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1.
Food Chem ; 462: 141007, 2025 Jan 01.
Article in English | MEDLINE | ID: mdl-39216376

ABSTRACT

In this study, covalent organic frameworks (COFs) were grown in situ on magnetic nitrogen-doped graphene foam (MNGF), and the resulting composite of COFs-modified MNGF (MNC) was wrapped by molecularly imprinted polymers (MNC@MIPs) for specifically capturing SAs. A magnetic solid phase extraction (MSPE) method for SAs was established using MNC@MIPs with good magnetic responsiveness. The adsorption performance of MNC@MIPs was superior to that of non-molecularly imprinted polymers (MNC@NIPs), with shorter adsorption/desorption time and higher imprinting factors. A high-efficiency SAs analytical method was developed by fusing HPLC and MNC@MIPs-based MSPE. This approach provides excellent precision, a low detection limit, and wide linearity. By analyzing fish samples, the feasibility of the approach was confirmed, with SAs recoveries and relative standard deviations in spiked samples in the ranges of 77.2-112.7 % and 2.0-7.2 %, respectively. This study demonstrated the potential use of MNC@MIPs-based MSPE for efficient extraction and quantitation of trace hazards in food.


Subject(s)
Fishes , Food Contamination , Metal-Organic Frameworks , Molecularly Imprinted Polymers , Solid Phase Extraction , Sulfonamides , Solid Phase Extraction/methods , Solid Phase Extraction/instrumentation , Animals , Molecularly Imprinted Polymers/chemistry , Adsorption , Food Contamination/analysis , Metal-Organic Frameworks/chemistry , Sulfonamides/isolation & purification , Sulfonamides/chemistry , Sulfonamides/analysis , Molecular Imprinting , Polymers/chemistry
2.
Food Chem ; 462: 140936, 2025 Jan 01.
Article in English | MEDLINE | ID: mdl-39232273

ABSTRACT

Aromatic amino acid oxidation products (AAAOPs) are newly discovered risk substances of thermal processes. Due to its significant polarity and trace level in food matrices, there are no efficient pre-treatment methods available to enrich AAAOPs. Herein, we proposed a magnetic cationic covalent organic framework (Fe3O4@EB-iCOF) as an adsorbent for dispersive magnetic solid-phase extraction (DMSPE). Benefiting from the unique charged characteristics of Fe3O4@EB-iCOF, AAAOPs can be enriched through electrostatic interaction and π-π interactions. Under the optimal DMSPE conditions, the combined HPLC-MS/MS method demonstrated good linearity (R2 ≥ 0.990) and a low detection limit (0.11-7.5 µg·kg-1) for AAAOPs. In addition, the method was applied to real sample and obtained satisfactory recoveries (86.8 % âˆ¼ 109.9 %). Especially, we applied this method to the detection of AAAOPs in meat samples and conducted a preliminarily study on its formation rules, which provides a reliable basis for assessing potential dietary risks.


Subject(s)
Amino Acids, Aromatic , Oxidation-Reduction , Solid Phase Extraction , Solid Phase Extraction/methods , Amino Acids, Aromatic/chemistry , Amino Acids, Aromatic/analysis , Amino Acids, Aromatic/isolation & purification , Tandem Mass Spectrometry , Metal-Organic Frameworks/chemistry , Hot Temperature , Food Contamination/analysis , Chromatography, High Pressure Liquid , Animals , Adsorption , Meat/analysis , Food, Processed
3.
Biomed Chromatogr ; : e6011, 2024 Sep 19.
Article in English | MEDLINE | ID: mdl-39300201

