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Sample Preparation-Quo Vadis: Current Status of Sample Preparation Approaches—3rd Edition
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Sample Preparation-Quo Vadis: Current Status of Sample Preparation Approaches—3rd Edition

A special issue of Molecules (ISSN 1420-3049). This special issue belongs to the section "Analytical Chemistry".

Deadline for manuscript submissions: 31 May 2025 | Viewed by 12582

Special Issue Editors

Prof. Dr. Victoria Samanidou

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Guest Editor
Laboratory of Analytical Chemistry, School of Chemistry, Aristotle University of Thessaloniki, 54124 Thessaloniki, Greece
Interests: analytical chemistry; sample preparation; chromatography; HPLC; method validation; method development; separation science; food analysis; bioanalysis; environmental analysis; green analytical chemistry; sorptive extraction; microextraction techniques
Special Issues, Collections and Topics in MDPI journals
Prof. Dr. Irene Panderi

E-Mail Website
Guest Editor
Laboratory of Pharmaceutical Analysis, Division of Pharmaceutical Chemistry, School of Pharmacy, National and Kapodistrian University of Athens, Panepistimiopolis, Zografou, 15771 Athens, Greece
Interests: pharmaceutical analysis; analytical chemistry; analytical methods; drug analysis, metabolites; bioactive compounds; pharmaceuticals; cosmeceuticals
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Sample preparation is and will always be the most important step in chemical analysis. Numerous techniques, methods, methodologies, and approaches are published in the literature, offering a wide range of analytical tools to the lab practitioner. Analytical scientists all over the world try to develop protocols for a plethora of analytes in various sample matrices. In the past decade, advances in sample pre-treatment have followed the demand for green chemistry and green analytical chemistry, focusing on miniaturization and automation, using the least possible amount of organic solvents. The question is, how far have we come, and what are the future perspectives? Analytical chemists are invited to share their experience in the field and report on recent advances in sample preparation approaches.

Prof. Dr. Victoria Samanidou
Prof. Dr. Irene Panderi
Guest Editors

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Keywords

  • sample preparation
  • sample pretreatment
  • extraction techniques
  • microextraction techniques
  • green analytical chemistry
  • miniaturization
  • automated techniques

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Published Papers (6 papers)

