limit of detection
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Analytica ◽  
2022 ◽  
Vol 3 (1) ◽  
pp. 24-35
Daniel Baecker ◽  
Sebastian Guenther

This communication introduces the first-time application of high-resolution continuum-source molecular absorption spectrometry (HR CS MAS) for the quantification of a peptide. The graphite furnace technique was employed and the tripeptide glutathione (GSH) served as a model compound. Based on measuring sulfur in terms of carbon monosulfide (CS), a method was elaborated to analyze aqueous solutions of GSH. The most prominent wavelength of the CS molecule occurred at 258.0560 nm and was adduced for monitoring. The methodological development covered the optimization of the pyrolysis and vaporization temperatures. These were found optimally to be 250 °C and 2250 °C, respectively. Moreover, the effect of modifiers (zirconium, calcium, magnesium, palladium) on the absorption signals was investigated. The best results were obtained after permanent coating of the graphite tube with zirconium (total amount of 400 μg) and adding a combination of palladium (10 µL, 10 g L−1) and calcium (2 µL, 1 g L−1) as a chemical modifier to the probes (10 µL). Aqueous standard samples of GSH were used for the calibration. It showed a linear range of 2.5–100 µg mL−1 sulfur contained in GSH with a correlation coefficient R2 > 0.997. The developed method exhibited a limit of detection (LOD) and quantification (LOQ) of 2.1 µg mL−1 and 4.3 µg mL−1 sulfur, respectively. The characteristic mass accounted for 5.9 ng sulfur. The method confirmed the general suitability of MAS for the analysis of an oligopeptide. Thus, this study serves as groundwork for further development in order to extend the application of classical atomic absorption spectrometry (AAS).

Biosensors ◽  
2022 ◽  
Vol 12 (1) ◽  
pp. 45
Xia Hong ◽  
Yin Cui ◽  
Ming Li ◽  
Yifan Xia ◽  
Daolin Du ◽  

A magnetic-based immunoassay (MBI) combined with biotin-streptavidin amplification was proposed for butyl benzyl phthalate (BBP) investigation and risk assessment. The values of LOD (limit of detection, IC10) and IC50 were 0.57 ng/mL and 119.61 ng/mL, with a detection range of 0.57–24977.71 ng/mL for MBI. The specificity, accuracy and precision are well demonstrated. A total of 36 environmental water samples of urban sewage from Zhenjiang, China, were collected and assessed for BBP contamination. The results show that BBP-positive levels ranged from 2.47 to 89.21 ng/mL, with a positive rate of 77.8%. The health effects of BBP in the urban sewage were within a controllable range, and the ambient severity for health (ASI) was below 1.49. The highest value of AS for ecology (ASII) was 7.43, which indicates a potential harm to ecology. The entropy value of risk quotient was below 100, the highest being 59.47, which poses a low risk to the environment and ecology, indicating that there is a need to strengthen BBP controls. The non-carcinogenic risk of BBP exposure from drinking water was higher for females than that for males, and the non-carcinogenic risk from drinking-water and bathing pathways was negligible. This study could provide an alternative method for detecting BBP and essential information for controlling BBP contamination.

Molecules ◽  
2022 ◽  
Vol 27 (2) ◽  
pp. 542
Yiliang Cheng ◽  
Jennifer Rae Savits ◽  
Aude Annie Watrelot

Cold-hardy interspecific hybrid grape varieties (Vitis spp.) have distinctive chemical compositions such as high acidity, a high content of anthocyanin diglucoside and a low condensed tannins content, compared to Vitis vinifera varieties. Considering the importance of phenolic compounds on the quality of red wine, a mechanical maceration technique, accentuated cut edges (ACE), has been evaluated when applied directly to crushed grapes (ACE-C), and 24 h before pressing (ACE-P), to improve the extraction of phenolic compounds. Samples were collected at crushing, bottling, and after five months of aging. Phenolic compounds and color characteristics of the wines were analyzed by high-performance liquid chromatography (HPLC) with diode array and fluorescence detectors and UV-Visible spectrophotometry. The color intensity, non-anthocyanin monomeric compounds and total iron-reactive phenolics content increased after applying ACE, compared to the control (CTL) after aging, and was significantly higher (37%) after ACE-C, compared to ACE-P. However, the concentration of condensed tannins was below the limit of detection in all the samples, indicating that ACE did not help their extraction or further interactions occurred with disrupted cell wall material. Applying ACE at crushing was considered as the optimum time to achieve a higher color stability in Marquette red wines.

