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1.
J Clin Lab Anal ; : e25107, 2024 Sep 30.
Artigo em Inglês | MEDLINE | ID: mdl-39345045

RESUMO

BACKGROUND: Catecholamines (epinephrine; norepinephrine; and dopamine) and their O-methylated metabolites (metanephrine; normetanephrine; and 3-methoxytyramine) are biomarkers for pheochromocytoma and paraganglioma. Liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) was recommended by Endocrine Society for detecting these compounds. The influence of blood collection tubes on the analysis of the six analytes by LC-MS/MS was not thoroughly investigated, which we want to clarify in our study. METHODS: Blood samples of healthy individuals were collected into serum, lithium heparin, and K2EDTA plasma tubes separately. Samples were subjected to solid phase extraction and then analyzed by LC-MS/MS. The retention behavior and assay performance of the six analytes were assessed for samples from different collection containers. The impacts of potassium and sodium as the counter ions of EDTA on the retention time and matrix effect were also studied. RESULTS: Compared with O-methylated metabolites, the results for catecholamines were more affected by the collection tubes, especially for norepinephrine, which displayed severely suppressed signal and very low extraction efficiency in K2EDTA plasma. Changing the counter ion of EDTA from potassium to sodium dramatically changed the retention behavior and matrix effect of norepinephrine. CONCLUSIONS: It is necessary to evaluate blood collection tubes for catecholamines and their O-methylated metabolites analyzed by LC-MS/MS. In addition, attention should also be paid when the anticoagulant counter ion was changed.

2.
Molecules ; 29(16)2024 Aug 17.
Artigo em Inglês | MEDLINE | ID: mdl-39202981

RESUMO

Among the various compounds regarded as emerging contaminants (ECs), pharmaceuticals and personal care products (PPCPs) are of particular concern. Their continuous release into the environment has a negative global impact on human life. This review summarizes the sources, occurrence, persistence, consequences of exposure, and toxicity of PPCPs, and evaluates the various analytical methods used in the identification and quantification of PPCPs in a variety of solid and liquid environmental matrices. The current techniques of choice for the analysis of PPCPs are state-of-the-art liquid chromatography coupled to mass spectrometry (LC-MS) or tandem mass spectrometry (LC-MS2). However, the complexity of the environmental matrices and the trace levels of micropollutants necessitate the use of advanced sample treatments before these instrumental analyses. Solid-phase extraction (SPE) with different sorbents is now the predominant method used for the extraction of PPCPs from environmental samples. This review also addresses the ongoing analytical method challenges, including sample clean-up and matrix effects, focusing on the occurrence, sample preparation, and analytical methods presently available for the determination of environmental residues of PPCPs. Continuous development of innovative analytical methods is essential for overcoming existing limitations and ensuring the consistency and diversity of analytical methods used in investigations of environmental multi-class compounds.


Assuntos
Cosméticos , Extração em Fase Sólida , Preparações Farmacêuticas/análise , Preparações Farmacêuticas/química , Cosméticos/análise , Cosméticos/química , Extração em Fase Sólida/métodos , Cromatografia Líquida/métodos , Monitoramento Ambiental/métodos , Humanos , Poluentes Ambientais/análise , Espectrometria de Massas em Tandem/métodos
3.
Sci Total Environ ; 950: 175304, 2024 Nov 10.
Artigo em Inglês | MEDLINE | ID: mdl-39127205

RESUMO

Nonylphenols (NPs) are confirmed endocrine disruptors that are banned in many countries due to correlations with human cancers. NPs pollution in surfactant oilfield chemicals (OFCs) has become an important environmental safety issue. It is significant to establish a simple, accurate and low-cost method for detection of NPs in OFCs. In this research, computer-aided molecular design technology was utilized to design NPs haptens. High affinity monoclonal antibodies against NPs were obtained using a matrix effect-enhanced screening method, with an IC50 value of 183.01 ng/mL. A colloidal gold immunochromatography assay (ICA) for detection of NPs enabled rapid on-site detection of large volumes of OFCs. Under optimal conditions, the limit of detection was 0.72-1.82 mg/kg, with a detection range of 4.49-191.28 mg/kg. The recovery was 84 %-104 %, with coefficients of variation < 13 %. As confirmed by high-performance liquid chromatography of natural positive OFCs samples, the proposed colloidal gold ICA demonstrated accuracy and reliability, with potential for fast and economical on field test.