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Research

15 pages, 1728 KiB  
Article
Advancements in Adenine Nucleotides Extraction and Quantification from a Single Drop of Human Blood
by Ivana Popović, Lucija Dončević, Renata Biba, Karla Košpić, Maja Barbalić, Mija Marinković and Mario Cindrić
Molecules 2024, 29(23), 5630; https://doi.org/10.3390/molecules29235630 - 28 Nov 2024
Viewed by 940
Abstract
Adenine nucleotides (ANs)—adenosine 5′-triphosphate (ATP), adenosine 5′-diphosphate (ADP), and adenosine 5′-monophosphate (AMP)—are essential for energy transfer and the supply of countless processes within cellular metabolism. Their concentrations can be expressed as adenylate energy charge (AEC), a measure of cellular metabolic energy that directly [...] Read more.
Adenine nucleotides (ANs)—adenosine 5′-triphosphate (ATP), adenosine 5′-diphosphate (ADP), and adenosine 5′-monophosphate (AMP)—are essential for energy transfer and the supply of countless processes within cellular metabolism. Their concentrations can be expressed as adenylate energy charge (AEC), a measure of cellular metabolic energy that directly correlates with the homeostasis of the organism. AEC index has broad diagnostic potential, as reduced ATP levels are associated to various conditions, such as inflammatory diseases, metabolic disorders, and cancer. We introduce a novel methodology for rapid isolation, purification, and quantification of ANs from a single drop of capillary blood. Of all the stationary phases tested, activated carbon proved to be the most efficient for the purification of adenine nucleotides, using an automated micro-solid phase extraction (µ-SPE) platform. An optimized µ-SPE method, coupled with RP-HPLC and a run time of 30 min, provides a reliable analytical framework for adenine nucleotide analysis of diverse biological samples. AN concentrations measured in capillary blood samples were 1393.1 µM, 254.8 µM, and 76.9 µM for ATP, ADP, and AMP molecules aligning with values reported in the literature. Overall, this study presents a streamlined and precise approach for analyzing ANs from microliters of blood, offering promising applications in clinical diagnostics. Full article
(This article belongs to the Special Issue Sample Preparation-Quo Vadis: Current Status of Sample Preparation Approaches—3rd Edition)
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12 pages, 4427 KiB  
Article
Exploiting the Applicability of Polytetrahydrofuran-Modified Polyester for the Fabric Phase Sorptive Extraction of Doxycycline from Human Urine
by Panagiotis Chatzintounas, Marianna Ntorkou, Abuzar Kabir and Constantinos K. Zacharis
Molecules 2024, 29(17), 4076; https://doi.org/10.3390/molecules29174076 - 28 Aug 2024
Cited by 1 | Viewed by 1013
Abstract
In this report, a polytetrahydrofuran-coated polyester fabric phase sorptive extraction (FPSE) for the determination of doxycycline in human urine was described. The sol-gel polytetrahydrofuran sorbent proved to be superior against other sol-gel coated cellulose and polyester membranes tested. The effect of the extraction [...] Read more.
In this report, a polytetrahydrofuran-coated polyester fabric phase sorptive extraction (FPSE) for the determination of doxycycline in human urine was described. The sol-gel polytetrahydrofuran sorbent proved to be superior against other sol-gel coated cellulose and polyester membranes tested. The effect of the extraction parameters including membrane surface area, sample pH and volume, salt concentration, extraction time, stirring rate, etc., on the extraction efficiency of the analyte was studied using the “one-factor-at-a-time” (OFAT) and Box–Behnken design approaches. The analytical method proposed was validated in compliance with FDA guidelines for bioanalytical procedures. The method was linear in the determination range of 100–5000 ng/mL with the determination coefficient of 0.9953. The limit of detection (LOD) and the lower limit of quantification for doxycycline was 17 and 100 ng/mL, respectively. The relative recoveries for intra-day and inter-day studies ranged from 98.5–112.2% and 89.6–96.8%, respectively. The relative standard deviation was lower than 14.7% in all cases, exhibiting good precision. The sol-gel polytetrahydrofuran-modified FPSE membranes were reusable for at least 30 times. The greenness of the developed method was evaluated using Sample Preparation Metric of Sustainability (SPMS) and Blue Applicability Grade Index (BAGI) metric tools. Finally, the analytical scheme was successfully employed for the quantitation of urinary doxycycline collected at various time points following the administration of doxycycline-containing tablets. Full article
(This article belongs to the Special Issue Sample Preparation-Quo Vadis: Current Status of Sample Preparation Approaches—3rd Edition)
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16 pages, 2399 KiB  
Article
Using a Simple Magnetic Adsorbent for the Preconcentration and Determination of Ga(III) and In(III) by Electrothermal Atomic Absorption Spectrometry
by Yesica Vicente-Martínez, María José Muñoz-Sandoval, Manuel Hernández-Córdoba and Ignacio López-García
Molecules 2023, 28(6), 2549; https://doi.org/10.3390/molecules28062549 - 10 Mar 2023
Cited by 6 | Viewed by 1724
Abstract
A solid-phase dispersive microextraction procedure has been developed using ferrite (Fe3O4), an inexpensive magnetic material, as an adsorbent for the separation and subsequent determination of Ga(III) and In(III). The ions were removed from an aqueous solution by adsorption on [...] Read more.
A solid-phase dispersive microextraction procedure has been developed using ferrite (Fe3O4), an inexpensive magnetic material, as an adsorbent for the separation and subsequent determination of Ga(III) and In(III). The ions were removed from an aqueous solution by adsorption on Fe3O4, which was next easily collected from the medium by the action of a magnet. The analytes were then desorbed using 50 µL of 2 M NaOH or 50 µL of a 4:1 mixture of 0.1 M EDTA and 2 M HNO3 for the determination of Ga(III) or In(III), respectively. The level of the elements in the desorption phase was measured by electrothermal atomic absorption spectrometry (ETAAS) by injecting 10 µL of this phase into the atomizer. The enrichment factor was 163, and detection limits of 0.02 and 0.01 µg L−1 were achieved for Ga(III) and In(III), respectively. The reliability of the procedure has been verified by means of standard reference materials and by means of standard additions. Results are given for waters, soils and samples obtained from various electronic devices. It is of note that the procedure could be the basis for a useful way of recovering these valuable elements from different matrices for reuse. Full article
