Limit Of Quantitation Research Articles

Development of Magnetic Porous Polymer Composite for Magnetic Solid Phase Extraction of Three Fluoroquinolones in Milk.

In this study, a magnetic porous polymer composite with both hydrophilic and hydrophobic groups was synthesized for magnetic solid phase extraction (MSPE) of milk substrates. Optimization was conducted on various parameters, including adsorption dose, solution pH, adsorption time, and some elution conditions. Coupled with a high-performance liquid chromatography fluorescence detector, a novel MSPE method for determination of norfloxacin (NFX), ciprofloxacin (CIP), and enrofloxacin (ENR) in milk was developed based on magnetic metal organic framework polystyrene polymer (Fe3O4@MOF@PLS) as adsorbent. The Fe3O4@MOF@PLS exhibited significantly improved adsorption performance compared to MOF and PLS. Under optimized experimental conditions, the method exhibited good linearity for the three fluoroquinolones (FQs) in the range of 0.5-1000 μg/kg, with limit of detections (LODs) ranging from 0.21 to 1.33 μg/kg, and limit of quantitations (LOQs) from 0.71 to 4.42 μg/kg. The relative standard deviation (RSD) for the three FQs were 3.4-8.8%. The recoveries of three FQs in milk samples ranged from 84.2% to 106.2%. This method was successfully applied to the detection of three FQs in 20 types of milk, demonstrating its simplicity, speed, and effectiveness in analyte enrichment and separation. The method presented advantages in adsorbent dosage, adsorption time, LODs, and LOQs, making it valuable for the analysis and detection of FQs in milk.

A real-time on-site precision nutrient monitoring system for hydroponic cultivation utilizing LIBS

Indoor hydroponic farming is an advanced cultivation technique with diverse sustainability benefits, such as facilitating local produce, minimizing transportation costs and emissions, and enabling year-round crop cultivation. To optimize crop growth for enhanced yield, improved crop quality, and reduced environmental footprint, precise monitoring and replenishment of essential nutrients within hydroponic systems is crucial. Current methods employed in most commercial farms for online nutrient supply monitoring is limited to pH and conductivity measurements. These techniques can only offer an indication of the overall change in the complex nutrient mixture and lack the capability to precisely identify the specific nutrient or quantify the nutrient content. Most of the existing techniques for measuring individual nutrient levels are expensive and invasive, necessitating sample preparation, frequent recalibration, and skilled personnel for operation. In this context, we propose and demonstrate a real-time, on-site monitoring system for the precise analysis of hydroponic nutrient supply based on laser-induced breakdown spectroscopy (LIBS). We also discuss the system design considerations, parametric optimizations, limit of detection (LOD), and limit of quantitation (LOQ) of key nutrient components such as potassium (K), sodium (Na), calcium (Ca), and magnesium (Mg), using the proposed approach. The detection range of the developed LIBS-based monitoring system can encompass the typical concentration range observed in hydroponic nutrient solutions used at agricultural farms. This technique offers rapid online monitoring of individual nutrient components, providing precise, real-time analysis and the potential to enable comprehensive automation capabilities for current and future hydroponic farms.Graphical abstract

Non-invasive detection of hazardous materials with a thermal-to-epithermal neutron station: a feasibility study towards practical application

The growing scale of the devastation that even a single terrorist attack can cause requires more effective methods for the detection of hazardous materials. In particular, there are no solutions for effectively monitoring threats at sea, both for the off-shore infrastructure and ports. Currently, state-of-the-art detection methods determine the density distribution and the shapes of tested subjects but only allow for a limited degree of substance identification. This work aims to present a feasibility study of the possible usage of several methods available on the thermal-to-epithermal neutron station, VESUVIO, at the ISIS neutron and muon spallation source, UK, for the detection of hazardous materials. To this end, we present the results of a series of experiments performed concurrently employing neutron transmission and Compton scattering using melamine, a commonly used explosive surrogate, in order to determine its signal characteristics and limits of detection and quantitation. The experiments are supported by first-principles modelling, providing detailed scrutiny of the material structure and the nuclear dynamics behind the neutron scattering observables.