Assuntos
Fenóis , Tensoativos , Fenóis/análise , Tensoativos/química , Imunoensaio/métodos , Monitoramento Ambiental/métodos , Disruptores Endócrinos/análise , Campos de Petróleo e Gás
4.
Se Pu ; 42(9): 856-865, 2024 Sep.
Artigo em Chinês | MEDLINE | ID: mdl-39198944

RESUMO

Neonicotinoid pesticides are a relatively new class of pesticides that have garnered significant attention owing to their potential ecological risks to nontarget organisms. A method combining solid phase extraction with liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) was developed for the rapid and accurate detection of eight neonicotinoid pesticides (dinotefuran, E-nitenpyram, thiamethoxam, clothianidin, imidacloprid, imidaclothiz, acetamiprid, and thiacloprid) in wastewater. The chromatographic mobile phase and MS parameters were selected, and a single-factor method was used to determine the optimal column type, extraction volume, sample loading speed, and pH for SPE. The optimal parameters were as follows: column type, HLB column (500 mg/6 mL); sample extraction volume, 500 mL; sample loading speed, 10 mL/min; and sample pH, 6-8. The matrix effects of the wastewater samples were reduced by optimizing the chromatographic gradient-elution program, examining the dilution factor of the samples, and using the isotope internal standard calibration method. Prior to analysis, the wastewater samples were diluted 5-fold with ultrapure water for pretreatment. Subsequently, 2 mmol/L ammonium acetate aqueous solution containing 0.1% (v/v) formic acid and methanol was used as mobile phases for gradient elution on a ZORBAX Eclipse Plus C18 column (100 mm×2.1 mm, 1.8 µm). The samples were quantified using positive-ion multiple reaction monitoring (MRM) mode for 10 min. Imidacloprid-d4 was used as the isotope internal standard. The SPE process was further optimized by applying response surface methodology to select the type and mass of rinsing and elution solvents. The optimal pretreatment of the SPE column included rinsing with 10% methanol aqueous solution and elution with methanol-acetonitrile (1∶1, v/v) mixture (7 mL). The eight neonicotinoid pesticides showed satisfactory linearity within the relevant range, with linear correlation coefficients (r) all greater than 0.9990. The method detection limits (MDLs) ranged from 0.2 to 1.2 ng/L, and the method quantification limits (MQLs) ranged from 0.8 to 4.8 ng/L. The average recoveries of the eight neonicotinoid pesticides were in the range of 82.6%-94.2% at three spiked levels, with relative standard deviations (RSDs) ranging from 3.9% to 9.4%. Finally, the optimized method was successfully applied to analyze wastewater samples collected from four sewage treatment plants. The results indicated that the eight neonicotinoid pesticides could be generally detected at concentrations ranging from not detected (ND) to 256 ng/L. The developed method has a low MDL and high accuracy, rendering it a suitable choice for the trace detection of the eight neonicotinoid pesticides in wastewater when compared with other similar methods. The proposed method can be utilized to monitor the environmental impact and assess the potential risks of neonicotinoid pesticides in wastewater, thus promoting the protection of nontarget organisms and the sustainable use of these pesticides in agriculture.


Assuntos
Neonicotinoides , Nitrocompostos , Extração em Fase Sólida , Espectrometria de Massas em Tandem , Águas Residuárias , Poluentes Químicos da Água , Espectrometria de Massas em Tandem/métodos , Extração em Fase Sólida/métodos , Águas Residuárias/química , Águas Residuárias/análise , Neonicotinoides/análise , Poluentes Químicos da Água/análise , Cromatografia Líquida/métodos , Nitrocompostos/análise , Tiametoxam/análise , Guanidinas/análise , Tiazóis/análise , Praguicidas/análise , Tiazinas/análise , Oxazinas/análise
5.
Environ Sci Pollut Res Int ; 31(39): 51253-51266, 2024 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-39106010