ABSTRACT

Huperzine A is a reversible and selective cholinesterase inhibitor and has been approved for the treatment of Alzheimer's diseases. In this study, we developed a highly sensitive and specific ulta-high-performance liquid chromatography-tandem mass spectrometry method for the determination of Huperzine A in rat plasma. An aliquot of 50 µL of rat plasma sample was pretreated with 200 µL of acetonitrile-methanol (v/v; 1:1) containing 0.2% formic acid followed by solid phase extraction. The resulting sample was separated on a Waters ACQUITY BEH C18 column using acetonitrile and water containing 0.2% formic acid as mobile phase, at a flow rate of 0.3 mL/min. Multiple-reaction monitoring (MRM) mode was used for quantitative analysis of Huperzine A in positive electrospray ionization. In the concentration range of 0.01-10 ng/mL, Huperzine A showed excellent linearity with correlation coefficient > 0.998. The intra- and inter-day RSD% were less than 9.7%, while the RE% ranged from -6.7% to 10.0%. The mean recovery was >84.5%. The validated method was demonstrated to be selective, sensitive, and reliable, which has been successfully applied to pharmacokinetic study of Huperzine A in rat plasma. Huperzine A displayed a long half-life in rat plasma and high oral bioavailability.

4.
Talanta ; 281: 126911, 2024 Sep 18.
Article in English | MEDLINE | ID: mdl-39317067

ABSTRACT

In this study, an ultrasonic assisted dispersive magnetic solid phase extraction leveraging Fe3O4@nitrogen-doped carbon@Pd core-double shell nanotubes was developed for the extraction of organophosphorus pesticides (OPPs) in trace levels from real samples. Incorporation of Pd species into the structure of the nanosorbent could enhance its interactions with sulfur groups in the structure of OPPs. X-ray photoelectron spectroscopy and X-ray diffraction, brunauer-emmett-teller, field emission scanning electron microscopy, and high-resolution transmission electron microscopy were used to characterize the nanosorbent after its synthesis. Then, effective variables on the extraction efficiency of OPPs using the nanosorbent were optimized. These parameters included 2-propanol as the adsorption solvent; the sample pH of 7.0; the sorbent quantity of 10 mg; and the extraction and desorption times of 3 min. Under optimized conditions, linear ranges with determination coefficients (R2) higher than 0.99, low detection limits of 0.30 ng mL-1, high preconcentration factors (423-470) and relatively high extraction recoveries (84-94 %) were obtained. The proposed extraction system was then successfully applied to the analysis of OPPs in fruits, vegetables, water, and agricultural soil samples, yielding relative recoveries from 90.4 to 107 %.

5.
J Agric Food Chem ; 2024 Sep 25.
Article in English | MEDLINE | ID: mdl-39318234

ABSTRACT

Neonicotinoid insecticides (NNIs) are extensively utilized globally because of their efficient and broad-spectrum properties. However, their residues are also extensively distributed in the environment. Herein, MIL-101-SO3Na with abundant -NH- and sulfonate groups was synthesized via chloromethylation and nucleophilic substitution postmodification strategies and used to extract NNIs via solid-phase extraction. MIL-101-SO3Na was enhanced by introducing C-H···N hydrogen bonds to strengthen interaction forces and -SO3Na groups to adjust surface charge and enhance electrostatic attraction. This modification and the substantial specific surface area (998 m2·g-1) of the metal-organic framework markedly enhanced the enrichment efficiency of MIL-101. The proposed method based on MIL-101-SO3Na exhibited a minimal detection threshold (0.04-0.87 ng·L-1), an extensive linear spectrum (1-2000 ng·L-1), and notable accuracy (a variation of 3.02-11.8%) in water and drink samples. NNI concentrations between 0.25 and 24.2 ng·L-1 in fruit juice and tea samples were accurately identified using the proposed method, demonstrating its feasibility in practical applications. The postmodification of MIL-101-SO3Na is an exceptional and promising approach for the sensitive detection of ultratrace NNI levels in complex matrices.

7.
J Sep Sci ; 47(18): e202400418, 2024 Sep.
Article in English | MEDLINE | ID: mdl-39304642

ABSTRACT

Abnormal levels of catecholamine (CA) neurotransmitters and their metabolites in biological fluids can lead to various neurological disorders. Herein, a boric acid-functionalized hypercrosslinked polymer was prepared and utilized as a sorbent for the dispersive solid-phase extraction of CAs and their metabolites in rat serum. By combination with a high-performance liquid chromatography-fluorescence detector, the extraction parameters for the seven target analytes were optimized. Under the optimal extraction condition, the methodology for the quantitative analysis of CAs and their metabolites in rat serum samples was established. The limits of detection and limits of quantification were found to be in the ranges of 0.010-0.015 and 0.033-0.050 ng/mL, respectively. The results demonstrated satisfactory recoveries, with values ranging from 88.02% to 113.27%, accompanied by relative standard deviations within the range of 2.69%-9.59%. In addition, the method showed good anti-interference ability (matrix effect ranged from 2.64% to 18.07%). The developed method was validated for the determination of CAs and their metabolites in normal and Alzheimer's disease model rats' serum, which proved the promising application of the method for CAs neurotransmitter analysis in biological samples.