Electrochemical detection of indigo carmine in candies using Y2O3 nanoparticles infused graphite electrode

This article presents the use of Yttrium Oxide (Y2O3) nanoparticles to modify the graphite paste electrode (GPE) for the sensitive and selective electrochemical determination of Indigo Carmine (ICN), one of the well-known synthetic food colorants. These nanoparticles were formed via a simple sol and gel method and characterized by a few non-destructive analytical methods like X-ray Photoelectron Spectroscopy (XPS), Scanning Electron Microscopy (SEM), and Energy Dispersive Spectroscopy (EDX) techniques. The electrode response was studied via Cyclic Voltammetry (CV) and Differential Pulse Voltammetry (DPV) methods for the variation of some fundamental parameters such as buffer, pH, scan rates, and concentrations. The efficiency of the developed Yttrium Oxide (Y2O3) nanoparticles modified Graphite Paste Electrode (Y2O3@GPE) sensor was assessed via repeatability, reproducibility and long-term stability analysis. Various similar interferants were added with ICN molecules for accomplishing the selectivity study while a widely linear operating range with a Limit of Detection (LOD) and a Limit of Quantitation (LOQ) of 0.11 µM and 0.35 µM, respectively were found. The performance of the electrode was justified in the real samples through its application for the detection of ICN in different candies where a satisfactory recovery rate of 96.25 %-117.5 % was achieved.

Electrochemical Detection of Bisphenol a By Modified Gold Electrode with Ternary Quantum Dot Metal Organic Framework Composites

Modified gold electrode with Metal-organic framework (MOFs), ternary quantum dots (TQDs) and their composite (TQDs@MOFs) were as electrochemical sensor to determine bisphenol A (BPA). A comparative electrochemical study of the MOFs, QDs and QDs@MOFs reveals that the composite (QDs@MOFs) have the highest conductivity, largest effective surface area, lowest peak potential separation (∆Ep) and the highest oxidation peak current. Under optimal conditions and wide range of BPA concentrations, the ternary quantum dots metal organic frameworks were a better sensor for bisphenol A with 0.488 nM limit of detection and 1.473 nM. limit of quantitation in comparison to metal organic framework and quantum dots. The results show that QDs@MOFs responded remarkable to BPA and could be adapted a practical and efficient efficient sensor for the determination of BPA

Modern chromatographic method for estimating Loratadine and affections on healthcare

PurposeThe purpose of this study is to establish Loratadine [LRD] quantification in purified and capsule formulations using a precise and specific Reversal Phase with a very high-performance liquid Chromatographic [RP-HPLC] technique. The approach was evaluated in agreement with the principles of the International Conference on Harmonization [ICH]. Arcus EP-C18 Ion Pac column, 5 m, 4.6 mm, 250 mm, mobile phase Methanol: Acetonitrile (60:40) v/v. Dibasic potassium phosphate buffer, pH 7.2, flow rate 1.0 ml/min.Design/methodology/approachThe HPLC system used a 340 nm UV detector for testing. A 10-min run time was used for the analysis. At concentrations ranging from 2 to 10 g/ml, the technique was linear (R2 = 0.9998), exact (intra-day and inter-day relative standard deviation [RSD] values 1.0%), accurate (range recovery = 96%–102%), exclusive and strong.FindingsThe detecting and quantitation limits were 0.92 g/ml and 2.15 g/ml, respectively.Originality/valueThe findings demonstrated that the proposed method could accurately determine LRD in bulk and pill dose formats quickly and accurately.

Development and Application of a Liquid Chromatography-Tandem Mass Spectrometry Method for the Analysis of 20 Perfluoroalkyl Substances in Fruit and Vegetables at Sub-Parts-per-Trillion Levels.

In response to the European Food Safety Authority's establishment of a tolerable weekly intake (TWI) for the sum of PFOA, PFNA, PFHxS, and PFOS, a method was developed to quantify and confirm 20 PFASs at the sub-parts-per-trillion level in fruit and vegetables. Improved sensitivity was achieved by (i) increasing the sample intake, (ii) decreasing the solvent volume in the final extract, and (iii) using a highly sensitive mass spectrometer. Except for PFTrDA, target PFASs could be quantitatively determined with an apparent recovery of 90-119%, limits of quantitation down to 0.5 ng/kg, and a relative standard deviation under within-laboratory reproducibility conditions of <28%. The method was successfully applied to 215 fruit and vegetable samples obtained from local grocery stores and markets. Leafy vegetables prove to be the main vegetable category responsible to PFAS exposure, mainly of PFOA, followed by PFHpA and PFHxA.

Simultaneous determination of sixteen phthalic acid esters (PAEs) in soil and evaluation of matrix effect using a QuEChERS/GC/MS-internal standard method.

