Sample Pretreatment Research Articles

Rapid Sample Pretreatment Facilitating SERS Detection of Trace Weak Organic Acids/Bases in Complex Matrices.

Fast and efficient sample pretreatment is the prerequisite for realizing surface-enhanced Raman spectroscopy (SERS) detection of trace targets in complex matrices, which is still a big issue for the practical application of SERS. Recently, we have proposed a highly performed liquid-liquid extraction (LLE)-back extraction (BE) for weak acids/bases extraction in drinking water and beverage samples. However, the performance efficiency decreased drastically on facing matrices like food and biological blood. Based on the total interaction energies among target, interferent, and extractant molecules, solid-phase extraction (SPE) with a higher selectivity was introduced in advance of LLE-BE, which enabled the sensitive (μg L-1 level) and rapid (within 10 min) SERS detection of both koumine (a weak base) and celastrol (a weak acid) in different food and biological samples. Further, the high SERS sensitivity was determined unmanned by Vis-CAD (a machine learning algorithm), instead of the highly demanded expert recognition. The generality of SPE-LLE-BE for various weak acids/bases (2 < pKa < 12), accompanied by the high efficiency, easy operation, and low cost, offers SERS as a powerful on-site and efficient inspection tool in food safety and forensics.

Glucose sensing performance of bimetallic MOFs CoFe-ZIF/CC for enzyme-free saliva sensor applications

Co-ZIF is widely believed as a promising material which shows potential in MOFs based enzyme-free sensors. However, the research of Co-ZIF in glucose sensor filed has been hampered, due to its poor electronic conductivity and slow ion diffusion caused by closed rhombohedral dodecahedron structure. In this work, the obtained Co0.95Fe0.05-ZIF presents highly opened nanosheet structure on CC, resulting in rich open active sites and ions moving channels. Compared with other reported ZIFs, the Co0.95Fe0.05-ZIF/CC exhibits excellent sensing performance with a high sensitivity of 3232.30 μA mM−1 cm−2 in the range of 0.20–1.00 mM and a low detection limit of less than 5 μM, due to its highly opened nanosheet structure. The Co0.95Fe0.05-ZIF/CC also shows excellent selectivity, repeatability and reproducibility for glucose detection. Furthermore, the variation trend of test results measured by this saliva sensor without any sample pre-treatment, is consistent with that of commercial blood glucose meter, indicating its potential in real applications. This synthesis strategy also provides a new direction of structure construction for high performance MOFs in enzyme-free glucose sensor field.

Drying Kinetics and Thermodynamic Properties of Ultrasound Pretreatment Bitter Melon Dried by Infrared

Determination of drying characteristics of ripe and unripe bitter melon in an infrared dryer at 50, 60, and 70°C with airborne ultrasonic pretreatment with a power of 20 kW for 0, 10, and 20 minutes and a frequency of 20 kHz is the purpose of this study. At the end of drying, among the five used models that fit the moisture ratio data, the Midilli and logarithmic models were selected to properly characterize the drying behavior in the infrared dryer with ultrasonic pretreatment of ripe and unripe bitter melon samples. Moisture transfer from bitter melon samples’ ripeness and early maturity was defined using Fick’s diffusion equation. Then, the Arrhenius equation was utilized to determine the effective moisture diffusivity. Also, the activation energy of unripe and ripe bitter melon slices was reduced with the enhancement in the ultrasound pretreatment time. Water activity (aw) amounts of ripe and unripe bitter melon were achieved at various drying temperatures and ultrasound pretreatment. The trends of the experiment indicate a decrease in enthalpy (ΔH) and entropy (ΔS) amounts of bitter melon with enhancing temperature and ultrasonic. The Gibbs free energy (ΔG) increases with enhancing drying temperature and ultrasonic pretreatment. Specific energy consumption decreased with enhancing drying temperature and ultrasound pretreatment duration for both ripe and unripe bitter melon samples.

