Pub Date : 2025-05-01Epub Date: 2025-03-03DOI: 10.1016/j.sampre.2025.100168
Photini Papaioakeim , Efstathios A. Elia , Agapios Agapiou
Disinfection of drinking water is essential for ensuring public health; however, it leads to the formation of various undesirable disinfection by-products (DBPs). To comply with the recent European Union (EU) drinking water directive legislation (EU 2020/2184), a headspace HiSorb thermal desorption-gas chromatography-mass spectrometry (HS-HiSorb-TD-GC-MS) method was developed and validated for the quantification of 12 DBPs in drinking water. The HS-HiSorb-TD-GC-MS method presented high sensitivity and selectivity, linearity (1–120 ppb), limit of detection (LOD) 0.33–3.33 ppb, and limit of quantification (LOQ) 1–10 ppb. The method's accuracy was verified at three different concentrations, showing good repeatability (intra-day) and reproducibility (inter-day), ranging from 1.3 to 10 % and 3.3–15 %, respectively. Additionally, the method's recovery rates, at 10 ppb and 50 ppb, were estimated between 80 and 120 %. Water sample stability was also examined at various temperatures (4°C, 25°C, -20°C). The HS-HiSorb-TD-GC-MS method was used to investigate the presence of DBPs in tap water samples, highlighting its applicability to drinking water monitoring. The development of a green analytical method based on a sorbent-based sample preparation technique, contributes to sustainable and green analytical chemistry.
{"title":"Monitoring of 12 DBPs in drinking water using a microextraction TD-GC-MS method","authors":"Photini Papaioakeim , Efstathios A. Elia , Agapios Agapiou","doi":"10.1016/j.sampre.2025.100168","DOIUrl":"10.1016/j.sampre.2025.100168","url":null,"abstract":"<div><div>Disinfection of drinking water is essential for ensuring public health; however, it leads to the formation of various undesirable disinfection by-products (DBPs). To comply with the recent European Union (EU) drinking water directive legislation (EU 2020/2184), a headspace HiSorb thermal desorption-gas chromatography-mass spectrometry (HS-HiSorb-TD-GC-MS) method was developed and validated for the quantification of 12 DBPs in drinking water. The HS-HiSorb-TD-GC-MS method presented high sensitivity and selectivity, linearity (1–120 ppb), limit of detection (LOD) 0.33–3.33 ppb, and limit of quantification (LOQ) 1–10 ppb. The method's accuracy was verified at three different concentrations, showing good repeatability (intra-day) and reproducibility (inter-day), ranging from 1.3 to 10 % and 3.3–15 %, respectively. Additionally, the method's recovery rates, at 10 ppb and 50 ppb, were estimated between 80 and 120 %. Water sample stability was also examined at various temperatures (4°C, 25°C, -20°C). The HS-HiSorb-TD-GC-MS method was used to investigate the presence of DBPs in tap water samples, highlighting its applicability to drinking water monitoring. The development of a green analytical method based on a sorbent-based sample preparation technique, contributes to sustainable and green analytical chemistry.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100168"},"PeriodicalIF":5.2,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143592453","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-05-01Epub Date: 2025-04-11DOI: 10.1016/j.sampre.2025.100182
Miryam Perrucci , Erika Maria Ricci , Marcello Locatelli , Imran Ali , Fotou R. Mansour , Abuzar Kabir , Halil I. Ulusoy
The emergence of Green Chemistry (GC), Green Analytical Chemistry (GAC), and Green Sample Preparation (GSP) has significantly influenced the evolution of sample preparation techniques. A central tenet of these approaches is the reduction of sample size, and the minimization of solvent and reagent consumption prior to chromatographic analysis. While these advancements promote sustainability and analytical efficiency, a persistent challenge lies in developing innovative techniques that adhere to these principles without compromising analytical performance-the fundamental goal of analytical chemistry.
In this context, recent advancements in microsampling techniques are gaining increased attention. Techniques such as Solid-Phase Microextraction (SPME) and Volumetric Absorptive Microsampling (VAMS) are being explored as promising tools for obtaining dried biological matrices, such as blood, urine, and saliva offering potential improvements over traditional methods like Dried Blood Spotting (DBS). Moreover, this review discusses recent methods designed to reduce the volume of samples and reagents used in preparation protocols. The primary aim of this review is to explore the latest trends in microsampling and, subsequently, to examine how these methods align with the evolving landscape of green sample preparation.
