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Pretreatment steps of current rapid detection methods for mycotoxins in edible oils not only restrict detection efficiency, but also produce organic waste liquid to pollute environment. In this work, a pretreatment-free and eco-friendly rapid detection method for edible oil is established. This proposed method does not require pretreatment operation, and automated quantitative detection could be achieved by directly adding oil samples. According to polarity of target molecules, the content of surfactant in reaction solutions could be adjusted to achieve the quantitative detection of AFB1 in peanut oil and ZEN in corn oil. The recoveries are between 96.5%-110.7% with standard deviation <10.4%, and the limit of detection is 0.17 µg/kg for AFB1 and 4.91 µg/kg for ZEN. This method realizes full automation of the whole chain detection, i.e. sample in-result out, and is suitable for the on-site detection of batches of edible oils samples.
Assuntos
Contaminação de Alimentos , Micotoxinas , Óleos de Plantas , Contaminação de Alimentos/análise , Micotoxinas/análise , Óleos de Plantas/química , Limite de Detecção , Óleo de Milho/químicaRESUMO
Numerous studies have demonstrated the role of making choices as an internal motivator to improve performance, and recent studies in the domain of memory have focused on adults. To chart the developmental trend of the choice effect on memory, we conducted a series of seven experiments involving children, adolescents, and young adults. Participants (N = 512) aged 5 to 26 years performed a choice encoding task that manipulated the opportunities to choose and then took a memory test. Using different types of experimental materials and corroborated by a mini meta-analysis, we found that the choice effect on memory was significant in childhood and early adolescence but not significant in late adolescence and early adulthood. The developmental changes were statistically significant, particularly evident during the transition from early to late adolescence. These findings suggest that the internal value of choice decreases across development and contributes to our understanding of developmental differences in the role of choice in memory.
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Desenvolvimento Infantil , Comportamento de Escolha , Humanos , Adolescente , Comportamento de Escolha/fisiologia , Feminino , Masculino , Criança , Adulto Jovem , Adulto , Pré-Escolar , Desenvolvimento Infantil/fisiologia , Memória , Fatores EtáriosRESUMO
This study presents a novel approach toward the one-pot green synthesis of ZIF-8/IgG composite, focusing on its precise orientation and protection of the anti-aflatoxins antibody. The antibody orientation is achieved through the specific binding of IgG to the Fc region of the antibody, while the antibody protection is accomplished by the structural change restriction of ZIF-8 framework to the antibody. Consequently, the antibody exhibits enhanced target capability and significantly improved tolerance to organic solvents. The ZIF-8/IgG/anti-AFT was employed for the purification and detection of AFTs by coupling with UPLC. Under optimized conditions, the recoveries of spiked AFTs in peanut oils are between 86.1% and 106.4%, with relative standard deviations (RSDs) ranging from 0.8% to 8.8%. The linearity range is 0.5-20.0 ng for AFB1 and AFG1, 0.125-5.0 ng for AFB2 and AFG2, the limit of detection is 0.1 ng for AFB1 and AFG1, 0.03 ng for AFB2 and AFG2.