Fabrication of magnetic hydrophilic imprinted polymers via two-step immobilization approach for targeted detecting bisphenol A

Molecularly imprinted polymer with water-compatibility for effective separation and enrichment of targeted trace pollutants from complicated matrix has captured extensive attention in terms of their high selectivity and matrix compatibility. This study focuses on modified β-cyclodextrin is used as a hydrophilic functional monomer to develop magnetic molecularly imprinted polymers (MMIPs). MMIPs were prepared using Fe3O4 nanoparticles as carriers and bisphenol A (BPA) as templates using a two-step fixation strategy and surface imprinting technology. The structural characteristic and binding properties of the prepared MMIPs were thoroughly studied. The MMIPs exhibited high crystallinity, high adsorption capacity, fast rebinding rate, remarkable selectivity and distinguish reusability. In addition, through magnetic solid-phase extraction separation technology and high-performance liquid chromatography ultraviolet quantitative detection technology, MMIPs are used for selective enrichment and detection of BPA in complex media such as environmental water and milk. This work provides a new route to construct the hydrophilic molecularly imprinted materials and a new sight on developing more effective sample pretreatment strategies for monitoring targeted pollution in complicated aqueous media.

High sensitive detection of Cd, Hg, Pb and Cr in rice based on LA-MPT-OES with optimized excitation regions by two-dimensional characterization of plasma plume

Direct, rapid and highly sensitive detection of heavy metals in rice is essential to ensure food safety. In this research, a combination of laser ablation and microwave plasma torch optical emission spectrometry (LA-MPT-OES) was proposed. Based on the optimal observation positions, a high sensitivity and direct determination of Cd, Hg, Pb and Cr in rice were realized. The limits of detection (LOD) were 0.97, 0.12, 0.61 and 0.15 μg/kg, respectively, which were reduced by one order of magnitude compared to the optimal observation height. In addition, the LOD was reduced by one to two orders of magnitude compared with the techniques that require sample pre-treatment. Moreover, the results of the Certified Reference Materials and real samples were in agreement with the reference values with a relative error in the range of 0.28% ∼ 14.16%. The results demonstrated that LA-MPT-OES could be a promising tool to detect heavy metals in rice.

Online monitoring system for qualitative and quantitative analysis of bioaerosols by combined ATP bioluminescence assay with loop-mediated isothermal amplification

Rapid detection of airborne pathogens is crucial in preventing respiratory infections and allergies. However, technologies aiming to real-time analysis of microorganisms in air remain limited due to the sparse and complex nature of bioaerosols. Here, we introduced an online bioaerosol monitoring system (OBMS) comprised of integrated units including a rotatable stainless-steel sintered filter-based sampler, a lysis unit for extracting adenosine triphosphate (ATP), and a single photon detector-based fluorescence unit. Through optimization of the ATP bioluminescence method and establishment of standard curves between relative luminescence units (RLUs) and ATP as well as microbial concentration, we achieved simultaneous detection of bioaerosols' concentration and activity. Testing OBMS with four bacterial and two fungal aerosols at a sampling flow rate of 10 to 50 L/min revealed an outstanding collection efficiency of 95 % at 30 L/min. A single OBMS measurement takes only 8 min (sampling: 5 min; lysis and detection: 3 min) with detection limits of 3 Pcs/ms photons (2.9 × 103 and 292 CFU/m3 for Staphylococcus aureus and Candida albicans aerosol). In both laboratory and field tests, OBMS detected higher concentrations of bioaerosol compared to the traditional Andersen impactor and liquid biosampler. When combined OBMS with loop-mediated isothermal amplification (LAMP), the bioaerosol can be qualitative and quantitative analyzed within 40 min without the cumbersome procedures of sample pretreatment and DNA extraction. These results offer a high compressive and humidity resistance membrane filtration sampler and validate the potential of OBMS for online measurement of bioaerosol concentration and composition.

An Optimized Microwave-Assisted Digestion Method to Analyze the Amino Acids Profile of Quisqualis Fructus from Different Planted Origins.