RESUMO

Phthalic acid esters (PAEs) are emerging pollutants that need to be analyzed precisely. Chromatography-based determination of PAE content in soils are frequently affected by matrix effect, which may limit the quantification of different kinds of PAEs from different types of soil. Here we optimized a QuEChERS protocol combined with gas chromatography-mass spectrometry (GC-MS) for simultaneous determination of 16 PAEs in different soils. PAEs in different type of soils (fluvo-aquic soil, red soil, and black soil) were extracted with acetonitrile followed by GC-MS detection based on quantitative ion internal standard method. All 16 PAEs showed excellent linear relationships with mass peak areas (R2 > 0.99). The limits of detection (LOD) and limits of quantitation (LOQ) of all the samples were in the range of 0.91-66.97 µg/kg and 2.7-200.9 µg/kg, respectively. The accurate test at 0.5, 0.1, and 1.0 mg/kg spiking level recorded recovery rate between 80.11% and 100.99% with relative standard deviations (RSDs) ranging from 0.37 to 8.50% in tested matrices. No significant matrix effect was observed for most tested PAEs. This is a simple method with high sensitivity and strong stability, which is suitable and reproducible for quantifying large number of PAEs in different types of soil.


Assuntos
Ésteres , Cromatografia Gasosa-Espectrometria de Massas , Ácidos Ftálicos , Poluentes do Solo , Solo , Ácidos Ftálicos/análise , Solo/química , Ésteres/análise , Poluentes do Solo/análise , Limite de Detecção
6.
Molecules ; 29(15)2024 Jul 31.
Artigo em Inglês | MEDLINE | ID: mdl-39125042

RESUMO

In ion chromatography studies, the matrix effect of other inorganic ions present in the sample is a well-known phenomenon. In this work, the behavior of inorganic and organic ions was studied in a system overloaded with ammonium ions. The ammonium ions came from a solution of ammonium hydroxide in various concentrations (0.25-1.25%). In this system, which was significantly overloaded with ammonium ions, the behavior of three ions were tested (lithium, tris, and sodium cations). The measurements were performed at different eluent concentrations (6-17 mM), chromatographic column temperatures (25-40 °C), and injected volumes (15-40 µL). The retention times of sodium and lithium ions increased with increasing amounts of injected ammonium, while tris remained essentially unchanged, indicating that the resolution of these ions can be influenced by varying the concentration of the matrix. The results suggested that the observed effect was due to a combination of the pH change caused by the injected matrix, the dissociation of tris ions, the dissociation of the carbocylic ion-exchange groups of stationary phase, the change in buffer capacity, and the amount of ammonium ion introduced. It has been shown that in a well-designed experiment, the addition of ammonium hydroxide to the sample at concentrations greater than 1% can improve the efficiency of organic and inorganic cation separation. It was found that 8 mM methanesulfonic acid eluent, 30 °C, 1% ammonium hydroxide matrix concentration, and 25 µL injection were optimal for the baseline separation of tris and sodium ions on the high-capacity Dionex CS16 column. These ions could not be separated on this column without the presence of the ammonium matrix.

7.
Food Chem ; 459: 140416, 2024 Nov 30.
Artigo em Inglês | MEDLINE | ID: mdl-39024877

RESUMO

Matrix effects limit the application of surface-enhanced Raman scattering (SERS) technology in the field of food safety. This study elucidated it from the perspective of protein corona by employing a model system for melamine SERS detection in milk. Compared with the melamine standard solution, higher detection limits (1 mg/L and 10 mg/L) are observed in milk matrix. The melamine signal exhibits an 80% reduction in whey protein solution, suggesting that protein has a significant impact on SERS signals. The changes in particle size, zeta potential and UV-vis spectra indicate the AuNPs interact with whey protein. Forming protein corona inhibits the melamine-induced AuNPs aggregation, reducing the number of 'hot spot' and the adsorption of melamine on AuNPs (from 0.28 mg/L to 0.07 mg/L), which may be responsible for signal loss. The found matrix effect from protein corona provides new insights for developing strategies about reducing matrix effect in SERS application.