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Aflatoxinas , Contaminação de Alimentos , Química Verde , Imunoglobulina G , Óleo de Amendoim , Aflatoxinas/análise , Aflatoxinas/imunologia , Aflatoxinas/isolamento & purificação , Contaminação de Alimentos/análise , Óleo de Amendoim/química , Imunoglobulina G/imunologia , Imunoglobulina G/química , Anticorpos/imunologia , Anticorpos/química , Cromatografia Líquida de Alta PressãoRESUMO
A one-pot synthesis afforded a magnetic, crosslinked polymer adsorbent (m-P6) with a variety of functional groups to realize simultaneous adsorption of Cd2+, Pb2+, Hg2+, and As3+. The material was characterized by TEM-EDS, XRD, FT-IR, VSM, and XPS. Kinetic and isothermal analyses suggested mainly chemisorption processes of heavy metal ions that form multiple layers on heterogeneous surfaces. Theoretical adsorption capacities calculated by a pseudo-2nd-order kinetic model and the Sips isothermal model were 282.88 mg/g for Cd2+, 326.18 mg/g for Pb2+, 117.85 mg/g for Hg2+, and 320.29 mg/g for As3+. m-P6 not only can efficiently adsorb divalent heavy metals (Cd2+, Pb2+, Hg2+), but also demonstrate a process of adsorption-driven catalytic oxidation by single-electron transfer (SET) from As3+ to As5+. In application, in addition to adsorption in water, m-P6 is capable of minimizing matrix interference, and extracting trace heavy metals in a complex environment (cereal) through easy operations for improving the detection accuracy, as well as it is potential for application in detection of trace heavy metals in foodstuffs. m-P6 can be readily regenerated and efficiently recycled for 5 cycles using eluent E12 and dilute acid.
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Sterigmatocystin (ST) is a known toxin whose aptamer has rarely been reported because ST is a water-insoluble small-molecule target with few active sites, leading to difficulty in obtaining its aptamer using traditional target fixation screening methods. To obtain aptamer for ST, we incorporated FAM tag size separation into the capture-systematic evolution of ligands by exponential enrichment and combined it with molecular activation for aptamer screening. The screening process was monitored using a quantitative polymerase chain reaction fluorescence amplification curve and recovery of negative-, counter-, and positive-selected ssDNA. The affinity and specificity of the aptamer were verified by constructing an aptamer-affinity column, and the binding sites were predicted using molecular docking simulations. The results showed that the Kd value of the H Seq02 aptamer was 25.3 nM. The aptamer-affinity column based on 2.3 nmol of H Seq02 exhibited a capacity of about 80 ng, demonstrating better specificity than commercially available antibody affinity columns. Molecular simulation docking predicted the binding sites for H Seq02 and ST, further explaining the improved specificity. In addition, circular dichroism and isothermal titration calorimetry were used to verify the interaction between the aptamer and target ST. This study lays the foundation for the development of a new ST detection method.
Assuntos
Aptâmeros de Nucleotídeos , Aptâmeros de Nucleotídeos/química , Esterigmatocistina , Técnica de Seleção de Aptâmeros/métodos , Simulação de Acoplamento Molecular , LigantesRESUMO
In this study, a dual-member bacterial consortium with the ability to oxidize deoxynivalenol (DON) to 3-keto-DON, designated SD, was first screened from the feces of Tenebrio molitor larvae. This consortium consisted of Pseudomonas sp. SD17-1 and Devosia sp. SD17-2, as determined by 16S rRNA-based phylogenetic analysis. A temperature of 30 °C, a pH of 8.0-9.0, and an initial inoculum concentration ratio of Devosia to Pseudomonas of 0.1 were optimal single-factor parameters for the DON oxidation activity of the bacterial consortium SD. Genome-based bioinformatics analysis revealed the presence of an intact PQQ biosynthesis operon (pqqFABCDEG) and four putative pyrroloquinoline quinone (PQQ)-dependent alcohol dehydrogenase (ADH) genes in the genomes of Pseudomonas strain SD17-1 and Devosia strain SD17-2, respectively. Biochemical analyses further confirmed the PQQ-producing phenotype of Pseudomonas and the DON-oxidizing enzymatic activities of two of four PQQ-dependent ADHs in Devosia. The addition of PQQ-containing a cell-free fermentation supernatant from Pseudomonas activated DON-oxidizing activity of Devosia. In summary, as members of the bacterial consortium SD, Pseudomonas and Devosia play indispensable and complementary roles in SD's oxidation of DON. Specifically, Pseudomonas is responsible for producing the necessary PQQ cofactor, whereas Devosia expresses the PQQ-dependent DON dehydrogenase, together facilitating the oxidation of DON.