This study aims to establish a rapid and convenient microwave-assisted digestion method for sample pretreatment to determine amino acid profiles in natural products. This method was applied to analyze the amino acid profiles of Quisqualis Fructus (QF) from different planted origins. The microwave-assisted digestion conditions were optimized by a response surface methodology (RSM), and 17 amino acids in different planted origins of QF were determined by an automatic amino acid analyzer according to the optimized digestion conditions. The contents of 17 amino acids in QF from different planted origins were further analyzed by fingerprint and chemometric analysis. The temperature of microwave digestion at 167 °C, time of microwave digestion at 24 min, and a solid-liquid ratio of 46.5 g/mL was selected as the optimal digestion conditions. The total content of 17 amino acids in QF from different planted origins ranged from 71.88 to 91.03 mg/g. Amino acid composition and nutritional evaluation indicated that the content of medicinal amino acids was higher than aromatic amino acids. The results of fingerprint analysis reflected that the similarity between the 16 batches of QF ranged from 0.889 to 0.999, while chemometrics analysis indicated amino acid content in QF varied from different planted origins, and six important differential amino acids were screened. Compared with the traditional extraction method, microwave-assisted digestion with response surface optimized has the advantages of rapidity, convenience, and reliability, which could be used to study the amino acid profiles in natural products. The amino acid profile of QF indicated that it has a rich medicinal nutritional value. Different planted origins of QF have a high degree of similarity and could be effectively distinguished by chemometric analysis.

Real-time in situ detection of petroleum hydrocarbon pollution in soils via a novel optical methodology

Petroleum hydrocarbon (PHC) contamination in soils is considered one of the most serious problems currently, of which the detection and identification is a fairly significant but challenging work. Conventional methods to do such work usually need complex sample pretreatment, consume much time and fail to do the in-situ detection. This paper set out to create a novel systematic methodology to realize the goals accurately and efficiently. Based on laser-induced breakdown spectroscopy (LIBS) and self-improved machine learning methods, the innovative methodology only uses extremely simple devices to do the real-time in situ detection and identification work and even realize the quantitative analysis of pollution level accurately. In the study, clean soils mixed with petroleum were served as polluted samples, clean soils to be the blank group for comparison. Based on the elemental information from the spectra obtained by LIBS, machine learning methods were improved and helped optimized the algorithm to identify the PHC polluted soil samples for the first time. Furthermore, a novel model was designed to perform the quantitative analysis of the concentration of PHC pollution in soils, which can be applied to detect the degree of PHC contamination in soils accurately. Finally, the harmful volatile component of the PHC polluted soils was also successfully and identified despite its extremely minimal content in the air. The newly-designed methodology is novel and efficient, which has extensive application prospect in the real-time in situ detection of petroleum hydrocarbon pollution.

From surface to core: Comprehensive ToF-SIMS insights into pharmaceutical tablet analysis

This study presents an innovative approach to pharmaceutical analysis using time-of-flight secondary ion mass spectrometry (ToF-SIMS) to investigate tablets containing paracetamol in the solid state without the need for traditional pretreatment methods (dissolution, filtration, etc.). Employing both MS1 and MS2 ToF-SIMS spectra, signals characteristic of paracetamol and a fragmentation mechanism were assigned. Some findings challenge previous interpretations of certain ToF-SIMS signals attributed to paracetamol, highlighting the need for reevaluation. Moreover, as the sample was used without any pretreatment (a purchased tablet), which has a complex matrix, the resulting ToF-SIMS mass spectra can suffer from spectral interferences. The use of multivariate statistical analysis resulted in the assignment of unique signals for paracetamol. Additionally, ToF-SIMS imaging was utilized with high mass and lateral resolution, employing the delayed-extraction ToF analyzer mode, to image the two-dimensional distribution of species on the tablet’s surface with an emphasis on paracetamol distribution. The use of a gas cluster ion beam (GCIB) sputtering source in association with ToF-SIMS enabled the visualization of the three–dimensional distribution of species within the tablet. This thorough investigation advances knowledge regarding the characterization of paracetamol and offers the examination of pharmaceuticals without sample pretreatment with elemental and molecular-specific information.