Subject(s)
Boric Acids , Catecholamines , Polymers , Animals , Rats , Catecholamines/blood , Boric Acids/chemistry , Polymers/chemistry , Chromatography, High Pressure Liquid , Solid Phase Extraction , Rats, Sprague-Dawley , Male , Alzheimer Disease/blood , Cross-Linking Reagents/chemistry
8.
Sci Total Environ ; 954: 176314, 2024 Sep 19.
Article in English | MEDLINE | ID: mdl-39306134

ABSTRACT

Organic Micropollutants (OMPs) might pose significant risks to aquatic life and have potential toxic effects on humans. These chemicals typically occur as complex mixtures rather than individually. Information on their co-occurrence and their association with land use is largely lacking, even in industrialized countries. Furthermore, data on the presence of OMPs in freshwater ecosystems in South America is insufficient. Consequently, we assessed the co-occurrence and distribution of OMPs, including pharmaceuticals, pesticides, personal care products, surfactants, and other industrial OMPs, in surface waters of two river basins in central Chile. We focused on identifying and ranking quantified chemicals, classifying their mode of actions, as well as correlating their occurrence with distinct land uses. We identified and quantified 311 compounds that occurred at least once in the River Aconcagua and River Maipo basins, encompassing compounds from urban, agricultural, industrial, and pharmaceutical sectors. Pharmaceuticals were the most frequently occurring chemicals, followed by pesticides, personal care and household products. OMPs with neuroactive properties dominated surface waters in Central Chile, along with OMPs known to alter the cardiovascular and endocrine systems of humans and aquatic animals. Finally, we observed positive correlations between agricultural and urban land uses and OMPs. Our findings represent a step forward in extending current knowledge on the co-occurrence patterns of OMPs in aquatic environments, particularly in developing countries of the southern hemisphere.

9.
Article in English | MEDLINE | ID: mdl-39303518

ABSTRACT

In this work, an imidazolium-based poly(ionic liquid) (poly(1-dodecyl-3-vinyl-imidazolium bromide) functionalized magnetic three-dimensional graphene oxide (Fe3O4@3D-GO@poly(ImC12+Br-)) was synthesized via a vacuum freezing-drying method and used as a magnetic solid phase extraction (MSPE) adsorbent for the efficient extraction of pyrethroid pesticides from tea samples. The prepared Fe3O4@3D-GO@poly(ImC12+Br-) was confirmed by scanning electron microscopy (SEM), Fourier transform infrared spectrometry (FT-IR), vibrating sample magnetometer (VSM) and X-ray photoelectron spectrogram (XPS). Due to its large specific surface area and the ability to offer multiple intermolecular interactions, including π-π stacking, hydrophobic and hydrogen bond interactions, the prepared Fe3O4@3D-GO@poly(ImC12+Br-) showed high extraction efficiency for pyrethroids. The experimental parameters were optimized by a combination of single-factor method and Box-Behnken design to improve the extraction efficiency. Under the optimum conditions, coupled with high performance liquid chromatography (HPLC), a sensitive analytical method was developed for the determination of pyrethroids, and the proposed method showed wide linear ranges (1.00-100 µg L-1) with correlation coefficients (R) ranging from 0.9980 to 0.9994, low limits of detection (0.100 µg L-1) and good repeatability with intra-day relative standard deviations (RSDs) in the range of 2.90-5.53 % and inter-day RSDs in the range of 1.83-7.76 %. Moreover, the developed method was successfully applied to the determination of pyrethroids in tea samples and satisfactory recoveries ranging from 82.37 % to 114.34 % were obtained. The results showed that the developed Fe3O4@3D-GO@poly(ImC12+Br-) was an ideal, effective and selective material for the extraction and enrichment of pyrethroids from tea samples.