{"title":"Recent trends in microsampling and reduced-volume sample preparation procedures","authors":"Miryam Perrucci , Erika Maria Ricci , Marcello Locatelli , Imran Ali , Fotou R. Mansour , Abuzar Kabir , Halil I. Ulusoy","doi":"10.1016/j.sampre.2025.100182","DOIUrl":"10.1016/j.sampre.2025.100182","url":null,"abstract":"<div><div>The emergence of Green Chemistry (GC), Green Analytical Chemistry (GAC), and Green Sample Preparation (GSP) has significantly influenced the evolution of sample preparation techniques. A central tenet of these approaches is the reduction of sample size, and the minimization of solvent and reagent consumption prior to chromatographic analysis. While these advancements promote sustainability and analytical efficiency, a persistent challenge lies in developing innovative techniques that adhere to these principles without compromising analytical performance-the fundamental goal of analytical chemistry.</div><div>In this context, recent advancements in microsampling techniques are gaining increased attention. Techniques such as Solid-Phase Microextraction (SPME) and Volumetric Absorptive Microsampling (VAMS) are being explored as promising tools for obtaining dried biological matrices, such as blood, urine, and saliva offering potential improvements over traditional methods like Dried Blood Spotting (DBS). Moreover, this review discusses recent methods designed to reduce the volume of samples and reagents used in preparation protocols. The primary aim of this review is to explore the latest trends in microsampling and, subsequently, to examine how these methods align with the evolving landscape of green sample preparation.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100182"},"PeriodicalIF":5.2,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143829286","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}
Pub Date : 2025-05-01Epub Date: 2025-02-23DOI: 10.1016/j.sampre.2025.100164
Fotouh R. Mansour , Alaa Bedair , Marcello Locatelli
Click analytical chemistry (CAC) is a novel approach inspired by the principles of click chemistry, emphasizing simplicity, efficiency, and reliability. While click chemistry revolutionized synthetic methods, CAC aims to enhance chemical analysis by providing a framework for method assessment from a different perspective, focusing on improving the practicality and applicability of analytical techniques. In this work, we present the Click Analytical Chemistry Index (CACI) as a practical and user-friendly tool that provides both a metric and software solution for evaluating analytical methods. The software is available as an open source at bit.ly/CACI2025. The CACI system allows for objective and unbiased comparisons between techniques, encouraging the development of methods that are easier to implement without sacrificing performance. By promoting simplicity and practicality in method design, CACI supports the development of analytical procedures that not only meet rigorous performance standards but also simplify the analytical process. This work explores the principles and methodology of CAC and presents case studies that demonstrate its practical applications in advancing chemical analysis towards more efficient method development and evaluation.