Assuntos
Tenebrio , Animais , Filogenia , RNA Ribossômico 16S , Biotransformação , Fezes , Larva , Cofator PQQ , Pseudomonas/genéticaRESUMO
Deoxynivalenol (DON) is frequently detected in cereals and cereal-based products and has a negative impact on human and animal health. In this study, an unprecedented DON-degrading bacterial isolate D3_3 was isolated from a sample of Tenebrio molitor larva feces. A 16S rRNA-based phylogenetic analysis and genome-based average nucleotide identity comparison clearly revealed that strain D3_3 belonged to the species Ketogulonicigenium vulgare. This isolate D3_3 could efficiently degrade 50 mg/L of DON under a broad range of conditions, such as pHs of 7.0-9.0 and temperatures of 18-30 °C, as well as during aerobic or anaerobic cultivation. 3-keto-DON was identified as the sole and finished DON metabolite using mass spectrometry. In vitro toxicity tests revealed that 3-keto-DON had lower cytotoxicity to human gastric epithelial cells and higher phytotoxicity to Lemna minor than its parent mycotoxin DON. Additionally, four genes encoding pyrroloquinoline quinone (PQQ)-dependent alcohol dehydrogenases in the genome of isolate D3_3 were identified as being responsible for the DON oxidation reaction. Overall, as a highly potent DON-degrading microbe, a member of the genus Ketogulonicigenium is reported for the first time in this study. The discovery of this DON-degrading isolate D3_3 and its four dehydrogenases will allow microbial strains and enzyme resources to become available for the future development of DON-detoxifying agents for food and animal feed.
Assuntos
Rhodobacteraceae , Tenebrio , Animais , Humanos , Larva , Cofator PQQ , Filogenia , RNA Ribossômico 16S/genética , Oxirredutases , Estresse OxidativoRESUMO
Aflatoxin (AFT) is an extremely toxic and highly toxic carcinogenic substance. This is particularly problematic due to the risk of aflatoxin contamination in raw feed materials and products during production, transportation, and storage. In this study, immunoaffinity magnetic beads (IMBs) were prepared for the purification of four aflatoxins (aflatoxin B1 (AFB1), aflatoxin B2 (AFB2), aflatoxin G1 (AFG1) and aflatoxin G2 (AFG2)). The aflatoxin contents were then determined rapidly and accurately using ultra performance liquid chromatography (UPLC). More specifically, the coupling ratio of magnetic beads (MBs) to the aflatoxin monoclonal antibody was initially optimized, wherein an MB volume of 1 mL and an antibody content of 2.0 mg was found to meet the purification requirements of this method. The magnetic properties of the MBs and the IMBs were then investigated using a vibrating sample magnetometer (VSM) at room temperature. As a result, the maximum saturation super magnetizations of the MBs and the IMBs were determined to be 28.61 and 23.22 emu/g, respectively, indicating that the saturation magnetization intensity of the IMBs was reduced by coupling with a non-magnetic antibody. However, the saturation magnetization intensity remained sufficiently high to permit magnetic separation from the solution. In addition, the appearance of the IMBs was examined using a biomicroscope, and it was clear that the magnetic cores were wrapped in agarose gel. Furthermore, the reaction time between the IMBs and the aflatoxins was investigated, and the optimal reaction time for meeting the purification requirements was determined to be 2 min. The stability of the IMBs was then evaluated under refrigerated storage conditions at 4 â. It was found that the prepared IMBs maintained a high aflatoxin enrichment capacity for at least eight months. Through the examination of three different extraction solutions, a mixture of acetonitrile and water (70â¶30, v/v) was found to be optimal for the extraction of aflatoxins from the feed samples. Moreover, five sample dilutions and purification effects were also examined, and phosphate-buffered saline (containing 0.5% Tween-20) was selected as the preferred sample dilutant. With the optimized conditions, the effectiveness of using IMB for the purification of different feed samples was investigated. The resulting UPLC chromatogram showed no spurious peaks close to the target peaks, demonstrating a good purification performance. Following matrix spiking (5, 20, and 40 µg/kg, calculated based on