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 0.91-66.97µg/kg and 2.7-200.9µg/kg, respectively. The accurate test at 0.5, 0.1, and 1.0mg/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.

Boronic acid-functionalized magnetic covalent organic frameworks based solid-phase extraction coupled with hydrophilic interaction chromatography-tandem mass spectrometry for the determination of trace gentamicin residues in milk

Boric acid-functionalized magnetic covalent organic frameworks (Fe3O4-TpBD-B) with large surface area and high porosity were prepared and applied for magnetic solid-phase extraction adsorbent of gentamicin from milk before UPLC-MS/MS detection. By utilizing a new HILIC chromatographic column with zwitterionic sulfoalkyl betaine stationary phase based on ethyl bridged hybrid particles (BEH), isomers of gentamicin (C1, C1a, and C2+C2a components). The developed methods demonstrated good linearity (R2 > 0.99), acceptable accuracy and good precision (<10 %), and low limit of quantitation (1.59 ng mL⁻1 for C1, 1.52 ng mL⁻1 for C1a and 2.72 ng mL⁻1 for C2+C2a). In addition, this method has been effectively applied to the analysis of real milk samples.

Dissipation behaviour and dietary risk evaluation of pesticides on cucumber.

Cucumber (Cucumis sativus L.) is the world's most widely consumed salad vegetable, and it is frequently treated with pesticides to prevent pest and disease outbreaks. Pesticide residues in food commodities impede trade and pose a major health risk. Prior to residue estimation, the QuEChERS approach was validated utilising criteria such as limit of detection, limit of quantitation, linearity, accuracy, and precision. The residues of carbendazim, cypermethrin, ethion, profenofos, quinalphos, and triazophos were examined using a Gas Chromatograph equipped with an Electron Capture Detector or a Flame Photometric Detector and a high-performance liquid chromatography coupled to a photo diode array. The initial deposits of carbendazim, cypermethrin, ethion, profenofos, quinalphos, and triazophos at the prescribed dose were 1.235, 0.407, 0.817, 0.960, 0.628, and 0.985mg/kg, respectively, with a pre-harvest interval of 5.58-11.30days. According to the consumer risk evaluation data, the Hazard Quotient is less than one, and the Theoretical Maximum Dietary Intake is less than the Maximum Permissible Intake and Maximum Residue Limit, both of which are considered safe for human consumption at the authorised dose.

GREEN HPLC DETERMINATION OF PHENYTOIN AND METHOD VALIDATION

Objective: In this study, the chromatographic behavior of the antiepileptic drug phenytoin was determined by the green HPLC method. The optimization of the developed method was based on the capacity factor values of phenytoin in varying water-ethanol binary mixtures and the ethanol concentration in the mobile phase where the compound was analyzed. Material and Method: Ethanol-water binary mixtures containing 35%, 40%, and 45% (v/v) ethanol were used in the optimization for the determination performed by the RPLC method. Retention times of the compound were determined with the Zorbax SB-CN (150x4.6 mm, 3.5 µm ID) column. Analyzes were performed at a constant flow rate (0.3 ml/min) and column temperature (37°C). The optimum condition for quantitative analysis was determined as an ethanol-water binary mixture containing 40% (v/v) ethanol with a pH of 6.5. Result and Discussion: In this study, the hydrophobicity of phenytoin was calculated using the logk-φ relationship. The optimum condition was determined using the obtained chromatographic data, and the quantitative determination of phenytoin in the commercial tablet formulation was made by the internal standard method. Under these conditions, excellent linearity (r&amp;gt;0.99) was obtained in the concentration range of 0.8-2.8 μg/ml. The detection limit of the developed method is 0.021 μg/ml; the limit of quantitation was calculated as 0.064 μg/ml. The recovery value of the method was determined as 99.61%. It was concluded that the parameters of precision, accuracy, and method robustness were appropriate for the validation procedures.