{"title":"Click Analytical Chemistry Index as a novel concept and framework, supported with open source software to assess analytical methods","authors":"Fotouh R. Mansour , Alaa Bedair , Marcello Locatelli","doi":"10.1016/j.sampre.2025.100164","DOIUrl":"10.1016/j.sampre.2025.100164","url":null,"abstract":"<div><div>Click analytical chemistry (CAC) is a novel approach inspired by the principles of click chemistry, emphasizing simplicity, efficiency, and reliability. While click chemistry revolutionized synthetic methods, CAC aims to enhance chemical analysis by providing a framework for method assessment from a different perspective, focusing on improving the practicality and applicability of analytical techniques. In this work, we present the Click Analytical Chemistry Index (CACI) as a practical and user-friendly tool that provides both a metric and software solution for evaluating analytical methods. The software is available as an open source at <span><span>bit.ly/CACI2025</span><svg><path></path></svg></span>. The CACI system allows for objective and unbiased comparisons between techniques, encouraging the development of methods that are easier to implement without sacrificing performance. By promoting simplicity and practicality in method design, CACI supports the development of analytical procedures that not only meet rigorous performance standards but also simplify the analytical process. This work explores the principles and methodology of CAC and presents case studies that demonstrate its practical applications in advancing chemical analysis towards more efficient method development and evaluation.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100164"},"PeriodicalIF":5.2,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143549844","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
A spherical ordered mesoporous silica functionalized with octadecylsilane ligand (SM-C18) was successfully synthesized and characterized, showing 647 m2/g of surface area, 45 Å of pore size, 4–6 μm of particle diameter and 0.37 mmol/g of functionalization degree. 1.5 mg of SM-C18 were packed into EPREP micro-solid phase extraction (µSPEed) cartridges for use with a handheld programmable digital analytical syringe (digiVOL®) to develop a sample preparation protocol for the analysis of two tropane (TAs) and twenty-one pyrrolizidine (PAs) alkaloids. The SM-C18 demonstrated greater retention capacity compared with commercial C18/hydrophilic amorphous silica sorbent. The optimized extraction conditions were as follows: 100 µL of methanol (2 cycles) and 100 µL of H2O (2 cycles) for conditioning, 100 µL of H2O-reconstituted sample (10 cycles), for a total of 1 mL of sample loaded, and 100 µL of methanol (2 cycles) for elution, followed by subsequent analysis by UHPLC-MS/MS. The method was successfully validated, showing good recoveries ranging between 91 and 97 %, low quantification limits and absence of matrix effect for the twenty-tree alkaloids. Additionally, cartridges packed with SM-C18 material allow for better reusability compared to the commercial material, as it has been demonstrated that they can be used for at least 75 extractions. This significantly enhances the method's sustainability. Finally, it was applied to 25 samples of flower extract supplements (FES). In two different batches of the sample obtained from Convolvulus arvensis flowers (FES4a and FES4b), atropine and scopolamine were quantified.
{"title":"Spherical C18-functionalized ordered mesoporous silica packed on micro-solid phase extraction cartridges for simultaneous determination of twenty-three alkaloids in flower extract supplements","authors":"Begoña Fernández-Pintor , Judith Gañán , Damián Pérez-Quintanilla , Sonia Morante-Zarcero , Isabel Sierra","doi":"10.1016/j.sampre.2025.100174","DOIUrl":"10.1016/j.sampre.2025.100174","url":null,"abstract":"<div><div>A spherical ordered mesoporous silica functionalized with octadecylsilane ligand (SM-C18) was successfully synthesized and characterized, showing 647 m<sup>2</sup>/g of surface area, 45 Å of pore size, 4–6 μm of particle diameter and 0.37 mmol/g of functionalization degree. 1.5 mg of SM-C18 were packed into EPREP micro-solid phase extraction (µSPEed) cartridges for use with a handheld programmable digital analytical syringe (digiVOL®) to develop a sample preparation protocol for the analysis of two tropane (TAs) and twenty-one pyrrolizidine (PAs) alkaloids. The SM-C18 demonstrated greater retention capacity compared with commercial C18/hydrophilic amorphous silica sorbent. The optimized extraction conditions were as follows: 100 µL of methanol (2 cycles) and 100 µL of H<sub>2</sub>O (2 cycles) for conditioning, 100 µL of H<sub>2</sub>O-reconstituted sample (10 cycles), for a total of 1 mL of sample loaded, and 100 µL of methanol (2 cycles) for elution, followed by subsequent analysis by UHPLC-MS/MS. The method was successfully validated, showing good recoveries ranging between 91 and 97 %, low quantification limits and absence of matrix effect for the twenty-tree alkaloids. Additionally, cartridges packed with SM-C18 material allow for better reusability compared to the commercial material, as it has been demonstrated that they can be used for at least 75 extractions. This significantly enhances the method's sustainability. Finally, it was applied to 25 samples of flower extract supplements (FES). In two different batches of the sample obtained from <em>Convolvulus arvensis</em> flowers (FES4a and FES4b), atropine and scopolamine were quantified.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100174"},"PeriodicalIF":5.2,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143629120","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Sustainability is a growing priority in scientific research, and metabolomics is no exception. Traditional metabolomics workflows rely on hazardous solvents, raising concerns regarding their environmental impact. Recent advancements in green analytical chemistry lay the ground for the integration of eco-friendly approaches in metabolomics from matrix collections and pre-treatment, through sample preparation till data analysis. This review explores the current state of sustainable metabolomic workflows, with a particular focus on green sample preparation methods, solvent-free, low-solvent extraction techniques, and energy-efficient instrumental analysis. Computational advancements, including AI-driven models, machine learning-based semi-quantification, and predictive algorithms for solvent selection, further enhance sustainability by reducing resource consumption. The applicability of these approaches in metabolomic studies, particularly in plant and food research is explored. By integrating innovative green methodologies across all stages of metabolomic workflows, researchers can significantly reduce environmental footprints while maintaining analytical rigor.