AFB1) of the four feed samples (i. e., soybean meal, distillers dried grains with solubles, pig feed, and chicken feed), the spiked recoveries of the four aflatoxins ranged from 91.1% to 119.4% with a relative standard deviation (RSD) of <6.9%. In addition, the inter-day precision was 4.5% to 7.5%, and the method exhibited a good reproducibility. Subsequently, the developed method was used to detect AFB1 using reference materials. The test value was 18.6 µg/kg with an accuracy of 110.3%, thereby constituting satisfactory results. Upon testing 21 randomly purchased feed samples using this method, four of these samples contained AFB1, and the test results obtained using the developed method and stable isotope dilution LC-MS/MS were comparable. It was therefore apparent that the IMB purification method combined with UPLC analysis exhibited a good accuracy for aflatoxin determination. Thus, an automatic purification system was established to facilitate the operation and use of IMBs. This system was able to purify 24 samples simultaneously in 30 min. An IMB purification kit for was also designed and produced for aflatoxin detection in feed samples. The kit contained the sample dilutant, IMBs, the washing solution, and the eluent. After extraction of the feed sample, the extraction solution was added to the sample wells provided in the kit, and the purification system automatically completed the steps of aflatoxin enrichment, impurity washing, and elution of the target toxin. It should be noted that the purification process does not require the operator to manually add the solution, thereby simplifying operation. Overall, the purification method established in this study achieved the high-throughput and automatic purification of the four aflatoxins in feed samples.
Assuntos
Aflatoxinas , Animais , Suínos , Aflatoxinas/análise , Cromatografia Líquida , Reprodutibilidade dos Testes , Cromatografia Líquida de Alta Pressão , Espectrometria de Massas em Tandem/métodosRESUMO
Sample pretreatment is a vital step in the detection of mycotoxins, and traditional pretreatment methods are time-consuming, labor-intensive and generate much organic waste liquid. In this work, an automatic, high-throughput and environmentally friendly pretreatment method is proposed. Immunomagnetic beads technology and dispersive liquid-liquid microextraction technology are combined, and the zearalenone in corn oils is directly purified and concentrated under the solubilization effects of surfactant. The proposed pretreatment method allows for the batch pretreatment of samples without pre-extraction using organic reagents, and almost no organic waste liquid is produced. Coupled with UPLC-FLD, an effective and accurate quantitative detection method for zearalenone is established. The recovery of spiked zearalenone in corn oils at different concentrations ranges from 85.7 to 89.0%, and the relative standard deviation is below 2.9%. The proposed pretreatment method overcomes the shortcomings of traditional pretreatment methods and has broad application prospects.
Assuntos
Microextração em Fase Líquida , Micotoxinas , Zearalenona , Zearalenona/análise , Microextração em Fase Líquida/métodos , Óleo de Milho , Zea mays , Micotoxinas/análise , Cromatografia Líquida de Alta Pressão/métodosRESUMO
In this study, based on the high-throughput automatic sample pretreatment with immunoaffinity magnetic beads with oriented immobilized antibodies, grain and feed fumonisin (FB) content was detected using pre-column automatic derivatization of high-performance liquid chromatography (HPLC). The FB capacity of well-oriented antibody immunoaffinity magnetic beads was 1.5-1.8 times that of magnetic beads with randomly fixed antibody. This pre-column automatic derivatization method using an autosampler can reduce error from manual injection and improve detection efficiency. The spiked recoveries for three different concentrations in maize, husked rice, and pig feed under optimized conditions were 84.6-104.0% (RSD < 9.3%). Our novel method was also applied to the analysis of FBs in 63 maize samples collected from the main maize-production regions in China. The results showed that as latitude increased, the contamination level of FBs tended to decrease. High temperature and high humidity are also more favorable for FB growth.