Assuntos
Contaminação de Alimentos , Ouro , Leite , Coroa de Proteína , Análise Espectral Raman , Triazinas , Triazinas/química , Triazinas/análise , Análise Espectral Raman/métodos , Animais , Leite/química , Contaminação de Alimentos/análise , Coroa de Proteína/química , Coroa de Proteína/análise , Ouro/química , Nanopartículas Metálicas/química , Bovinos
8.
Mycotoxin Res ; 2024 Jul 17.
Artigo em Inglês | MEDLINE | ID: mdl-39017819

RESUMO

Yogurt, a milk-derived product, is susceptible to mycotoxin contamination. While various methods have been developed for the analysis of dairy products, only a few have been specifically validated for yogurt. In addition, these methods are primarily focus on detecting aflatoxins and zearalenone. This study aimed to conduct a preliminary investigation into the presence of regulated, emerging, and modified mycotoxins in natural and oat yogurts available in the Spanish market. For this, a QuEChERS-based extraction method was optimized and then validated to detect and quantify 32 mycotoxins using ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The method was in-house validated for the analysis of natural and oat yogurt in terms of linearity, matrix effect, sensitivity, accuracy, and precision. Satisfactory performance characteristics were achieved; for most of the analytes, LOQs were lower than 2 ng/g, and recoveries ranged from 60 to 110% with a precision, expressed as the relative standard deviation of the recovery, lower than 15%. Subsequently, the validated method was applied to analyze commercial yogurt samples, revealing a notable incidence of beauvericin and enniatins, with some analogues found in up to 100% of the samples. Alternariol methyl ether was also frequently found, appearing in 50% of the samples. Additionally, the study identified regulated toxins such as fumonisins, ochratoxin A , and HT-2 toxin. These results provide new incidence data in yogurt, raising concerns about potential health risks for consumers.

9.
J Sci Food Agric ; 2024 Jul 23.
Artigo em Inglês | MEDLINE | ID: mdl-39041432

RESUMO

BACKGROUND: Hydroxytyrosol (HT) is a bioactive compound present in a limited number of foods such as wines, olives, and olive oils. During alcoholic fermentation, yeast converts aromatic amino acids into higher alcohols such as tyrosol, which can undergo hydroxylation into HT. The aim of this study was to validate an analytical method using ultra performance liquid chromatography coupled with mass spectrometry (UPLC/MS-MS) to quantify HT and its precursors (tyrosine, hydroxyphenylpyruvic acid, hydroxyphenylacetaldehyde, 4-hydroxyphenylacetic acid, and tyrosol) in wines. Their occurrence was evaluated in a total of 108 commercial Spanish wine samples. RESULTS: The validated method simultaneously determined both HT and its precursors, with adequate limits of detection between 0.065 and 21.86 ng mL-1 and quantification limits between 0.199 and 66.27 ng mL-1 in a 5 min run. The concentration of HT in red wines was significantly higher (0.12-2.24 mg L-1) than in white wines (0.01-1.27 mg L-1). The higher the alcoholic degree, the higher was the content of HT. The bioactive 4-hydroxyphenylacetic acid was identified in Spanish wines for the first time at 3.90-127.47 mg L-1, being present in all the samples. CONCLUSION: The highest HT concentrations were found in red wines and in wines with higher ethanol content. These data are useful for a further estimation of the intake of these bioactive compounds and to enlarge knowledge on chemical composition of wines. © 2024 The Author(s). Journal of the Science of Food and Agriculture published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry.

10.
Food Res Int ; 188: 114510, 2024 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-38823887

RESUMO

The aim of this study was to explore the copigmentation effect of gallic acid on red wine color and to dissect its mechanism at the molecular level. Three-dimensional studies, e.g., in model wine, in real wine and in silico, and multiple indicators, e.g., color, spectrum, thermodynamics and phenolic dynamics, were employed. The results showed that gallic acid significantly enhanced the color quality and stability of red wine. Physico-chemical interactions and chemical transformations should be the most likely mechanism, and physico-chemical interactions are also a prerequisite for chemical transformations. QM calculations of the physico-chemical interactions proved that the binding between gallic acid and malvidin-3-O-glucoside is a spontaneous exothermic reaction driven by hydrogen bonding and dispersion forces. The sugar moiety of malvidin-3-O-glucoside and the phenolic hydroxyl groups of gallic acid affect the formation of hydrogen bonds, while the dispersion interaction was related to the stacking of the molecular skeleton.