{"title":"Towards a greener future: The role of sustainable methodologies in metabolomics research","authors":"Chiara Spaggiari , Kgalaletso Othibeng , Fidele Tugizimana , Gabriele Rocchetti , Laura Righetti","doi":"10.1016/j.sampre.2025.100186","DOIUrl":"10.1016/j.sampre.2025.100186","url":null,"abstract":"<div><div>Sustainability is a growing priority in scientific research, and metabolomics is no exception. Traditional metabolomics workflows rely on hazardous solvents, raising concerns regarding their environmental impact. Recent advancements in green analytical chemistry lay the ground for the integration of eco-friendly approaches in metabolomics from matrix collections and pre-treatment, through sample preparation till data analysis. This review explores the current state of sustainable metabolomic workflows, with a particular focus on green sample preparation methods, solvent-free, low-solvent extraction techniques, and energy-efficient instrumental analysis. Computational advancements, including AI-driven models, machine learning-based semi-quantification, and predictive algorithms for solvent selection, further enhance sustainability by reducing resource consumption. The applicability of these approaches in metabolomic studies, particularly in plant and food research is explored. By integrating innovative green methodologies across all stages of metabolomic workflows, researchers can significantly reduce environmental footprints while maintaining analytical rigor<strong>.</strong></div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100186"},"PeriodicalIF":5.2,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143927482","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}
Pub Date : 2025-05-01Epub Date: 2025-04-07DOI: 10.1016/j.sampre.2025.100180
Juan L. Benedé , Cecilia Cagliero , Emirhan Nemutlu , Francisco Pena-Pereira , Carlo Bicchi , Enrique Javier Carrasco-Correa , Maria Celeiro , Alberto Chisvert , Alessandra Gentili , A. Ruth Godfrey , Mehmet Gumustas , Fragoulis Krokos , Paramee Kumkrong , Maria Llompart , Marcello Locatelli , Zoltan Mester , Sibel A. Ozkan , Stig Pedersen-Bjergaard , Marcela A. Segundo , Marek Tobiszewski , Elefteria Psillakis
This work evaluates the greenness of 174 standard methods with a sample preparation step and their 332 sub-method variations from CEN, ISO, and Pharmacopoeias, used in laboratories for environmental/organic, food, trace element, or pharmaceutical analyses. The widely adopted AGREEprep metric was applied to assess the greenness of the standard methods. The discussion begins with the overall scores of each method, followed by a detailed analysis of individual criteria, that highlights the strengths and weaknesses of the evaluated sample preparation methods in terms of greenness.
The results revealed a generally poor greenness performance, as 67 % of the methods scored below 0.2 on the AGREEprep scale, where 1 represents the highest possible score. Specifically, the percentage of methods scoring below 0.2 was 86 % for methods related to the environmental analysis of organic compounds, 62 % for methods used in food analysis, 62 % for those applied to inorganic and trace metals analysis, and 45 % for methods used in pharmaceutical analysis. The findings obtained in this work reveal that many official methods still rely on resource-intensive, outdated techniques, scoring poorly on key greenness criteria. This discrepancy highlights the urgent need to update standard methods by including contemporary and mature sample preparation methods, as the traditional methodologies currently used often conflict with global sustainability efforts and increase regulatory and societal pressures. As such, this contribution serves not only as a critique of the current state of official standard methods but also as a call to action for their reform. This work was conducted within the framework of the IUPAC project "Greenness of official standard sample preparation methods" (2021-015-2-500).