10.
Food Chem ; 463(Pt 2): 141312, 2024 Sep 16.
Article in English | MEDLINE | ID: mdl-39305668

ABSTRACT

In this work, new sorbents for the purification of anthocyanin-rich extracts were evaluated. Copolymers of 4-vinylpyridine crosslinked with trimethylolpropane trimethacrylate (poly(4VP-co-TRIM)) or 1,4-dimethacryloyloxybenzene (poly(4VP-co-14DMB)) were tested for their potential to capture polyphenols. Copolymers were obtained by seed swelling polymerization in the form of microspheres with permanent porous structure - attractive features of sorbents used for sample purification by dispersive solid phase extraction. The microspheres were characterized by AFM, elemental analysis, SEM, and nitrogen adsorption-desorption method. Their capacity to remove polyphenols was evaluated using spectrophotometry, HPLC-DAD, and LC-MS/MS. For proof-of-concept, the aqueous extracts of berries classified into three different groups regarding their anthocyanin composition (strawberries, raspberries, blackcurrants) were selected. It was found that studied microspheres adsorbed flavonoids more effectively compared to primary secondary amine and graphitized carbon black. Copolymers of 4-vinylpyridine also capture anthocyanins and might be used for the purification of extracts of fruits before LC-MS/MS analysis to reduce the matrix effect.

11.
Bull Environ Contam Toxicol ; 113(4): 42, 2024 Sep 21.
Article in English | MEDLINE | ID: mdl-39306638

ABSTRACT

In the present paper, the assessment of vortex-assisted dispersive magnetic solid-phase extraction using amino-functionalized mesoporous combined with direct magnetic sorbent sampling (DMSS) in flame or furnace atomic absorption spectrometry (FAAS or FF-AAS) was demonstrated for highly sensitive silver determination in water samples. The developed method showed significant enrichment factors compared to conventional pneumatic nebulization by FAAS, 607 for DMSS-FF-AAS and 114 for DMSS-FAAS. The analytical curve showed linearity in the range from 5.0 to 70.0 µg L- 1 and 1.0 to 15.0 µg L- 1 and limits of detection of 0.59 and 0.09 µg L- 1 for DMSS-FAAS and DMSS-FF-AAS, respectively. The intra and inter-day precision evaluated as a percentage of the relative standard deviation (RSD,%) ranged from 1.89 to 4.71% for levels of 25.0 and 65.0 µg L- 1. The method was applied in different kinds of water samples without matrix effects, yielding recovery values from 90 to 110%.


Subject(s)
Silver , Solid Phase Extraction , Spectrophotometry, Atomic , Water Pollutants, Chemical , Solid Phase Extraction/methods , Silver/chemistry , Water Pollutants, Chemical/analysis , Environmental Monitoring/methods , Limit of Detection
12.
Mikrochim Acta ; 191(10): 620, 2024 Sep 25.
Article in English | MEDLINE | ID: mdl-39320493

ABSTRACT

Magnetic particle spray mass spectrometry (MPS-MS), an innovative ambient ionization technique proposed by our research group, was employed to determine beta-blockers in human plasma samples. A dispersive solid phase extraction of atenolol, metoprolol, labetalol, propranolol, nadolol, and pindolol was carried out using magnetic molecularly imprinted polymer (M-MIP) particles that were attached to the tip of a metal probe, which was placed in the mass spectrometer inlet. A solvent (1% formic acid in methanol) was dispensed on the particles, and the Taylor cone was formed around them (in high voltage). The analytes were desorbed/ionized and determined by a triple quadrupole mass spectrometer. M-MIP was synthesized with oxprenolol as a pseudo-template, demonstrating good selectivity to beta-blockers compared with no-analog molecules, with an adsorption process occurring in monolayers, according to isotherm studies. Kinetic experiments indicated chemisorption as the predominant M-MIP/analyte interaction. The analytical curves were linear (R2 > 0.98), and the limit of quantification was 3 µg L-1 for all the analytes. Limits of detection ranged from 0.64 to 2.41 µg L-1. Precisions (relative standard deviation) and accuracies (relative error) ranged from 3.95 to 21.20% and -17.05 to 18.93%, respectively. MPS-MS proved to be a simple, sensitive, and advantageous technique compared with conventional approaches. The analyses were fast, requiring no chromatographic separation and without ionic suppression. The method is aligned with green chemistry principles, requiring minimal sample, solvent, and sorbent amounts. MPS-MS successfully integrates sample preparation and ambient ionization mass spectrometry and holds great potential for application with other sorbents, samples, and analytes.