Efficient Estimation of ascorbic acid in vitamin C tablets enabled by phase-transfer strategy

In this paper, we introduced a novel phase-transfer strategy tailored for the efficient batch detection of ascorbic acid in vitamin C tablets. This method entailed the reaction between ascorbic acid and an excess of potassium permanganate. Subsequent reaction of the residual potassium permanganate with sodium oxalate in an acidic medium led to the generation of carbon dioxide. The quantification of the produced carbon dioxide was achieved using headspace GC, enabling the indirect measurement of ascorbic acid. The obtained findings revealed that the headspace method exhibited satisfied precision with a relative standard deviation of less than 2.11 % and high sensitivity with a limit of quantitation of 0.27 μmol. These results firmly establish the reliability of this innovative approach for determining ascorbic acid. In addition, the highly automated feature of headspace method significantly enhances the efficiency of batch sample detection and reduces the errors caused by human operation. Thus, the adoption of the transformed phase strategy has demonstrated its effectiveness in assessing ascorbic acid, especially for large-scale sample analysis in industrial applications, owing to its efficiency, precision, and sensitivity.

Development and validation of a multiresidue method for the determination of antibiotic residues in crawfish using LCMS/MS

ABSTRACT This study developed a rapid multi-class method for determining 29 antibiotic residues in crawfish using liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. A quick and affordable extraction method was employed, and sample preparation was performed using a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) technique. The extraction process involved adding acetonitrile to crawfish samples. The sample was homogenised with a solution of sodium citrate buffer and sodium EDTA, followed by a cleanup step. The method was validated according to European Union (EU) guidelines 2002/657/EC. The limit of quantitation (LOQ) for all antibiotics was 5 µg/kg, except for flumequine and trimethoprim, which had LOQs of 2.5 µg/kg. The LOQ for the tetracycline group was 25 µg/kg, and for chloramphenicol, it was 0.015 µg/kg. The average recoveries at different concentration levels varied between 60–120%. The precision, expressed as repeatability and reproducibility, was calculated to be less than 16%. Thirty crawfish samples collected from local Egyptian market were monitored for antibiotic residues. The results revealed contamination with antibiotics belonging to three different groups. Of the thirty samples, 27% were contaminated with ciprofloxacin and enrofloxacin, 17% with chlortetracycline and oxytetracycline, 7% with oxolinic acid, and 3% with sulphamethazine. The applicability of the developed method was proven through successful proficiency testing. The developed method met performance criteria and is suitable for monitoring these antibiotics in crawfish.

Micro-Milli Scale for the Removal of Iron and Copper by a Positively Charged Foam before Nickel Colorimetric Detection using Handy Spectrometer

Introduction: Simple alternative detection of nickel with iron and copper as interferences was proposed. The procedure was based on sampling a milligram sample and a micro-milliliter operation. Methods: The method has been applied to jewelry items. A 50 mg sample was digested by 5 mL of nitric acid with heating. The obtained solution was added with KSCN before passing through polyurethane foam (PUF) (1 cm i.d. × 8 cm length). Some metal ions-SCN complexed (e.g., Fe(III) and Cu(II)) were retained in the column while Ni(II) ions were in the eluate. A 200-500 µL aliquot was added with 4-(2-pyridylazo)-resorcinol (PAR) as the color reagent. At least 30 µL of a portion was measured for the absorbance of the color product using a handy spectrometer. Results: The positively charged foam could remove iron and copper altogether before determining nickel. A standard calibration was a plot of absorbance versus Ni(II) concentration for 1-30 mg/L: absorbance = 0.0123[Ni(II), mg/L] + 0.0435 (R2=0.9945) with a limit of detection (LOD) and limit of quantitation (LOQ) of 0.24 mg/L and 0.81 mg/L, respectively. Two bracelet samples showed the presence of nickel at 0.97 ± 0.25 and 0.27 ± 0.04 mg/g, respectively, and agreed with the reference FlameAAS method. Conclusion: The proposed method could be used to assay nickel in samples containing high levels of iron and copper, such as jewelry. This will benefit general wearers with health concerns associated with nickel, particularly in case of inexpensive accessories. The handy spectrometer used in the study might make be helpful to carry out these studies with a limited tight budget.

A ratiometric fluorescent probe for the determination of quinolone antibiotics in milk based on N and S co-doped carbon quantum dots