{"title":"Greenness assessment of 174 CEN, ISO, and pharmacopoeia standard methods and their sub-methods used for environmental, food, trace element and pharmaceutical analyses","authors":"Juan L. Benedé , Cecilia Cagliero , Emirhan Nemutlu , Francisco Pena-Pereira , Carlo Bicchi , Enrique Javier Carrasco-Correa , Maria Celeiro , Alberto Chisvert , Alessandra Gentili , A. Ruth Godfrey , Mehmet Gumustas , Fragoulis Krokos , Paramee Kumkrong , Maria Llompart , Marcello Locatelli , Zoltan Mester , Sibel A. Ozkan , Stig Pedersen-Bjergaard , Marcela A. Segundo , Marek Tobiszewski , Elefteria Psillakis","doi":"10.1016/j.sampre.2025.100180","DOIUrl":"10.1016/j.sampre.2025.100180","url":null,"abstract":"<div><div>This work evaluates the greenness of 174 standard methods with a sample preparation step and their 332 sub-method variations from CEN, ISO, and Pharmacopoeias, used in laboratories for environmental/organic, food, trace element, or pharmaceutical analyses. The widely adopted AGREEprep metric was applied to assess the greenness of the standard methods. The discussion begins with the overall scores of each method, followed by a detailed analysis of individual criteria, that highlights the strengths and weaknesses of the evaluated sample preparation methods in terms of greenness.</div><div>The results revealed a generally poor greenness performance, as 67 % of the methods scored below 0.2 on the AGREEprep scale, where 1 represents the highest possible score. Specifically, the percentage of methods scoring below 0.2 was 86 % for methods related to the environmental analysis of organic compounds, 62 % for methods used in food analysis, 62 % for those applied to inorganic and trace metals analysis, and 45 % for methods used in pharmaceutical analysis. The findings obtained in this work reveal that many official methods still rely on resource-intensive, outdated techniques, scoring poorly on key greenness criteria. This discrepancy highlights the urgent need to update standard methods by including contemporary and mature sample preparation methods, as the traditional methodologies currently used often conflict with global sustainability efforts and increase regulatory and societal pressures. As such, this contribution serves not only as a critique of the current state of official standard methods but also as a call to action for their reform. This work was conducted within the framework of the IUPAC project \"Greenness of official standard sample preparation methods\" (2021-015-2-500).</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100180"},"PeriodicalIF":5.2,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143835036","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}
Pub Date : 2025-05-01Epub Date: 2025-04-28DOI: 10.1016/j.sampre.2025.100185
Ana Isabel García-Valcárcel, Esther Miguel, Antonio Martín-Esteban
In recent years, natural deep eutectic solvents (NADES) have been proposed as sustainable solvents capable of replacing the conventional harmful organic solvents typically used in sample preparation. In this regard, in this work, several NADES have been evaluated for the development of a matrix solid phase dispersion - ultrasound-assisted extraction (MSPD-UAE) method for selected pesticides (thiamethoxam, thiacloprid, pirimicarb, acetamiprid and tebuconazole) from pear (peel and pulp) samples and final determination by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Among the different NADES and dispersants tested, the one consisting of choline chloride:1,3-propanediol in a 1:4 molar ratio combined with alumina showed the best performance. The effect of the amount of dispersant, the volume of NADES, the temperature of the ultrasonic bath and the duration of sonication was then optimised using response surface methodology (RSM) based on a four-factor, three-level Box-Behnken design. Under optimal conditions, no matrix effect was observed and quantitative recoveries, ranging from 78.5 to 120 % with relative standard deviations (RSDs) lower than 20 % were obtained, reaching limits of quantification within the range 4–10 ng g-1, depending upon the analyte. In addition, after evaluation by Analytical Greenness Metric for Sample Preparation (AGREEprep), Sample Preparation Metric of Sustainability (SPMS) and Blue Applicability Grade Index (BAGI) metrics tools, the proposed method was found to be superior to other published methods in terms of safety and environmental impact with good applicability potential.