Assuntos
Antocianinas , Cor , Ácido Gálico , Glucosídeos , Ligação de Hidrogênio , Termodinâmica , Vinho , Ácido Gálico/química , Vinho/análise , Glucosídeos/química , Antocianinas/química , Teoria Quântica , Fenóis/química
11.
J Pestic Sci ; 49(2): 65-76, 2024 May 20.
Artigo em Inglês | MEDLINE | ID: mdl-38882703

RESUMO

The matrix effects (ME) in simultaneous analysis of pesticide residue using liquid chromatography-tandem mass spectrometry (LC-MS/MS) were evaluated by comparing the slopes of matrix-matched and reagent-only calibrations of four types of vegetable samples. Both the sampling and measurement variances of the ME were also determined using one-way analysis of variance. Substantial ion suppression (ME<-20%) was observed in komatsuna, spinach, and tomato when a modified Japanese official method was implemented. The ME magnitude varied significantly due to sample variability for some pesticides, but it varied by no more than 4% as a result of analytical procedure variance. This study also showed that the addition of stable isotope-labeled internal standards at low concentrations improved the recovery of pesticides from samples at various residue levels. The findings of this study highlight the importance and practical application of internal standards and the matrix-matched calibration method in residue analysis using LC-MS/MS.

12.
Anal Bioanal Chem ; 416(20): 4503-4517, 2024 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-38896239

RESUMO

Residues of various highly polar pesticides and their metabolites are commonly found in numerous food products. Some of these compounds, such as glyphosate, are not only used in large amounts in agriculture, but are also controversially discussed in public. Here, we present a method, employing ion chromatography (IC) coupled to tandem mass spectrometry (IC-MS/MS), for the analyses of glyphosate, aminomethyl phosphonic acid (AMPA), N-acetyl-glyphosate (NAGly), fosetyl, and 10 further highly polar pesticides and metabolites in various plant and animal matrices following a minimal sample preparation by means of the QuPPe method. Thorough investigations showed that an AS19 column enabled the analysis of all 14 compounds within 30 min. The best sensitivity could be obtained with the make-up solvent acetonitrile being admixed to the mobile phase at a 1:2 flow rate ratio. Matrix effects were thoroughly studied in terms of ion suppression and retention time shifts. Conductivity detection was used to monitor elution profiles of matrix co-extractives in comparison with matrix effect profiles obtained by continuous post-column infusion of a mix with 13 highly polar pesticides and metabolites. These tests indicated that a fivefold dilution of QuPPe extracts was suitable for the routine analysis of samples for MRL-conformity, as it considerably reduced matrix effects maintaining sufficient sensitivity and high recovery rates in eight different commodities. The suitability of the final method for its application in routine analysis was verified by the analysis of >130 samples containing incurred residues where the results were compared with two existing LC-MS/MS methods.


Assuntos
Contaminação de Alimentos , Resíduos de Praguicidas , Espectrometria de Massas em Tandem , Espectrometria de Massas em Tandem/métodos , Animais , Contaminação de Alimentos/análise , Resíduos de Praguicidas/análise , Praguicidas/análise , Ânions/análise , Análise de Alimentos/métodos , Cromatografia por Troca Iônica/métodos , Plantas/química
13.
Se Pu ; 42(6): 508-523, 2024 Jun.
Artigo em Chinês | MEDLINE | ID: mdl-38845512