Aptamer based hybrid monolithic pipette tips supported by melamine sponge for enrichment of proteins

BackgroundThe convenient preparation and application of functionalized organic-inorganic hybrid monolithic materials have obtained substantial interest in the pretreatment of complex samples by solid-phase extraction (SPE). Compared to the in-tube solid-phase microextraction in fused-silica capillaries, micro SPE in plastic pipette tips have fascinating merits for the easily operated enrichment of trace target analytes from biological samples. However, the poor compatibility of organic-inorganic hybrid monoliths with plastics leads to the rare appearance of commercial hybrid monolithic pipette tips (HMPTs). Therefore, how to synthesize the organic-inorganic hybrid monolithic materials with better extraction performance in plastic pipette tips becomes a challenge. ResultsWe develop a facile and cheap strategy to immobilize organic-inorganic hybrid monoliths in pipette tips. Melamine sponge was employed as the supporting skeleton to in situ assemble amine- and thiol-bifunctionalized hybrid monolithic material via “one pot” in a pipette tip, and gold nanoparticles (GNPs) and thiol-modified aptamer against human α-thrombin were sequentially attached to the hybrid monolith within the HMPTs. The average coverage density of the aptamer with GNPs as an intermediary reached as high as 818.5 pmol μL−1. The enriched thrombin concentration was determined by a sensitive enzymatic chromogenic assay with the limit of detection of 2 nM. The extraction recovery of thrombin at 10 nM in human serum was 86.1 % with a relative standard deviation of 6.1 %. This proposed protocol has been applied to the enrichment and determination of thrombin in real serum sample with strong anti-interference ability, low limit of detection and high recovery. SignificanceThe amine- and thiol-bifunctionalized HMPTs prepared with sponge as the skeleton frame provided a novel substrate material to decorate aptamers for efficient enrichment of proteins. This enlightens us that we can take advantage of the tunability of sponge assisted HMPTs to produce and tailor a variety of micro SPE pipette tips for broader applications on the analysis of trace targets in complex biological, clinic and environmental samples.

Paper Spray Mass Spectrometry with On‐Paper Electrokinetic Manipulations: Part‐Per‐Trillion Detection of Per/Polyfluoroalkyl Substances in Water and Opioids in Urine

AbstractWe developed a simple, paper‐based device that enables sensitive detection by mass spectrometry (MS) without solid phase extraction or other sample preparation. Using glass fiber filter papers within a 3D printed holder, the device employs electrokinetic manipulations to stack, separate, and desalt charged molecules on paper prior to spray into the MS. Due to counter‐balanced electroosmotic flow and electrophoresis, charged analytes stack on the paper and desalting occurs in minutes. One end of the paper strip was cut into a sharp point and positioned near the inlet of a MS. The stacked analyte bands move toward the paper tip with the EOF where they are ionized by paper spray. The device was applied to analysis of PFAS in tap water with sub part‐per‐trillion detection limits in less than ten minutes with no sample pretreatment. Analysis of opioids in urine also occurs in minutes. The crucial parameters to enable stacking, separation, and MS ionization of both positively and negatively charged analytes were determined and optimized. Experimental and computational modeling studies confirm the electrokinetic stacking and analyte transport mechanisms. On‐paper separations were carried out by stacking analyte bands at different locations depending on their electrophoretic mobility, achieving baseline separation in some cases.

Paper Spray Mass Spectrometry with On-Paper Electrokinetic Manipulations: Part-Per-Trillion Detection of Per/Polyfluoroalkyl Substances in Water and Opioids in Urine.

We developed a simple, paper-based device that enables sensitive detection by mass spectrometry (MS) without solid phase extraction or other sample preparation. Using glass fiber filter papers within a 3D printed holder, the device employs electrokinetic manipulations to stack, separate, and desalt charged molecules on paper prior to spray into the MS. Due to counter-balanced electroosmotic flow and electrophoresis, charged analytes stack on the paper and desalting occurs in minutes. One end of the paper strip was cut into a sharp point and positioned near the inlet of a MS. The stacked analyte bands move toward the paper tip with the EOF where they are ionized by paper spray. The device was applied to analysis of PFAS in tap water with sub part-per-trillion detection limits in less than ten minutes with no sample pretreatment. Analysis of opioids in urine also occurs in minutes. The crucial parameters to enable stacking, separation, and MS ionization of both positively and negatively charged analytes were determined and optimized. Experimental and computational modeling studies confirm the electrokinetic stacking and analyte transport mechanisms. On-paper separations were carried out by stacking analyte bands at different locations depending on their electrophoretic mobility, achieving baseline separation in some cases.