近年来，天然深共晶溶剂（NADES）被认为是一种可持续溶剂，能够取代传统的有害有机溶剂，通常用于样品制备。在这方面，本研究对几种NADES进行了评价，以建立基质固相分散-超声辅助提取（MSPD-UAE）方法，用于从梨（果皮和果肉）样品中提取农药（噻虫嗪、噻虫啉、吡虫威、啶虫啉和戊唑唑），并通过液相色谱-串联质谱（LC-MS/MS）进行最终测定。在不同的NADES和分散剂中，氯化胆碱：1,3-丙二醇以1:4的摩尔比与氧化铝复合的NADES和分散剂表现出最好的性能。然后利用响应面法（RSM），基于四因素、三级Box-Behnken设计，优化分散剂用量、NADES体积、超声浴温度和超声持续时间的影响。在最佳条件下，未观察到基质效应，定量回收率为78.5% ~ 120%，相对标准偏差（rsd）小于20%，根据分析物的不同，定量限在4 ~ 10 ng g-1。此外，通过对样品制备分析绿色度指标（AGREEprep）、可持续性样品制备指标（SPMS）和蓝色适用性等级指数（BAGI）指标工具的评价，发现该方法在安全性和环境影响方面优于其他已发表的方法，具有良好的适用性潜力。
{"title":"Natural deep eutectic solvent-based matrix solid-phase dispersion-ultrasound assisted extraction of pesticides in pears and their determination by liquid chromatography-tandem mass spectrometry","authors":"Ana Isabel García-Valcárcel, Esther Miguel, Antonio Martín-Esteban","doi":"10.1016/j.sampre.2025.100185","DOIUrl":"10.1016/j.sampre.2025.100185","url":null,"abstract":"<div><div>In recent years, natural deep eutectic solvents (NADES) have been proposed as sustainable solvents capable of replacing the conventional harmful organic solvents typically used in sample preparation. In this regard, in this work, several NADES have been evaluated for the development of a matrix solid phase dispersion - ultrasound-assisted extraction (MSPD-UAE) method for selected pesticides (thiamethoxam, thiacloprid, pirimicarb, acetamiprid and tebuconazole) from pear (peel and pulp) samples and final determination by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Among the different NADES and dispersants tested, the one consisting of choline chloride:1,3-propanediol in a 1:4 molar ratio combined with alumina showed the best performance. The effect of the amount of dispersant, the volume of NADES, the temperature of the ultrasonic bath and the duration of sonication was then optimised using response surface methodology (RSM) based on a four-factor, three-level Box-Behnken design. Under optimal conditions, no matrix effect was observed and quantitative recoveries, ranging from 78.5 to 120 % with relative standard deviations (RSDs) lower than 20 % were obtained, reaching limits of quantification within the range 4–10 ng g<sup>-1</sup>, depending upon the analyte. In addition, after evaluation by Analytical Greenness Metric for Sample Preparation (AGREEprep), Sample Preparation Metric of Sustainability (SPMS) and Blue Applicability Grade Index (BAGI) metrics tools, the proposed method was found to be superior to other published methods in terms of safety and environmental impact with good applicability potential.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100185"},"PeriodicalIF":5.2,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143891022","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}
Pub Date : 2025-05-01Epub Date: 2025-03-02DOI: 10.1016/j.sampre.2025.100167
Mariusz Marć , A. Martín-Esteban
It is now widely accepted that the incorporation of molecularly imprinted polymers (MIPs) into sample preparation techniques has enabled unprecedented selectivity performance of analytical methods for the determination of a wide range of analytes in biological, food and environmental samples. However, according to the Principles of Green Chemistry and the subsequent Principles of Green Sample Preparation, it is clear that MIPs are far from being considered green materials, both due to the common harmful reagents and the experimental conditions used for their synthesis. Accordingly, new greener routes for MIP synthesis have been proposed in recent years. However, although the titles of some of the published papers include terms such as 'green MIP' or 'sustainable MIP', such improved properties have only been assessed intuitively and it is therefore unclear whether such claimed green or sustainable MIPs are actually so. Therefore, in the present review, published papers using apparently green MIPs in sample preparation were evaluated using the recently developed metric tool AGREEMIP. Such a tool is based on the assessment of 12 criteria related to the greenness of the different reagents used, energy requirements and other aspects of MIP synthesis procedures. The final values of performed AGREEMIP assessment ranged from 0.28 to 0.80. The scores obtained after the AGREEMIP assessment clearly show that, although slight improvements have been achieved in terms of greenness, there is an abuse of the use of green-related terms and further development is needed. In this context, some guidelines for greening MIPs are provided.