Quinolone antibiotics are widely used to prevent and treat diseases caused by bacterial infection. However, overuse of antibiotics may lead to their residue in the environment and food, posing potential threats to human health. In this study, a ratiometric fluorescent probe based on nitrogen and sulfur co-doped carbon quantum dots (N, S-CQDs) was synthesized, which can realize the detection of moxifloxacin (MXF), gatifloxacin (GAT) and ofloxacin (OFX) in milk. After addition of these antibiotics, the fluorescence at 440 nm originating from N, S-CQDs was significantly quenched due to the fluorescence resonance energy transfer (FRET), while the fluorescence at 525 nm (MXF), 500 nm (GAT) and 515 nm (OFX) were enhanced due to aggregation induced emission (AIE). The fluorescence changes were completed within 30 s and stabilized for at least 14 days. Good linear relationships between the fluorescence intensity ratios (F525/F440 for MXF, F500/F440 for GAT and F515/F440 for OFX) and the antibiotic concentrations ranging from 0.1 to 100 mg L−1 were obtained, with R2 above 0.99. The limits of quantitation were in the range of 1.67–6.20 μg L−1, and MXF, GAT and OFX can be well identified by linear discriminant analysis. The probe enabled quantitative analysis of MXF, GAT and OFX in milk samples, with recoveries ranging from 82% to 107%. A test strip based on the ratiometric fluorescence probe was successfully applied for the detection of MXF and GAT in milk in combination with a smartphone. This method exerted high specificity and sensitivity, which has the potential to achieve in-site detection of MXF, GAT and OFX in milk.

Efficient and environmentally friendly spectrofluorimetric determination of cariprazine: An analytical and green chemistry approach.

Cariprazine represents a new generation of antipsychotic medication, characterized by its heightened affinity for the D3 receptor. It has recently obtained approval as an adjunctive treatment option for patients diagnosed with major depressive disorder. In this study, a novel approach utilizing fluorescence spectroscopy was developed to analyze cariprazine. The methodology involves the transformation of cariprazine into a fluorescent compound by means of chemical derivatization with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl). Following excitation at 470 nm, the fluorescent derivative displayed peak fluorescence emission at 550 nm. The factors influencing the derivatization process were optimized. Upon reaching the optimal reaction conditions, a linear correlation (r2=0.9995) was observed between the fluorescence intensity and concentrations of cariprazine ranging from 20 to 400 ng/ml. Detection and quantitation limits were determined to be 5.85 and 17.74 ng/ml, respectively. The approach was accurate and precise, with percent recovery values ranging from 98.14% to 99.91% and relative standard deviations of less than 2%. Application of the method to the analysis of cariprazine in bulk and commercial capsules forms yielded accurate results. Moreover, adherence to environmentally friendly analytical practices was evident through alignment with the principles of green analysis, as demonstrated by the analytical eco-scale, AGREE, and GAPI greenness assessment tools.

Fast On-Site Electroanalysis of Eicosapentaenoic Acid Ethyl Ester in the Liver and Meat of Stingray Using a Stochastic Miniplatform Based on a 3D Stochastic Microsensor

Eicosapentaenoic acid ethyl ester has an important role in metabolism and it is also an important antithrombotic agent. Its concentration in the liver and meat of the stingray is essential when one would like to use the extracts containing the eicosapentaenoic acid ethyl ester from stingray as biopharmaceutical products. A miniplatform having as detection tool a 3D stochastic microsensor was designed and used for the assay of eicosapentaenoic acid ethyl ester from stingray liver and meat. Natural monocrystalline diamond paste was modified with a solution of heptakis(2,3,6-tri-O-methyl)-beta-cyclodextrin to obtain the modified diamond paste used in the 3D stochastic microsensor. A wide working concentration range (5.0 × 10−15 – 5.0 × 10−8) and a very low limit of quantitation (5.0 × 10−15) were attained. The proposed miniplatform was successfully used for the assay of eicosapentaenoic acid ethyl ester from stingray liver and meat with recoveries higher than 99.90%, and % RSD values lower than 0.05 (N = 10).

A validated UPLC-MS/MS method for the quantification of immunosuppressive drugs in peripheral blood mononuclear cells using liquid-liquid extraction with low temperature purification without complex pretreatment steps