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Fumonisinas , Animais , Suínos , Fumonisinas/análise , Cromatografia Líquida de Alta Pressão/métodos , Contaminação de Alimentos/análise , Zea mays/química , Fenômenos MagnéticosRESUMO
In the present work, palygorskite (PAL) supported Co-Fe oxides (CoFe@PAL) were prepared and used as a peroxymonosulfate (PMS) activator for removal of rhodamine B (RhB) in water. The results showed that CoFe@PAL prepared at impregnation solution of 50 g L-1 and calcination temperature of 500 °C showed the best catalytic performance. The removal efficiency of RhB (10 mg L-1) by PMS (0.1 mmol L-1) activated with CoFe@PAL (1 g L-1) was above 98% within 60 min. The effects of various environmental factors including initial pH, humic acid (HA) and inorganic anions on the removal effect were simultaneously investigated. The radical quenching experiments and EPR characterization revealed that ËOH, SO4Ë-, O2Ë- and 1O2 radicals existed in the CoFe@PAL/PMS system simultaneously. The intermediates during RhB degradation were analyzed by LC-MS and possible degradation pathways of RhB were proposed. Moreover, CoFe@PAL exhibited superior stability and reusability.
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How to quickly separate and detect cadmium (Cd2+) and lead (Pb2+) from solid samples is a difficult problem that needs to be solved. For this, Fe3O4@agarose@iminodiacetic acid (IDA) was synthesized and used for rapid purification of Cd2+ and Pb2+. This material can remove complex matrix interference completely within a short time of 15 min. The mechanism of the adsorption kinetics fit well to a pseudo-second-order model. A portable screen-printed electrodes (SPEs)-based electrochemical detection platform was established. After coupling with the pretreatment, the whole detection process only took within 30 min. The limits of detection (LOD) were ten times lower than those of the Codex general standard, with values of 0.02 and 0.01 mg/kg for Pb2+ and Cd2+, respectively. The recoveries ranged from 84.1% to 109.7% in naturally contaminated grain, in good agreement with the ICP-MS, demonstrating great prospects for the rapid screening and monitoring of Cd2+ and Pb2+ in grain.
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The mycotoxin ochratoxin A (OTA) is toxic to humans and frequently contaminates wine and beer. Antibodies are essential recognition probes for the detection of OTA. However, they have several drawbacks, such as high costs and difficulty in preparation. In this study, a novel magnetic-bead-based automated strategy for efficient and low-cost OTA sample preparation was developed. Human serum albumin, which is an economical and stable receptor based on the mycotoxin-albumin interaction, was adapted and validated to replace conventional antibodies to capture OTA in the sample. Ultra-performance liquid chromatography-fluorescence detection was used in combination with this preparation method for efficient detection. The effects of different conditions on this method were investigated. The recovery of OTA samples spiked at three different concentrations ranged from 91.2% to 102.1%, and the relative standard deviations (RSDs) were 1.2%-8.2% in wine and beer. For red wine and beer samples, the LODs were 0.37 and 0.15 µg/L, respectively. This reliable method overcomes the drawbacks of conventional methods and offers significant application prospects.