Ambient mass spectrometry imaging of food natural products by angled direct analysis in real time high-resolution mass spectrometry

Direct surface analysis in ambient conditions provides information on the position and chemical composition of an object at the time of investigation. An angled sampling probe is developed in this work for direct analysis in real time (DART) ionization high-resolution mass spectrometry. The DART ion source and the interface were modified for improved surface resolution, increased ion transfer efficiency, as well as enabling two-dimensional surface scanning. The angled probe DART-MS system was used for investigating a variety of food samples including fruit peels, ginseng root, plant leaves and sections of radish. Abundant signals and distinct chemical profiles are obtained in seconds, and spatial distribution of different molecules across the sample surfaces can be observed. In addition, the developed system can quickly identify the chemical changes when the surfaces were treated. The method is capable of directly evaluating food sample surfaces with different shapes, hardness, and conditions, without any sample pretreatments.

Size-classifiable quantification of nanoplastic by rate zonal centrifugation coupled with pyrolysis-gas chromatography-mass spectrometry

Particle size is an important indicator to evaluate the environmental risk and biotoxicity of nanoplastic (NP, particle diameter <1000 nm). The methods available to determine size classes of NP in environmental samples are few and are rare to achieve efficient separation and recycling of NP with close particle sizes. Here, we show that rate-zonal centrifugation (RZC) can quickly and efficiently collect NP of different sizes based on their sedimentation coefficients. When combined with cloud-point extraction (CPE) and pyrolysis−gas chromatography−mass spectrometry (Py-GC-MS), our method can quantify three NP particle-size classes separately (including 100 nm, 300 nm, and 600 nm) in aqueous samples with high recovery (81.4 %–89.4 %), limits of detections (LODs, 33.5–53.4 μg/L), and limits of quantifications (LOQs, 110.6–167.2 μg/L). Compared with the conventional sample pretreatment process, our method can effectively extract and determine the NP with different sizes. Our approach is highly scalable and can be effectively applied to NP in a wide range of aquatic environments. Meanwhile, our approach is highly scalable to incorporate diverse assays to study the environmental behaviours and ecological risks of NP.

Facile preparation of hollow covalent organic frameworks as superior and universal matrix clean-up micro-structures for high throughout determination of food hazards

The complicated food matrix seriously limits the one-time test for the potential food hazards in non-targeted analysis. Accordingly, developing advanced sample pretreatment strategy to reduce matrix effects is of great significance. Herein, newly-integrated hollow-structured covalent organic frameworks (HCOFs) with large internal adsorption capacity and target-matched pore size were synthesized via etching the core-shell structured COFs. The as-prepared HCOFs could be directly applied for matrix clean-up of vegetable samples, while further modification of polydopamine (PDA) network facilitated application for animal samples. Both HCOFs and HCOFs@PDA with the comparable sizes to the matrix interference gave excellent adsorption performance to targets, achieving satisfied recoveries (70%–120%) toward 90 pesticides and 44 veterinary drugs in one-test, respectively. This work showed the great potential of the facile-integrated HCOFs with high stability and customized size to remove interference matrix and offered a universal strategy to achieve simultaneous screening of hazards with considerable quantity in high-throughput non-targeted analysis.