(This article belongs to the Special Issue Sample Preparation-Quo Vadis: Current Status of Sample Preparation Approaches—3rd Edition)
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14 pages, 1661 KiB  
Article
Autoxidation Kinetics of Tetrahydrobiopterin—Giving Quinonoid Dihydrobiopterin the Consideration It Deserves
by Ayoub Boulghobra, Myriam Bonose, Eskandar Alhajji, Antoine Pallandre, Emmanuel Flamand-Roze, Bruno Baudin, Marie-Claude Menet and Fathi Moussa
Molecules 2023, 28(3), 1267; https://doi.org/10.3390/molecules28031267 - 28 Jan 2023
Cited by 2 | Viewed by 2240
Abstract
In humans, tetrahydrobiopterin (H4Bip) is the cofactor of several essential hydroxylation reactions which dysfunction cause very serious diseases at any age. Hence, the determination of pterins in biological media is of outmost importance in the diagnosis and monitoring of H4Bip deficiency. More than [...] Read more.
In humans, tetrahydrobiopterin (H4Bip) is the cofactor of several essential hydroxylation reactions which dysfunction cause very serious diseases at any age. Hence, the determination of pterins in biological media is of outmost importance in the diagnosis and monitoring of H4Bip deficiency. More than half a century after the discovery of the physiological role of H4Bip and the recent advent of gene therapy for dopamine and serotonin disorders linked to H4Bip deficiency, the quantification of quinonoid dihydrobiopterin (qH2Bip), the transient intermediate of H4Bip, has not been considered yet. This is mainly due to its short half-life, which goes from 0.9 to 5 min according to previous studies. Based on our recent disclosure of the specific MS/MS transition of qH2Bip, here, we developed an efficient HPLC-MS/MS method to achieve the separation of qH2Bip from H4Bip and other oxidation products in less than 3.5 min. The application of this method to the investigation of H4Bip autoxidation kinetics clearly shows that qH2Bip’s half-life is much longer than previously reported, and mostly longer than that of H4Bip, irrespective of the considered experimental conditions. These findings definitely confirm that an accurate method of H4Bip analysis should include the quantification of qH2Bip. Full article
(This article belongs to the Special Issue Sample Preparation-Quo Vadis: Current Status of Sample Preparation Approaches—3rd Edition)
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10 pages, 1638 KiB  
Article
A Simple High-Throughput Field Sample Preparation Method Based on Matrix-Induced Sugaring-Out for the Simultaneous Determination of 5-Hydroxymethylfurfural and Phenolic Compounds in Honey
by Xijuan Tu, Fengjie Yu, Qian Jin, Chunping Du, Jiaxu Chen, Ji Yang, Yuchang He, Shaokang Huang and Wenbin Chen
Molecules 2022, 27(23), 8373; https://doi.org/10.3390/molecules27238373 - 30 Nov 2022
Cited by 1 | Viewed by 2435
Abstract
In the present work, a high-throughput field sample preparation method was reported for the simultaneous determination of 5-hydroxymethylfurfural and phenolic compounds in honey. Combining a simple and green homogenous liquid–liquid extraction, matrix-induced sugaring-out, with the use of a 96-deepwell plate and multichannel pipette, [...] Read more.
In the present work, a high-throughput field sample preparation method was reported for the simultaneous determination of 5-hydroxymethylfurfural and phenolic compounds in honey. Combining a simple and green homogenous liquid–liquid extraction, matrix-induced sugaring-out, with the use of a 96-deepwell plate and multichannel pipette, the proposed method showed its merits in instrument-free and high-throughput preparation. Due to the high-throughput property, the parameters of the method were rapidly and systematically studied using a constructed 4 × 2 × 4 × 3 array (sample amount × ratio of ACN:H2O × standing time × replicates) in a 96-deepwell plate. Analytical performance was fully validated, and the limits of detection and limits of quantification were in the range of 0.17–1.35 μg/g and 0.51–4.14 μg/g, respectively. Recoveries were between 83.98 and 117.11%, and all the precisions were <5%. Furthermore, the developed method was successfully applied in the outdoor preparation of commercial honey samples and the in-field preparation of raw honey samples in apiary. The current work presented a simple, rapid, and high-throughput method for the field sample preparation of honey and provides a valuable strategy for the design of field and on-site sample preparation. Full article
(This article belongs to the Special Issue Sample Preparation-Quo Vadis: Current Status of Sample Preparation Approaches—3rd Edition)
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18 pages, 2935 KiB  
Article
Separation and Purification of Two Saponins from Paris polyphylla var. yunnanensis by a Macroporous Resin
by Xiaoya Zhang, Junli Wu, Long Qin, Guangxi Wang, Ping Li, Anmin Yu, Aizhong Liu and Rui Sun
Molecules 2022, 27(19), 6626; https://doi.org/10.3390/molecules27196626 - 6 Oct 2022
Cited by 19 | Viewed by 2972
Abstract
An effective method for separating and purifying critical saponins (polyphyllin II and polyphyllin VII) from a Paris polyphylla var. yunnanensis extract was developed in this study which was environmentally friendly and economical. Static adsorption kinetics, thermodynamics, and the dynamic adsorption-desorption of macroporous resins [...] Read more.
An effective method for separating and purifying critical saponins (polyphyllin II and polyphyllin VII) from a Paris polyphylla var. yunnanensis extract was developed in this study which was environmentally friendly and economical. Static adsorption kinetics, thermodynamics, and the dynamic adsorption-desorption of macroporous resins were investigated, and then the conditions of purification and separation were optimized by fitting with an adsorption thermodynamics equation and a kinetic equation. Effective NKA-9 resin from seven macroporous resins was screened out to separate and purify the two saponins. The static adsorption and dynamic adsorption were chemical and physical adsorption dual-processes on the NKA-9 resin. Under the optimum parameters, the contents of polyphyllin II and polyphyllin VII in the product were 17.3-fold and 28.6-fold those in plant extracts, respectively. The total yields of the two saponins were 93.16%. This research thus provides a theoretical foundation for the large-scale industrial production of the natural drugs polyphyllin II and polyphyllin VII. Full article
(This article belongs to the Special Issue Sample Preparation-Quo Vadis: Current Status of Sample Preparation Approaches—3rd Edition)
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