{"title":"Assessment of the greenness of molecularly imprinted polymers used in sample preparation","authors":"Mariusz Marć , A. Martín-Esteban","doi":"10.1016/j.sampre.2025.100167","DOIUrl":"10.1016/j.sampre.2025.100167","url":null,"abstract":"<div><div>It is now widely accepted that the incorporation of molecularly imprinted polymers (MIPs) into sample preparation techniques has enabled unprecedented selectivity performance of analytical methods for the determination of a wide range of analytes in biological, food and environmental samples. However, according to the Principles of Green Chemistry and the subsequent Principles of Green Sample Preparation, it is clear that MIPs are far from being considered green materials, both due to the common harmful reagents and the experimental conditions used for their synthesis. Accordingly, new greener routes for MIP synthesis have been proposed in recent years. However, although the titles of some of the published papers include terms such as 'green MIP' or 'sustainable MIP', such improved properties have only been assessed intuitively and it is therefore unclear whether such claimed green or sustainable MIPs are actually so. Therefore, in the present review, published papers using apparently green MIPs in sample preparation were evaluated using the recently developed metric tool AGREEMIP. Such a tool is based on the assessment of 12 criteria related to the greenness of the different reagents used, energy requirements and other aspects of MIP synthesis procedures. The final values of performed AGREEMIP assessment ranged from 0.28 to 0.80. The scores obtained after the AGREEMIP assessment clearly show that, although slight improvements have been achieved in terms of greenness, there is an abuse of the use of green-related terms and further development is needed. In this context, some guidelines for greening MIPs are provided.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100167"},"PeriodicalIF":5.2,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143561856","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-05-01Epub Date: 2025-04-10DOI: 10.1016/j.sampre.2025.100181
Nur Fitrah Abdullah Sani , Rico Ramadhan , Noorfatimah Yahaya , Siti Maisharah Sheikh Ghadzi , Ahmad Husaini Mohamed , Sazlinda Kamaruzaman , Wan Nazihah Wan Ibrahim , Nor Suhaila Mohamad Hanapi , Nur Nadhirah Mohamad Zain
Deep eutectic solvents have emerged as a sustainable alternative to conventional organic solvents and ionic liquids, offering advantages such as low toxicity, biodegradability, and cost-effectiveness. Their integration into membrane-based systems has revolutionized extraction, separation, and preconcentration techniques, particularly for organic compounds in aqueous matrices. This review provides a comprehensive analysis of deep eutectic solvent-based membranes, focusing on their classifications, preparation methods, and fabrication strategies. The application of different types of deep eutectic solvent-based membranes is critically evaluated. Special attention is given to the optimization of extraction parameters, and mechanisms governing analyte-membrane interactions. While deep eutectic solvent-based membranes demonstrate significant potential for enhanced selectivity, enrichment, and recovery, challenges such as membrane stability, scalability, and compatibility with analytical instrumentation remain. Addressing these limitations through advanced material engineering and process optimization will be crucial for broader adoption. This review highlights recent advancements, identifies research gaps, and outlines future perspectives to enhance the applicability of deep eutectic solvent-based membranes in analytical and environmental sciences.