Determination of fifteen illegal colorants in traditional Chinese medicines by two hydrophobic DES-based microextraction methods coupled with an HPLC-DAD

The dyeing and adulteration of traditional Chinese medicines (TCMs) are continuously updated. Valuable analytical methods for the daily inspection of illegal colorant additives in TCMs and the preparations are in demand. Two deep eutectic solvent (DES)-based vortex-assisted liquid-liquid microextraction (VA-LLME) and ultrasonic-assisted solid-liquid microextraction (UA-SLME) were developed for the sample pretreatment of ten water-soluble colorants and five water-insoluble colorants, respectively, followed by an HPLC-DAD detection. Fifteen colorants were analyzed at four detection wavelengths within 40 min of gradient elution. The optimal DES of VA-LLME and UA-SLME were screened from 23 homemade DESs. The factors affecting the extraction efficiency of VA-LLME and UA-SLME were optimized systematically. Under the optimal conditions, ten water-soluble colorants analyzed by DES-based VA-LLME-HPLC-DAD showed good linearity (R ≥ 0.9995) within the optimal linear range. The LODs and LOQs were 0.2–1.0 μg g−1 and 0. 5–5.0 μg g−1, respectively. The recoveries of spiked samples were 80.2%–104.7 %, with RSDs ≤ 4.39 %. Five water-insoluble colorants of Sudan I‒IV and Sudan 7B analyzed by DES-based UA-SLME-HPLC-DAD showed good linearity (R ≥ 0.9995) within the optimal linear range. The LODs and LOQs were 0.8–8.0 μg g−1 and 4.0–40.0 μg g−1, respectively. The recoveries of spiked samples were 94.2%–103.1 %, with RSDs ≤ 4.81 %. The proposed DES-based VA-LLME-HPLC-DAD was successfully applied to analyze six water-soluble yellow colorants in Cuscutae Semen, salted Cuscutae Semen, and four water-soluble red colorants in Schisandrae Chinensis Fructus. The proposed DES-based UA-SLME-HPLC-DAD was successfully applied to analyze five water-insoluble red colorants in Dieda pills. The study provides analytical method options for routine tests of water-soluble, water-insoluble, or both water-soluble/-insoluble illegal colorant additives in herbal medical materials and preparations by the relevant proposed DES-based sample pretreatment method or a combination of the two proposed DES-based methods.

Carbonized polymer dots-based molecular imprinting: An adsorbent with enhanced selectivity for highly efficient recognition and removal of ceftiofur sodium from complex samples

Highly selective removal of residual cephalosporin antibiotics from complex systems is crucial for human health and ecological environment protection. Herein, a newly molecularly imprinted polymer adsorbent (CPDs-NH2@MIP) with enhanced selectivity for ceftiofur sodium (CTFS) was developed by using the special carbonized polymer dots (CPDs-NH2) as functional monomer. The CPDs-NH2 has a nano-spherical structure and functionalized groups (CC, −NH2) via the incomplete carbonization polymerization of citric acid, acrylamide and ethylenediamine, which can accurately interact with CTFS by overcoming steric hindrance, resulting in more precisely imprinted sites and reducing non-imprinted regions in MIP. The presented CPDs-NH2@MIP exhibited excellent adsorption capacity for CTFS (68.62 mg g−1), achieving equilibrium within 10 min, and highly selectivity in mixed solution containing five coexisting substances, with an imprinted factor (5.61). Compared with commercial adsorbents and MIPs prepared with traditional chain functional monomers, the CPDs-NH2@MIP showed significant advantage in selective recognition and separation of target. Analysis of microstructure and mechanism proved that usage of the spherical functional monomer generated precise imprinting sites and dense structure in CPDs-NH2@MIP, which effectively enhanced the selectivity in complex system combined with hydrogen bonding interaction. The idea of designing and using spherical functional monomer will promote the practicality of molecularly imprinted polymer adsorbents.