Subject(s)
Adrenergic beta-Antagonists , Adrenergic beta-Antagonists/blood , Adrenergic beta-Antagonists/chemistry , Humans , Limit of Detection , Molecularly Imprinted Polymers/chemistry , Solid Phase Extraction/methods , Mass Spectrometry/methods , Adsorption
13.
Food Chem X ; 24: 101810, 2024 Dec 30.
Article in English | MEDLINE | ID: mdl-39310888

ABSTRACT

A novel ultrasound-assisted magnetic solid-phase extraction coupled with gas chromatography-mass spectrometry (US-MSPE-GC/MS) was developed to detect trace amounts of polycyclic aromatic hydrocarbons (PAHs) in tomato paste, using a magnetic biochar adsorbent derived from nectarine cores. The highest extraction recovery was attained under 10 mg adsorbent mass, 30 min extraction time, 9 % (w/v) sodium chloride, and elution with 200 µL of dichloromethane. Under optimum conditions, the method demonstrated excellent linearity (R2 > 0.992) across a wide concentration range (0.01-100 ng g-1) with high sensitivity (LODs: 0.028-0.053 ng g-1, LOQs: 0.094-0.176 ng g-1) and good repeatability (RSDs <5.96 %). The application of the US-MSPE-GC/MS method was tested on four brands of real tomato paste and no PAHs were detected in unspiked samples, indicating no background contamination. This method showed high relative recoveries 88.03-98.52 %) and good reproducibility (<9.19 %.) at two concentration levels, confirming its effectiveness for PAH analysis in real samples.

14.
Food Chem X ; 24: 101795, 2024 Dec 30.
Article in English | MEDLINE | ID: mdl-39310895

ABSTRACT

Furfural compounds, including 5-hydroxymethylfurfural, furfural, and 5-methylfurfural, are common in foods and pose health risks. This study presents a pipette-tip solid-phase extraction with in-situ derivatization (PT-KF-SPE/ISD) method for rapid analysis of furfural compounds in various food matrices. Utilizing natural kapok fiber as an efficient adsorbent, this method integrates extraction and derivatization into a single step via a simple pull-push operation. Derivatization with 2,4-dinitrophenylhydrazine increases the hydrophobicity and ultraviolet absorption of furfural compounds, enabling sensitive liquid chromatography-ultraviolet detection. The method shows good linearity, sensitivity, and reproducibility, with limits of detection in ranges of 3.9-6.0 ng/mL. Real sample analysis confirms its applicability in detecting furfural compounds in beverages and herbal products, offering a reliable and eco-friendly solution for food safety and quality control. Five greenness assessment metrics demonstrate the method's excellent environmental friendliness. This approach highlights the advantages of combining natural adsorbents with in-situ derivatization for efficient food analysis.

15.
J Hazard Mater ; 479: 135653, 2024 Nov 05.
Article in English | MEDLINE | ID: mdl-39217939

ABSTRACT

In this study, a novel COFTABT@COFTATp modified magnetic MXene composite (CoFe2O4 @Ti3C2 @COFTABT@COFTATp) was synthesized by Schiff base reaction and irre-versible enol-keto tautomerization, and employed to establish a sensitive monitoring method for six thiophene compounds in oilfield produced water samples based on magnetic solid-phase extraction (MSPE) prior to gas chromatography coupled with a triple quadruple mass spectrometer (GC-MS/MS). The designed magnetic materials exhibited unexpected enrichment ability to target thiophene compounds and achieved good extraction efficiencies ranging from 83 % to 98 %. The developed MSPE/GC-MS/MS method exhibited good linearity in the range of 0.001-100 µg L-1, and obtained lower limits of detection ranging from 0.39 to 1.9 ng L-1. The spiked recoveries of thiophene compounds obtained in three oilfield produced water samples were over the range of 96.26 %-99.54 % with relative standard deviations (RSDs) less than 3.7 %. Notably, benzothiophene, 4-methyldibenzothiophene and 4,6-dimethyldibenzothiophene were detected in three oilfield-produced water samples. Furthermore, the material still kept favorable stability after six recycling experiments. The adsorption kinetics, adsorption isotherms as well as adsorption thermodynamics of thiophene compounds were investigated in detail to provide insight into the mechanisms. Overall, the present work contributed a promising strategy for designing and synthesizing new functionalized materials for the enrichment and detection of typical pollutants in the environment.