RESUMO

Given continuous improvements in industrial production and living standards, the analysis and detection of complex biological sample systems has become increasingly important. Common complex biological samples include blood, serum, saliva, and urine. At present, the main methods used to separate and recognize target analytes in complex biological systems are electrophoresis, spectroscopy, and chromatography. However, because biological samples consist of complex components, they suffer from the matrix effect, which seriously affects the accuracy, sensitivity, and reliability of the selected separation analysis technique. In addition to the matrix effect, the detection of trace components is challenging because the content of the analyte in the sample is usually very low. Moreover, reasonable strategies for sample enrichment and signal amplification for easy analysis are lacking. In response to the various issues described above, researchers have focused their attention on immuno-affinity technology with the aim of achieving efficient sample separation based on the specific recognition effect between antigens and antibodies. Following a long period of development, this technology is now widely used in fields such as disease diagnosis, bioimaging, food testing, and recombinant protein purification. Common immuno-affinity technologies include solid-phase extraction (SPE) magnetic beads, affinity chromatography columns, and enzyme linked immunosorbent assay (ELISA) kits. Immuno-affinity techniques can successfully reduce or eliminate the matrix effect; however, their applications are limited by a number of disadvantages, such as high costs, tedious fabrication procedures, harsh operating conditions, and ligand leakage. Thus, developing an effective and reliable method that can address the matrix effect remains a challenging endeavor. Similar to the interactions between antigens and antibodies as well as enzymes and substrates, biomimetic molecularly imprinted polymers (MIPs) exhibit high specificity and affinity. Furthermore, compared with many other biomacromolecules such as antigens and aptamers, MIPs demonstrate higher stability, lower cost, and easier fabrication strategies, all of which are advantageous to their application. Therefore, molecular imprinting technology (MIT) is frequently used in SPE, chromatographic separation, and many other fields. With the development of MIT, researchers have engineered different types of imprinting strategies that can specifically extract the target analyte in complex biological samples while simultaneously avoiding the matrix effect. Some traditional separation technologies based on MIP technology have also been studied in depth; the most common of these technologies include stationary phases used for chromatography and adsorbents for SPE. Analytical methods that combine MIT with highly sensitive detection technologies have received wide interest in fields such as disease diagnosis and bioimaging. In this review, we highlight the new MIP strategies developed in recent years, and describe the applications of MIT-based separation analysis methods in fields including chromatographic separation, SPE, diagnosis, bioimaging, and proteomics. The drawbacks of these techniques as well as their future development prospects are also discussed.


Assuntos
Impressão Molecular , Humanos , Cromatografia de Afinidade/métodos , Extração em Fase Sólida/métodos , Ensaio de Imunoadsorção Enzimática
14.
Food Res Int ; 190: 114604, 2024 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-38945616

RESUMO

Sheep's milk (SM) is known to differ from cow's milk (CM) in nutritional composition and physicochemical properties, which may lead to different digestion behaviours. This work aimed to investigate the impact of the species (cow vs sheep) and the structure (milk vs yogurt) on the digestion of dairy products. Using an in vitro static gastrointestinal digestion model, CM, SM, cow's milk yogurt (CY) and sheep's milk yogurt (SY) were compared on particle size evolution, microscopic observations, degree of lipolysis, degree of proteolysis, specific protein degradation and calcium bioaccessibility. Species and structure affected particle size evolution during the gastric phase resulting in smaller particles for yogurts compared to milks as well as for CM products compared to SM products. Species impacted lipid composition and lipolysis, with SM products presenting higher short/medium-chain fatty acids content and higher intestinal degree of lipolysis. Proteolysis was influenced by structure, with milks showing higher intestinal degree of proteolysis compared to yogurts. Caseins were digested faster in CM, ⍺-lactalbumin was digested faster in SM despite its higher concentration, and during gastric digestion ß-lactoglobulin was more degraded in CM products compared to SM products and more in yogurts compared to milks. Lastly, SM products released more bioaccessible calcium than CM products. In conclusion, species (cow vs sheep) impacted more the digestion compared to the structure (milk vs yogurt). In fact, SM was different from CM mainly due to a denser protein network that might slow down the accessibility of the enzyme to its substrate which induce a delay of gastric disaggregation and thus lead to slower the digestion of the nutrients.


Assuntos
Digestão , Lipólise , Leite , Tamanho da Partícula , Proteólise , Iogurte , Animais , Digestão/fisiologia , Bovinos , Iogurte/análise , Ovinos , Leite/química , Lactoglobulinas/metabolismo , Trato Gastrointestinal/metabolismo , Laticínios/análise , Lactalbumina/metabolismo , Caseínas/metabolismo , Caseínas/análise , Especificidade da Espécie , Proteínas do Leite/análise , Proteínas do Leite/metabolismo
15.
Environ Pollut ; 355: 124180, 2024 Aug 15.
Artigo em Inglês | MEDLINE | ID: mdl-38768676