Rapid and reliable quantification of urinary malondialdehyde by HILIC-MS/MS: A derivatization-free breakthrough approach

BackgroundThe development of fast analytical methods is crucial for the research, discovery, and confirmation of crucial biomarkers. Furthermore, the implementation of fast analytical strategies contributes to efficient and time-effective procedures. In this sense, analysis of malondialdehyde (MDA) has become an important tool for understanding the role of oxidative stress in various diseases and for evaluating the efficacy of therapeutic interventions. ResultsA rapid and robust liquid chromatography tandem mass spectrometry method (HPLC-MS/MS) has been developed to determine endogenous amounts of malondialdehyde (MDA) in human urine without any associated derivatization reaction. MDA was separated in 4 min through a Urea-HILIC column and was analyzed using a triple quadrupole mass spectrometer in negative electrospray ionization mode. With a 50-fold dilution as the only sample pretreatment after alkaline hydrolysis, no matrix effect was present, which allowed for a fast and simple quantification by means of an external standard calibration with a limit of detection of 0.20 ng mL−1. The whole methodology was validated by analyzing unspiked and spiked urine samples from ten healthy individuals and comparing with the results obtained by the standard addition method. MDA was detected in all cases, with natural concentrations varying from 0.11 ± 0.03 to 0.31 ± 0.03 mg g−1 creatinine. Accuracies were found to be satisfactory, ranging from 95 % to 101 %. The proposed method also exhibited good repeatability and reproducibility (RSD<15 %) for four quality control levels. SignificanceThe main significance of this method is the avoidance of a derivatization reaction for the determination of urinary MDA, this constituting a step forward when compared with previous literature. This breakthrough not only streamlines time analysis to less than 5 min per sample but also results in a more robust procedure. Consequently, the method here developed could be applied to subsequent future research involving the determination of MDA as a lipid peroxidation biomarker, where simple, rapid, and reliable methods could represent a significant improvement.

Molecularly imprinted resin modified with ionic liquid for dispersive filter extraction and determination of perfluoroalkyl acids in eggs

Perfluoroalkyl acids (PFAAs) are emerging pollutants that endangers food safety. Developing methods for the selective determination of trace PFAAs in complex samples remains challenging. Herein, an ionic liquid modified porous imprinted phenolic resin-dispersive filter extraction-liquid chromatography-tandem mass spectrometry (IL-PIPR−DFE−LC-MS/MS) method was developed for the determination of perfluorooctanoic acid (PFOA) and perfluorooctane sulfonate (PFOS) in eggs. The new IL-PIPR adsorbent was prepared at room temperature, which avoids the disorder and instability of the template at high temperatures. The imprinting factor of IL-PIPR for PFOA and PFOS exceeded 7.3. DFE, combined with IL-PIPR (15 mg), was used to extract PFOA and PFOS from eggs within 15 min. The established method exhibits low limits of detection (0.01–0.02 ng/g) and high recoveries (84.7%–104.7%), which surpass those of previously reported methods. This work offers a new approach to explore advanced imprinted adsorbents for PFAAs, efficient sample pretreatment technique, and analytical method for pollutants in foods.

Preconcentrating extractive polymeric network in paper-based sensing of copper

The concept of using an extractive polymeric sensing network on a paper-based substrate for the pretreatment of samples in the colorimetric analysis of heavy metals is demonstrated with the determination of Cu2+ in aqueous samples. The newly developed paper-based device combines the advantages of both liquid–liquid extraction-based separation and the analytical capabilities of microfluidic paper-based analytical devices (μPADs). The preconcentrating extractive polymeric network composed of 53.5 wt% poly(vinyl chloride) (PVC), 45 wt% extractant (di-(2-ethylhexyl)phosphoric acid (D2EHPA)) and 1.5 wt% dye (1-(2′-pyridylazo)-2-naphthol (PAN)), coated on filter paper, shows good water-wicking properties, allowing the transmission of high sample volumes. This results in significant analyte preconcentration. The extractant (D2EHPA) selectively binds Fe3+ and Zn2+ which otherwise will compete with Cu2+ in its colour reaction with PAN at the chosen pH of 3.0. The device’s capacity to process higher sample volumes resulting in higher sensitivity is increased by the integration of several filter paper absorption layers. The optimized device is characterized by a limit of detection (LOD) for tap and environmental waters of 3.4 and 9.6 µg/L, respectively; stability of 51 days if stored in a refrigerator; and total analysis time (from sample insertion to colour detection) of less than 5 min.