16.
J Hazard Mater ; 479: 135685, 2024 Nov 05.
Article in English | MEDLINE | ID: mdl-39226690

ABSTRACT

Based on the important feature of sulfur with excellent selectivity toward selenite in the presence of selenate, a simple and low-cost adsorbent of solid phase extraction known as sulfur loading activated carbon (SAC-6) was successfully prepared and applied for selenite (Se(IV)) analysis in water. Microstructure and morphological characteristics of SAC-6 had been identified by XRD, TEM, BET and FT-IR. In the static adsorption experiments, Se(IV) could be separated in a wide range of pH values (pH=3-11). The retention process of Se(IV) onto SAC-6 was characterized as spontaneous exothermic reaction. An obvious change of adsorption mechanism occurred in static and dynamic adsorption processes shown that the behaviors followed monolayer and hybrid adsorption. The theoretical maximum adsorption capacity of SAC-6 calculated by Langmuir-Freundlich was 13.48 mg/g. The microcolumn filled with SAC-6 was applied to extract Se(IV) in water solution. The detection limit of Se(IV) analytical procedure was confirmed as 0.27 µg/L within a linear range of 10-1000 µg/L. A good precision with relative standard deviation of 1.34 % (100 µg/L, n = 6) was achieved. The high adaptability and accuracy of SAC-6 microcolumn was validated by analyzing natural water samples and certified reference materials. Our work successfully excavated the application value of the sulfur selectivity, and also provided a new adsorbent for Se(IV) extraction and analysis.

17.
Chemistry ; : e202402221, 2024 Sep 09.
Article in English | MEDLINE | ID: mdl-39250519

ABSTRACT

This work introduces a novel method of recovering bioactive berry natural products (BNPs) using solid phase extraction with metal-organic frameworks (MOF-SPE). Two pyrene-based MOFs with different structural topologies, Al-PyrMOF and Zr-NU-1000, were evaluated for their ability to capture and desorb BNPs, including ellagic acid, quercetin, gallic acid, and p-coumaric acid. Time-dependent BNP uptake via dispersive SPE revealed that NU-1000 outperformed Al-PyrMOF in capturing all BNPs. Our findings show NU-1000 demonstrated a higher and more consistent BNP capture profile, achieving over 90% capture of all BNPs within 36 hours, with only a 9% variation between the most and least effectively captured BNPs. In contrast, Al-PyrMOF, displayed a staggered uptake profile, with a significant 53% difference in capture efficiency between the most and least effectively captured BNP. However, when a BNP mixture was used at a loading concentration of 50 µg/mL, Al-PyrMOF outperformed NU-1000, capturing over 70% of all BNPs. Al-PyrMOF also exhibited improved BNP recovery, with a minimum of two-fold greater amount recovered for all BNPs. Further testing with a BNP mixture at a concentration of 15 µg/mL demonstrated that Al-PyrMOF efficiently concentrated all BNPs, achieving a maximum extraction factor of 2.71 observed for quercetin.

