPE using multiwalled carbon nanotubes/Fe3O4@polypyrrole (MWCNTs/Fe3O4@PPy). For this, 20 mg of the magnetic nanocomposite was added to 30 mL of sample solution/extract and vortexed for 10 min before proceeding to the desorption step using 1 mL of methanol. Analysis was carried out by liquid chromatography with tandem mass spectrometry using electrospray ionization and a triple quadrupole mass analyzer (LC-ESI-QqQ-MS/MS). Matrix-matched calibration was applied for quantification. Limits of detection ranged between 0.01 and 0.22 ng mL−1 for energy drinks and between 0.25 and 7.5 ng g−1 for hair, lubricating gels, and dietary supplements. Relative standard deviations in the 4.3–12.2% (n = 10) were obtained for repeatability studies. The trueness of the proposed method was studied by fortifying the samples at two concentration levels and recoveries in the 85–112% range were obtained. None of the PDE-5 inhibitors studied were detected in real samples.</div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"7 ","pages":"Article 100071"},"PeriodicalIF":0.0,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49750630","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 1

Synthesis of amphiphilic magnetic nanoparticles for highly efficient enrichment of steroid hormones in aquatic environment 两亲性磁性纳米颗粒在水生环境中高效富集类固醇激素的合成

Advances in Sample Preparation Pub Date : 2023-08-01 DOI: 10.1016/j.sampre.2023.100078

Hao-Dong Wang , Nian Li , Jia-Hui Zhao , Bo Liu , Ning-Lan Xiao , Miao Zhang , Qiang Li , Hua-Jie Lai

{"title":"Synthesis of amphiphilic magnetic nanoparticles for highly efficient enrichment of steroid hormones in aquatic environment","authors":"Hao-Dong Wang , Nian Li , Jia-Hui Zhao , Bo Liu , Ning-Lan Xiao , Miao Zhang , Qiang Li , Hua-Jie Lai","doi":"10.1016/j.sampre.2023.100078","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100078","url":null,"abstract":"<div>The steroid hormones in the aquatic environment have attracted widespread attentions due to their harmful effects to organisms. In order to improve the sensitivity and accuracy of steroid hormone detection, amphiphilic magnetic nanoparticles (AMNPs) were prepared through suspension copolymerization for microSPE of steroid hormones in water. The divinylbenzene and N-vinylpyrrolidone were selected as modified monomers, and Fe3O4 as the magnetic core. The FT-IR and SEM analyses showed that amphiphilic modified polymers were successfully coated on the surface of Fe3O4 magnetic beads. The hysteresis loop showed that the saturation magnetization value of obtained AMNPs was 36 emu·g−1. In the adsorption test, the adsorption rate of nine steroid hormones by AMNPs can reach more than 90%. Based on this, an AMNPs-microSPE coupled with HPLC-MS/MS method was established to detect steroid hormones in the aquatic environment. The detection limit and quantitation limit of this analytical method was 0.01–0.72 μg·L−1 and 0.10–2.4 μg·L−1 respectively, with good linear fit and low relative standard deviation. The prepared AMNPs extraction materials show good recovery and reproducibility for steroid hormones in water, and have the advantages of low price, easy availability and reusable.</div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"7 ","pages":"Article 100078"},"PeriodicalIF":0.0,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49758867","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0