Assuntos
Micotoxinas , Ocratoxinas , Vinho , Humanos , Micotoxinas/análise , Ocratoxinas/análise , Vinho/análise , Albuminas , Fenômenos Magnéticos , Cromatografia Líquida de Alta Pressão/métodos , Contaminação de Alimentos/análiseRESUMO
ß-N-methylamino-L-alanine (BMAA), which has been considered as an environmental factor that caused amyotrophic lateral sclerosis/parkinsonism-dementia complex (ALS/PDC) or Alzheimer's disease, could be produced by a variety of genera cyanobacteria. BMAA is widely present in water sources contaminated by cyanobacteria and may threaten human health through drinking water. Although oxidants commonly used in drinking water plants such as chlorine, ozone, hydrogen peroxide, and hydroxyl radicals have been shown to effectively degrade BMAA, there are limited studies on the mechanism of BMAA degradation by different oxidants, especially ozone. This work systematically explored the effectiveness of BMAA ozonation degradation, investigated the effect of the operating parameters on the effectiveness of degradation, and speculated on the pathways of BMAA decomposition. The results showed that BMAA could be quickly eliminated by ozone, and the removal rates of BMAA were nearly 100% in pure water, but the removal rates were reduced in actual water. BMAA was primarily degraded by direct oxidation of ozone molecules in acidic and near-neutral conditions, and indirect oxidation of â¢OH accounted for the main part under strong alkaline conditions. The pH value had a significant effect on the decomposition of BMAA, and the degradation rate of BMAA was fastest at near-neutral pH value. The degradation rates of TOC were significantly lower than that of BMAA, indicating that by-products were generated during the degradation process. Three by-products ([M-H]+ = 105, 90, and 88) were identified by UPLC-MS/MS, and the degradation pathways of BMAA were proposed. The production of by-products was attributed to the fracture of the C-N bonds. This work is helpful for the in-depth understanding on the mechanism and demonstration of the feasibility of the oxidation of BMAA by the ozone process. HIGHLIGHTS: ⢠The reaction of ozonation BMAA was easy to occur. ⢠The degradation rate was fast under near-neutral conditions. ⢠Direct oxidation under neural conditions was the main pathway for ozone degradation of BMAA. ⢠Three products were detected, and the reaction path was inferred.
Assuntos
Diamino Aminoácidos , Água Potável , Ozônio , Humanos , Neurotoxinas , Cromatografia Líquida , Espectrometria de Massas em Tandem , Toxinas de Cianobactérias , Diamino Aminoácidos/química , OxidantesRESUMO
Fusarium graminearum species complex (FGSC) is one of the most devastating fungal plant pathogens of cereal crops worldwide, resulting in a corresponding mycotoxins contamination in cereal-based food. The detection of FGSC to study its population structure and species distribution is of great concern for the integrated control of mycotoxins contamination in grains entering food supply chains. In this study, real time quantitative PCR (RT-qPCR) and droplet digital PCR (ddPCR) methods were developed for the species-specific detection of Fusarium graminearum species complex in winter wheat growing regions in China. Primers and probes were designed basing the on the sequence of Fg-16 SCAR fragment (sequence characterized amplified regions analysis) and confirmed to make a distinguishment between the two prevailing species including Fusarium graminearum sensu stricto and Fusarium asiaticum. The assay specificity was tested against 24 isolates of target Fusarium species and several non-target Fusarium species that were frequently isolated from wheat in China. Consistent results could be obtained by the developed RT-qPCR and ddPCR assays, and both of them were sensitive enough for the detection of FGSC in these regions. Population structure and species distribution of FGSC in North China plain and Yangtze River plain by the developed qPCR assays accorded with previous results obtained by fungal isolation method. The newly developed qPCR assays are time-saving and will provide new insights during the routine surveillance of FGSC in winter wheat growing regions in China and possibly other countries.
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Fusarium , Micotoxinas , Triticum/microbiologia , Reação em Cadeia da Polimerase em Tempo Real , ChinaRESUMO
Deoxynivalenol (DON) in wheat is one of the major food safety concerns worldwide. In this study, 70 characteristic precursive factors associated with environment and 6 agronomic practicing factors were explored, using historical data of 479 wheat fields in the Huang-Huai-hai, China. Results showed that DON concentrations influenced by air temperature, relative humidity, precipitation, and sunshine duration in the period from 17 days before flowering to 10 days before harvest. Rice crop rotation, straw returning, larger density of sowing, and lower latitude planting increased DON risk. Furthermore, an empirical model of DON prediction was established. The classification accuracy of internal and external validation were 87.73% (R2 = 0.62) and 80.21% (R2 = 0.60), respectively. This model is the first large-scale prediction of mycotoxin contamination in grain at harvest in China. It can be used to predict the risk of DON contamination for nearly 14 % of the global wheat supply.