18.
Anal Chim Acta ; 1326: 343138, 2024 Oct 16.
Article in English | MEDLINE | ID: mdl-39260916

ABSTRACT

BACKGROUND: Sulfonamide (SA) residues in food of animal origin possess a potential threat to human health and environment. However, due to the polar and ionic characteristics and trace level of SAs and the complexity of food matrices, direct measurement of SAs in these samples is still very difficult. Development of efficient sample pretreatment method for sensitive and selective extraction of trace SAs is of great significance and urgently desired. Therefore, rational design and synthesizing advanced and selective extractants is quite important. RESULTS: In this work, a novel phenazine-based microporous organic network (MON) named TEPM-DP is reasonably synthesized and employed as a packing material for selective solid phase extraction (SPE) and sensitive determination of four typical SAs in milk samples. Phenazine-based monomer with aromatic and heteroaromatic ring and numerous N atoms is chosen to construct TEPM-DP adsorbent to provide π-π, hydrogen bonding, hydrophobic, and electrostatic extraction sites for SAs. The proposed method owns wide linear ranges, low limits of detection, high enrichment factors, and good precisions and recoveries for SAs in complex milk samples. The recoveries of SAs on TEPM-DP are much higher than those of commercial C18 and activated carbon. The extraction mechanisms are also elucidated via FT-IR, XPS, and comparative experiments. SIGNIFICANCE: This work reports the first example of design and synthesizing phenazine-based MON in SPE via a simple and rapid solvothermal method. The results reveal the great prospects of TEPM-DP for enriching polar and ionic SAs in complex samples and uncover the potency of phenazine-based MON in sample pretreatment, which will promote the development of MON.


Subject(s)
Milk , Phenazines , Solid Phase Extraction , Sulfonamides , Phenazines/chemistry , Milk/chemistry , Animals , Sulfonamides/analysis , Sulfonamides/isolation & purification , Solid Phase Extraction/methods , Porosity , Limit of Detection , Adsorption , Food Contamination/analysis
19.
Article in English | MEDLINE | ID: mdl-39264496

ABSTRACT

Perfluoroalkyl substances (PFAS) are chemical compounds that have been widely used in industry and manufacture. Occurrence, together with persistence and recent toxicological effects data, has promoted the regulation of 20 PFAS (carboxylic and sulfonic) acids in drinking water through the recent Directive 2020/2184/EU. This Regulation included PFAS with different carbon chain lengths (from C4 to C13) and limited the total PFAS concentration (as sum) to a maximum of 0.1 µg/L, for which law-enforcement analytical methods are required. In this work, three different methodologies have been developed and evaluated as regards their performance to determine those 20 PFAS in tap and bottled water, based on on-line and off-line solid-phase extraction (SPE) and direct injection. In all cases, ultra-high pressure liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was used as a determination technique. Off-line SPE with Oasis Weak Anion Exchange (WAX) cartridges provided the best results in terms of limits of quantification (LOQ ≤ 0.3 ng/L) and accuracy (R ≥ 70%) in drinking water samples. On-line SPE and direct injection presented some drawbacks such as background contamination problems and lower accuracies for the least polar compounds. This off-line SPE methodology was then applied to the analysis of 46 drinking water samples (11 commercial bottled samples, 23 Spanish and 12 international tap water samples). Ten PFAS were quantified in such samples at concentrations and detection frequencies ranging from 0.1 to 20.1 ng/L and 2 to 91%, respectively. However, the sum concentration did not surpass the established limit in any sample.

20.
Food Chem ; 463(Pt 2): 141267, 2024 Sep 12.
Article in English | MEDLINE | ID: mdl-39288463

ABSTRACT

Co-extraction of multiple types of target substances is the key to achieve high throughput detection. In this work, PDA@MOF-808/PAN NFsM was prepared by co-modified polyacrylonitrile nanofiber membrane (PAN NFsM) with polydopamine (PDA) and metal-organic framework-808 (MOF-808), and its potential as a solid-phase extraction (SPE) adsorbent was investigated by using the most typical nine veterinary drug residues in eggs and chicken as model target substances. The results show that PDA@MOF-808/PAN NFsM could effectively co-extract all the target substances (adsorption efficiency ranged from 81.46 % to 96.78 %), and had good capability of sample matrix purification (matrix effect was lower than -15.26 %), so a new SPE method has been established. Combined with UPLC-MS/MS, the detection limits were 0.3 to 3.1 µg/kg, the recoveries were between 71.02 % and 106.48 %, and the relative standard deviations were lower than 12.03 %, indicating that the method has considerable good sensitivity, accuracy and precision.

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