Coatings ◽  
2022 ◽  
Vol 12 (1) ◽  
pp. 97
Olga Bochkova ◽  
Alexey Dovjenko ◽  
Rustem Zairov ◽  
Kirill Kholin ◽  
Rinata Biktimirova ◽  

The present work introduces coordinative binding of CuII ions with both amino-functionalized silica nanoparticles (SNs) and green-emitting carbon dots (CDs) as the pregrequisite for the CuII-assisted self-assembly of the CDs at the surface of the SNs. The produced composite SNs exhibit stable in time stimuli-responsive green fluorescence derived from the CuII-assisted assemblage of CDs. The fluorescence response of the composite SNs is sensitive to the complex formation with glutathione (GSH), enabling them to detect it with the lower limit of detection of 0.15 μM. The spin-trap-facilitated electron spin resonance technique indicated that the composite SNs are capable of self-boosting generation of ROS due to CuII→CuI reduction by carbon in low oxidation states as a part of the CDs. The intensity of the ESR signals is enhanced under the heating to 38 °C. The intensity is suppressed at the GSH concentration of 0.35 mM but is enhanced at 1.0 mM of glutathione, while it is suppressed once more at the highest intracellular concentration level of GSH (10 mM). These tendencies reveal the concentrations optimal for the scavenger or reductive potential of GSH. Flow cytometry and fluorescence and confocal microscopy methods revealed efficient cell internalization of SNs-NH2-CuII-CDs comparable with that of “free” CDs.

2022 ◽  
Vol 8 (1) ◽  
Stefan Nedelcu ◽  
Kishan Thodkar ◽  
Christofer Hierold

AbstractCustomizable, portable, battery-operated, wireless platforms for interfacing high-sensitivity nanoscale sensors are a means to improve spatiotemporal measurement coverage of physical parameters. Such a platform can enable the expansion of IoT for environmental and lifestyle applications. Here we report a platform capable of acquiring currents ranging from 1.5 nA to 7.2 µA full-scale with 20-bit resolution and variable sampling rates of up to 3.125 kSPS. In addition, it features a bipolar voltage programmable in the range of −10 V to +5 V with a 3.65 mV resolution. A Finite State Machine steers the system by executing a set of embedded functions. The FSM allows for dynamic, customized adjustments of the nanosensor bias, including elevated bias schemes for self-heating, measurement range, bandwidth, sampling rate, and measurement time intervals. Furthermore, it enables data logging on external memory (SD card) and data transmission over a Bluetooth low energy connection. The average power consumption of the platform is 64.5 mW for a measurement protocol of three samples per second, including a BLE advertisement of a 0 dBm transmission power. A state-of-the-art (SoA) application of the platform performance using a CNT nanosensor, exposed to NO2 gas concentrations from 200 ppb down to 1 ppb, has been demonstrated. Although sensor signals are measured for NO2 concentrations of 1 ppb, the 3σ limit of detection (LOD) of 23 ppb is determined (1σ: 7 ppb) in slope detection mode, including the sensor signal variations in repeated measurements. The platform’s wide current range and high versatility make it suitable for signal acquisition from resistive nanosensors such as silicon nanowires, carbon nanotubes, graphene, and other 2D materials. Along with its overall low power consumption, the proposed platform is highly suitable for various sensing applications within the context of IoT.

Abolfazl Darroudi ◽  
Saeid Nazari ◽  
Seyed Ali Marashi ◽  
Mahdi Karimi-Nazarabad

Abstract An accurate, rapid, simple, and novel technique was developed to determine simvastatin (SMV). In this research, a screen-printed electrode (SPE) was deposited with graphene oxide (GO) and sodium dodecyl sulfate (SDS), respectively. For the first time, the handmade modified SPE measured the SMV by differential pulse voltammetry (DPV) with high sensitivity and selectivity. The results of cyclic voltammetry indicated the oxidation irreversible process of SMV. Various parameters (pH, concentration, scan rate, support electrolyte) were performed to optimize the conditions for the determination of SMV. Under the optimum experiment condition of 0.1 M KNO3 as support electrolyte and pH 7.0, the linear range was achieved for SMV concentration from 1.8 to 36.6 µM with a limit of detection (LOD), and a limit of quantitation (LOQ) of 0.06 and 1.8 µM, respectively. The proposed method was successfully utilized to determine SMV in tablets and urine samples with a satisfactory recovery in the range of 96.2 to 103.3%.