RESUMO

Solid phase extraction (SPE) has been widely used for pretreatment in target screening (TS) analysis. However, some compounds are difficult to recover by SPE or their recovery is unstable for environmental samples. In this study, we tested large-volume injection (LVI) without SPE for TS analysis of 103 compounds listed by the Ministry of the Environment (Japan)-so-called 'items to be surveyed'-using liquid chromatography high-resolution mass spectrometry. We evaluated the limit of quantification (LOQ) by LVI and compared this LOQ with the LOQ by SPE pretreatment using a hydrophilic-lipophilic balance (HLB) combined with activated carbon, which was found previously to afford the best SPE cartridges for target compounds recovery. The LOQ generally decreased as the injection volume increased, and the LOQ was at least 250 times lower for a 500-µL injection than for a 2-µL injection for half of the compounds. LVI provided LOQs lower than the predicted no effect concentration for more compounds than the SPE method. The average matrix effect (ME) by LVI was in the range 70%-130% for 69 out of 97 compounds. The ME was higher or lower for some of the remaining compounds, but the ME was in the range 10%-1000% for all 18 water samples for 84 of the 97 compounds. Comparing the ME by LVI and the recovery ratio by the SPE method showed that LVI achieved more accurate quantitation than the SPE method for a larger number of compounds. Therefore, LVI provides better sensitivity and quantitativeness than the SPE method using HLB and activated carbon for TS analysis of as many 'items to be surveyed' as possible.


Assuntos
Monitoramento Ambiental , Espectrometria de Massas , Extração em Fase Sólida , Poluentes Químicos da Água , Poluentes Químicos da Água/análise , Extração em Fase Sólida/métodos , Monitoramento Ambiental/métodos , Cromatografia Líquida/métodos , Espectrometria de Massas/métodos , Japão
16.
Materials (Basel) ; 17(10)2024 May 11.
Artigo em Inglês | MEDLINE | ID: mdl-38793348

RESUMO

Harmful substances in consumer goods pose serious hazards to human health and the environment. However, due to the vast variety of consumer goods and the complexity of their substrates, it is difficult to simultaneously detect multiple harmful substances in different materials. This paper presents a method for the simultaneous determination of 41 harmful substances comprising 17 phthalates (PAEs), 8 organophosphate flame retardants (OPFRs), and 16 polycyclic aromatic hydrocarbons (PAHs) in five types of products using the matrix-matching calibration strategy. The method employs an efficient ultrasonic extraction procedure using a mixture of dichloromethane and methylbenzene, followed by dissolution-precipitation and analysis through gas chromatography-mass spectrometry. Compared with previous experiments, we established a universal pretreatment method suitable for multi-matrix materials to simultaneously determine multiple harmful substances. To evaluate the effects of the matrix on the experimental results, we compared neat standard solutions and matrix-matching standard solutions. The results demonstrated that all compounds were successfully separated within 30 min with excellent separation efficiency. Additionally, the linear relationships of all analytes showed strong correlation coefficients (R2) of at least 0.995, ranging from 0.02 mg/L to 20 mg/L. The average recoveries of the target compounds (spiked at three concentration levels) were between 73.6 and 124.1%, with a relative standard deviation (n = 6) varying from 1.2% to 9.9%. Finally, we tested 40 different materials from consumer products and detected 16 harmful substances in 31 samples. Overall, this method is simple and accurate, and it can be used to simultaneously determine multiple types of hazardous substances in multi-matrix materials by minimizing matrix effects, making it an invaluable tool for ensuring product safety and protecting public health.

17.
Water Res ; 257: 121685, 2024 Jun 15.
Artigo em Inglês | MEDLINE | ID: mdl-38728774

RESUMO

Water disinfection is undoubtedly regarded as a critical step in ensuring the water safety for human consumption, and ozone is widely used as a highly effective disinfectant for the control of pathogenic microorganisms in water. Although the diminished ozone efficiencies in complex water matrices have been widely reported, the specific extent to which individual components of matrix act on the virus inactivation by ozone remains unclear, and effective methodologies to predict the comprehensive effects of various factors are needed. In this study, the decoupled impact of the intricate water matrix on the ozone inactivation of viruses was systematically investigated and assessed from a simulative perspective. The concept of "equivalent ozone depletion rate constant" (k') was introduced to quantify the influence of different species, and a kinetic model was developed based on the k' values for simulating the ozone inactivation processes in complex matrix. The mechanisms through which diverse species influenced the ozone inactivation effectiveness were identified: 1) competition effects (k' = 105∼107 M-1s-1), including organic matters and reductive ions (SO32-, NO2-, and I-), which were the most influential species inhibiting the virus inactivation; 2) shielding effects (k' = 103∼104 M-1s-1), including Ca2+, Mg2+, and kaolin; 3) insignificant effects (k' = 0∼1 M-1s-1), including Cl-, SO42-, NO3-, NH4+, and Br-; 4) promotion effects (k' = ∼-103 M-1s-1), including CO32- and HCO3-. Prediction of ozone disinfection efficiency and evaluation of species contribution under complex aquatic matrices were successfully realized utilizing the model. The systematic understanding and methodologies developed in this research provide a reliable framework for predicting ozone inactivation efficiency under complex matrix, and a potential tool for accurate disinfectant dosage determination and interfering factors control in actual wastewater treatment processes.