Immunosuppressive drugs (ISDs) are given to avoid the allograft rejection after transplantation. The concentrations of ISDs should be closely monitored owing to their wide inter-individual variability in its pharmacokinetics and narrow therapeutic window. Currently, the whole blood concentration measurement is the major approach of therapeutic drug monitoring of clinical ISDs in organ transplantation. Its correlation with the efficacy of ISDs remains elusive. While the acute rejection after transplantation may occur even when whole-blood ISDs concentrations are within the target range. Since the site of action of ISDs are within the lymphocyte, direct measurement of drug exposure in target cells may more accurately reflect the clinical efficacy of ISDs. Although several methods have been developed for the peripheral blood mononuclear cells (PBMCs) extraction and drug concentration measurement, the complex pre-processing has limited the study of the relationship between intracellular ISDs concentrations and the occurrence of rejection. In this study, the extraction of ISDs in PBMCs was carried out by the liquid-liquid extraction with low temperature purification, without centrifugation. The lower limit of quantitation were 0.2 ng/mL for cyclosporine A, tacrolimus and sirolimus, 1.0 ng/mL for mycophenolic acid, and the within-run and between-run coefficient of variations were both less than 12.4 %. The calibration curves of mycophenolic acid had a linear range (ng/mL): 1.0–128.0 (r2 = 0.9992). The calibration curves of other three ISDs had a linear range (ng/mL): 0.2–20.48 (r2 > 0.9956). A total of 157 clinical samples were analyzed by the UPLC-MS/MS for ISDs concentration in blood or plasma ([ISD]blood or plasma) and the concentration within PBMCs ([ISD]PBMC). Although there was strong association between [ISD]PBMC and [ISD]blood or plasma, the large discrepancies between concentration within [ISD]blood or plasma and [ISD]PBMC were observed in a small proportion of clinical samples. The developed method with short analysis time and little amounts of blood sample can be successfully applied to therapeutic drug monitoring of ISDs in PBMCs for analysis of large numbers of clinical samples and is helpful to explore the clinical value of ISDs concentration in PBMCs.

Immunochromatographic Strip Based on Tetrahedral DNA Immunoprobe for the Detection of Aflatoxin B1 in Rice Bran Oil.

Aflatoxin B1 (AFB1), a widespread contaminant in food and feeds, poses a threat to the health of animals and humans. Consequently, it is significant to develop a rapid, precise and highly sensitive analytical method for the detection of AFB1. Herein, we developed an immunochromatographic strip (ICS) based on a tetrahedral DNA (TDN) immunoprobe for AFB1 determination in rice bran oil. Three sizes of TDN immunoprobes (AuNP-TDN13bp-mAb, AuNP-TDN17bp-mAb, AuNP-TDN26bp-mAb) were constructed, and the performance of these three immunoprobes, including the effective antibody labeling density and immunoaffinity, was measured and compared with that of the immunoprobe (AuNP-mAb) developed using the physical adsorption method. Subsequently, the optimal TDN immunoprobe, namely AuNP-TDN13bp-mAb, was selected to prepare the immunochromatographic strip (ICS) for the qualitative and quantitative detection of AFB1 in rice bran oil. The visual limits of detection (vLODs) of the ICS based on AuNP-TDN13bp-mAb and AuNP-mAb were 0.2 ng/mL and 2 ng/mL, with scanning quantitative limits (sLOQs) of 0.13 ng/mL and 1.4 ng/mL, respectively. The ICS demonstrated a wide linear range from 0.02 ng/mL to 0.5 ng/mL, with good specificity, accuracy, precision, repeatability, and stability. Moreover, a high consistency was observed between the constructed ICS and ultra-high-performance liquid chromatography (UPLC) in the quantification of AFB1. The results indicated that the introduction of TDN was beneficial for promoting efficient antibody labeling, protecting the bioactivity of immunoprobes, and increasing the sensitivity of detection, which would provide new perspectives for the achievement of the highly sensitive detection of mycotoxins.

Development of a simultaneous analytical method for the dietary exposure determination of β-Carboline alkaloids in foods

As β-carboline (βC) alkaloids, posing potential health risks, are present in a wide variety of foods, determining the exposure degrees of food to these alkaloids from dietary activity is key to ensuring food safety. Here, we developed a rapid and sensitive simultaneous analytical method for six βC alkaloids in food. We optimized the buffered QuEChERS method, which includes a clean-up process through dispersive solid phase extraction, to extract the target compounds from food matrices; then, these compounds were detected via liquid chromatography–tandem mass spectrometry. We established calibration ranges for each target compound and matrix within the range of 0.05–250 μg/kg, and verified linearity (R2 ≥ 0.99) and limit of quantitation (≤1.63 μg/kg). Furthermore, we validated trueness (85.8%–118.8%) and precision (≤18.7%) at three levels within the calibration range, including the lowest and highest concentrations. Finally, we employed the developed method to determine the βC alkaloid contents in 304 samples of 41 food items and dietary exposure of six βC alkaloids resulting from daily intake. Although βC alkaloids were detected in 86.2% of the samples, exposure level to the 41 food items was insufficient to cause toxicity.