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Fusarium , Micotoxinas , Triticum , Contaminação de Alimentos/análise , Micotoxinas/análise , ChinaRESUMO
Matrix certified reference materials (CRMs) play a critical role in analytical method validation and the assurance of reliable measurement results. A certified reference material (GBW(E)100813) for whole-wheat flour was developed to ensure an accurate and reliable measurement of the main Fusarium mycotoxins (deoxynivalenol (DON), nivalenol (NIV), deoxynivalenol-3-glucoside (DON-3G), and zearalenone (ZEN)). CRM candidates were prepared using sun-drying, grinding, sieving, homogenising, packaging, and gamma irradiation. The final produced CRM was packaged at 50 g per unit and stored at 20 °C. Certification was performed using isotope dilution-liquid chromatography-tandem mass spectrometry. CRM characterization was performed in eight laboratories in accordance with the requirements of ISO Guide 35. The certified values and expanded uncertainties (at a confidence of 95%, k = 2) for DON, NIV, DON-3G, and ZEN were determined to be 0.98 ± 0.12 mg/kg, 1.37 ± 0.20 mg/kg, 242 ± 35 µg/g, and 382 ± 50 µg/g. The CRM was sufficiently homogeneous between and within bottles, and remained stable for up to 12 months at 20 °C and 9 days below 40 °C for transportation. Thus, CRM can be used for quality control and method validation to ensure the accurate and reliable quantification of the main Fusarium mycotoxins in whole-wheat flour.
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A rapid, accurate, and ecofriendly pretreatment plays an extremely important role prior to ICP-MS for heavy metal analysis. In order to improve the pretreatment efficiency, a high-throughput and automatic magnetic solid-phase extraction of five heavy metals (Cd, Pb, Mn, Cu, and Zn) was carried out by a magnet-controlled pretreatment system with an ecofriendly diluted acid as an extracting agent and carboxyl-functionalized magnetic beads as a pretreatment material. Key conditions, including the pH, adsorption time, and eluent solution, were optimized. The time for purification and enrichment was only 8 min. The adsorption capacities of the carboxyl-functionalized magnetic beads were in the range of 152~426 mg g-1. The preconcentration factor of Cu was 40, and others were 200. In the optimal conditions, the limits of detection for Mn, Zn, Cd, Cu, and Pb by ICP-MS were 3.84, 2.71, 0.16, 11.54, and 6.01 ng L-1, respectively. The percentage recoveries were in the range of 80~110%, and the relative standard deviations were less than 3%. The developed method was in good agreement with traditional standard microwave digestion. Additionally, the designed system could simultaneously process up to 24 samples within 22 min, reducing the time to less than 1 min/sample. Thus, the proposed auto-MSPE-ICP-MS method was successfully applied to analyze five heavy metals in cereals and feeds with a simple operation and high precision, safety, and reliability.
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A simple, rapid, sensitive, accurate, and automatic graphite furnace atomic absorption spectrometry (GFAAS) method for detecting Cd and Pb in cereals is presented. This method enables the simultaneous determination of Cd and Pb in cereals with a pre-treatment method of diluted acid extraction and a high-performance lead-cadmium composite hollow-cathode lamp (LCC-HCL), and it realizes automatic determination from sample weighing to result output through an automatic diluted acid extraction system. Under the optimization, Pb and Cd in cereals were simultaneously and automatically detected in up to 240 measurements in 8 h. The LOD and LOQ of this method were 0.012 and 0.040 mg·kg-1 for Pb, and 0.0014 and 0.0047 mg·kg-1 for Cd, respectively. The results of the four certified reference materials were satisfied; there was no significant difference compared with the ICP-MS method according to a t-test, and the RSDs were less than 5% for Cd and Pb. The recoveries of naturally contaminated samples compared with the ICP-MS method were favorable, with 80-110% in eight laboratories. The developed method is rapid, low-cost, and highly automated and may be a good choice for grain quality discrimination and rapid analysis of Cd and Pb in different institutions.