{"title":"Advancements in deep eutectic solvent-based membranes for the extraction, separation, and preconcentration of organic compounds","authors":"Nur Fitrah Abdullah Sani , Rico Ramadhan , Noorfatimah Yahaya , Siti Maisharah Sheikh Ghadzi , Ahmad Husaini Mohamed , Sazlinda Kamaruzaman , Wan Nazihah Wan Ibrahim , Nor Suhaila Mohamad Hanapi , Nur Nadhirah Mohamad Zain","doi":"10.1016/j.sampre.2025.100181","DOIUrl":"10.1016/j.sampre.2025.100181","url":null,"abstract":"<div><div>Deep eutectic solvents have emerged as a sustainable alternative to conventional organic solvents and ionic liquids, offering advantages such as low toxicity, biodegradability, and cost-effectiveness. Their integration into membrane-based systems has revolutionized extraction, separation, and preconcentration techniques, particularly for organic compounds in aqueous matrices. This review provides a comprehensive analysis of deep eutectic solvent-based membranes, focusing on their classifications, preparation methods, and fabrication strategies. The application of different types of deep eutectic solvent-based membranes is critically evaluated. Special attention is given to the optimization of extraction parameters, and mechanisms governing analyte-membrane interactions. While deep eutectic solvent-based membranes demonstrate significant potential for enhanced selectivity, enrichment, and recovery, challenges such as membrane stability, scalability, and compatibility with analytical instrumentation remain. Addressing these limitations through advanced material engineering and process optimization will be crucial for broader adoption. This review highlights recent advancements, identifies research gaps, and outlines future perspectives to enhance the applicability of deep eutectic solvent-based membranes in analytical and environmental sciences.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100181"},"PeriodicalIF":5.2,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143829285","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}
Pub Date : 2025-05-01Epub Date: 2025-03-07DOI: 10.1016/j.sampre.2025.100172
Mussab Uddin , Faizah Mohammad Yunus , Zaharaddeen Muhammad , Muggundha Raoov , Andrew William King , Waleed Alahmad , Sibel A. Ozkan
The emergence of antibiotic contamination in food, water, and environmental matrices has necessitated the development of efficient, sensitive, and environmentally sustainable analytical methods. Deep eutectic solvents (DESs) have attracted significant attention as green alternatives to conventional solvents owing to their tunable properties, low toxicity, and biodegradability. This review comprehensively explores recent advancements in DES-based microextraction techniques for antibiotic detection, including solid-phase microextraction, liquid-liquid microextraction, and vortex-assisted approaches. Integration with cutting-edge analytical instruments, such as high-performance liquid chromatography with mass spectrometry and ion-mobility spectrometry, has enhanced the selectivity and sensitivity of trace-level antibiotics.
Key challenges, such as DES viscosity and scalability, were critically examined alongside emerging solutions, including novel DES formulations and functional additives for improved extraction efficiency. This review underscores the role of DES-based microextraction in facilitating greener analytical practices, and highlights its potential for broader applications in environmental monitoring, pharmaceutical residue analysis, and food safety. By identifying the current limitations and offering strategies for future research, this review provides a valuable resource for advancing sustainable antibiotic extraction approaches.
{"title":"Advances in microextraction techniques utilizing deep eutectic solvents for the extraction of antibiotics","authors":"Mussab Uddin , Faizah Mohammad Yunus , Zaharaddeen Muhammad , Muggundha Raoov , Andrew William King , Waleed Alahmad , Sibel A. Ozkan","doi":"10.1016/j.sampre.2025.100172","DOIUrl":"10.1016/j.sampre.2025.100172","url":null,"abstract":"<div><div>The emergence of antibiotic contamination in food, water, and environmental matrices has necessitated the development of efficient, sensitive, and environmentally sustainable analytical methods. Deep eutectic solvents (DESs) have attracted significant attention as green alternatives to conventional solvents owing to their tunable properties, low toxicity, and biodegradability. This review comprehensively explores recent advancements in DES-based microextraction techniques for antibiotic detection, including solid-phase microextraction, liquid-liquid microextraction, and vortex-assisted approaches. Integration with cutting-edge analytical instruments, such as high-performance liquid chromatography with mass spectrometry and ion-mobility spectrometry, has enhanced the selectivity and sensitivity of trace-level antibiotics.</div><div>Key challenges, such as DES viscosity and scalability, were critically examined alongside emerging solutions, including novel DES formulations and functional additives for improved extraction efficiency. This review underscores the role of DES-based microextraction in facilitating greener analytical practices, and highlights its potential for broader applications in environmental monitoring, pharmaceutical residue analysis, and food safety. By identifying the current limitations and offering strategies for future research, this review provides a valuable resource for advancing sustainable antibiotic extraction approaches.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100172"},"PeriodicalIF":5.2,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143577967","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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