Assuntos
Desinfecção , Ozônio , Inativação de Vírus , Águas Residuárias , Ozônio/farmacologia , Águas Residuárias/virologia , Inativação de Vírus/efeitos dos fármacos , Desinfecção/métodos , Purificação da Água , Desinfetantes/farmacologia , Modelos Teóricos , Cinética
19.
Diagnostics (Basel) ; 14(8)2024 Apr 11.
Artigo em Inglês | MEDLINE | ID: mdl-38667445

RESUMO

Glucose meters provide a rapid blood glucose status for evidence-based diagnosis, monitoring, and treatment of diabetes mellitus. We aimed to evaluate the commutability of processed blood materials (PBMs) and their use in the performance evaluation of glucose meters. Two PBMs obtained by the fixed-cell method were analyzed for homogeneity, stability, and commutability. The compatibility of ten pairs between mass spectrometry and each glucose meter was categorized as compatible (mean paired difference ≤ 5%) and incompatible (mean paired difference > 5%). The performance of glucose meter 1 (n = 767) and glucose meter 2 (n = 266) was assessed. The glucose in the PBMs remained homogenized and stable for at least 180 days. Six out of ten pairs had commutable PBMs. Commutability of PBMs was observed in both well-compatible and incompatible glucose results. Target glucose values from mass spectrometry were significantly different (p ≤ 0.05) from consensus values in one group of glucose meters. When commutable PBMs were used, glucose meter 1 showed better performance than glucose meter 2, and the percentage of satisfaction was associated when using target values for glucose from mass spectrometry and consensus values, but the performance of glucose meter 2 was not associated. PBM from a fixed-cell method could be mass produced with acceptable homogeneity and stability. Commutability testing of PBMs is required prior to use in the performance evaluation of glucose meters, as the commutability of glucose in the PBMs obtained by a fixed-cell method was variable and depended on the individual glucose meter.

20.
J Food Prot ; 87(6): 100278, 2024 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-38631420

RESUMO

The use of antibiotics in agriculture and livestock poses health risks to consumers. Treatments such as High Hydrostatic Pressure (HHP) have been shown to reduce antibiotic and pesticide residues in food. This study aims to investigate the matrix effect on the effectiveness of HHP on hydrochloride tetracycline (HTC) and sulfathiazole (STZ) residues in spiked food matrices. The effect of viscosity, as well as carbohydrate, protein, and fat content on the effectiveness of HHP on antibiotic residues, was investigated. The studied matrices were full-fat and fat-free bovine milk and model food systems consisting of aqueous solutions of sugars, aqueous solutions of proteins, and oil in water emulsions. Model food systems were also used to study the viscosity effect. These systems consisted of aqueous solutions of honey, aqueous solutions of apple puree, and aqueous solutions of glycerol. The HHP processing (580 MPa, 6 min, 25 °C) took place under industrial conditions. For both antibiotics, the concentration of sugars and proteins was found to affect the effectiveness of treatment. The concentration of oils affected treatment efficacy only for HTC. Reduction of antibiotics by HHP was also affected by the type of carbohydrate and the viscosity. In conclusion, the composition and the viscosity of the food matrix exert a variable effect on the studied antibiotic residues reduction by HHP indicating different underlying mechanisms of the interactions between food constituents and antibiotics under the same process conditions.


Assuntos
Antibacterianos , Pressão Hidrostática , Antibacterianos/farmacologia , Animais , Humanos , Bovinos , Viscosidade , Contaminação de Alimentos/análise , Leite/química , Resíduos de Drogas
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