Chemosensors ◽  
2022 ◽  
Vol 10 (1) ◽  
pp. 33
Anastasia Goida ◽  
Yurii Kuzin ◽  
Vladimir Evtugyn ◽  
Anna Porfireva ◽  
Gennady Evtugyn ◽  

A highly sensitive electrochemical DNA sensor for detection of the chemotherapeutic drug idarubicin mediated by Methylene blue (MB) has been developed. DNA from fish sperm has been immobilized at the electropolymerized layers of Azure B. The incorporation of MB into the DNA layers substantially increased the sensor sensitivity. The concentration range for idarubicin determination by cyclic voltammetry was from 1 fM to 0.1 nM, with a limit of detection (LOD) of 0.3 fM. Electrochemical impedance spectroscopy (EIS) in the presence of a redox probe ([Fe(CN)6]3−/4−) allowed for the widening of a linear range of idarubicin detection from 1 fM to 100 nM, retaining LOD 0.3 fM. The DNA sensor has been tested in various real and artificial biological fluids with good recovery ranging between 90–110%. The sensor has been successfully used for impedimetric idarubicin detection in medical preparation Zavedos®. The developed DNA biosensor could be useful for the control of the level of idarubicin during cancer therapy as well as for pharmacokinetics studies.

2022 ◽  
Vol 9 ◽  
Huaxu Zhou ◽  
Yao Ding ◽  
Ruobing Su ◽  
Dongming Lu ◽  
Hongliang Tang ◽  

Convenient and sensitive detection of active analytes in complex matrix is crucial in biological, medical, and environmental analysis. Silica nanochannel array film (SNF) equipped electrochemical sensors have shown excellent anti-fouling performance in direct analysis of complex samples. In this work, we demonstrated an electrochemical sensor with anti-fouling performance for highly sensitive detection of acetaminophen (APAP) based on SNF supported by ß-cyclodextrin-graphene (CDG) nanocomposite modified Au film electrode (AuF). Because of their rich surface hydroxyls and 2D lamellar structure, CDG on AuF can serve as the nanoadhesive for compact binding SNF, which can be grown by electrochemical assisted self-assembly method in a few seconds. Attributable to the electrocatalytic property of graphene and the synergistic enrichment from both CD and SNF nanochannels towards analyte, the SNF/CDG/AuF sensor demonstrates sensitive detection of acetaminophen ranged from 0.2 to 50 μM with an ultralow limit-of-detection of 14 nM. Taking advantage of the anti-fouling ability of SNF, the sensor is able to realize accurate and convenient analysis of APAP in commercially available paracetamol tablets.

Olha Dushna ◽  
Liliya Dubenska ◽  
Serhiy Plotycya ◽  
Mariana Rydchuk ◽  
Mykola Blazheyevskіy

Abstract In the present paper, for the first time, the electrochemical behaviour of nicotine metabolite nicotine N-oxide (NNO) on static mercury dropping electrode (SMDE) and mercury meniscus modified silver solid amalgam electrode (m-AgSAE) has been reported. Nicotine N-oxide is reduced forming one peak at the potential -0.78 V on SDME and -0.86 V on m-AgSAE in Britton-Robinson buffer medium at pH 4.5 using cyclic voltammetry (CV). One electron and one proton take part in the reaction of NNO reduction. Calibration graphs for NNO determination using linear sweep voltammetry (LSV) on SDME and square-wave voltammetry (SWV) and differential pulse voltammetry (DPV) on m-AgSAE were obtained. Limit of detection (LOD) is 0.13 μM on SDME, and 0.16 μM (SWV) and 0.29 μM (DPV) on m-AgSAE. Since NNO can be used as an analytical form for nicotine voltammetric determination, so the developed methods were applied for the analysis of pharmaceutical preparations, and the recoveries from 97.3 to 104.6 % were achieved. Also, the elaborated methods were used in the analysis of biological fluids, and tobacco products. The obtained results were compared to those indicated in the certificates of drugs analysis, and to the results, obtained by reference methods (HPLC and GC).

Sensors ◽  
2022 ◽  
Vol 22 (2) ◽  
pp. 618
Mizaj Shabil Sha ◽  
Muni Raj Maurya ◽  
Mithra Geetha ◽  
Bijandra Kumar ◽  
Aboubakr M. Abdullah ◽  

Carbon dioxide (CO2) is a greenhouse gas in the atmosphere and scientists are working on converting it to useful products, thereby reducing its quantity in the atmosphere. For converting CO2, different approaches are used, and among them, electrochemistry is found to be the most common and more efficient technique. Current methods for detecting the products of electrochemical CO2 conversion are time-consuming and complex. To combat this, a simple, cost-effective colorimetric method has been developed to detect methanol, ethanol, and formic acid, which are formed electrochemically from CO2. In the present work, the highly efficient sensitive dyes were successfully established to detect these three compounds under optimized conditions. These dyes demonstrated excellent selectivity and showed no cross-reaction with other products generated in the CO2 conversion system. In the analysis using these three compounds, this strategy shows good specificity and limit of detection (LOD, ~0.03–0.06 ppm). A cost-effective and sensitive Internet of Things (IoT) colorimetric sensor prototype was developed to implement these dyes systems for practical and real-time application. Employing the dyes as sensing elements, the prototype exhibits unique red, green, and blue (RGB) values upon exposure to test solutions with a short response time of 2 s. Detection of these compounds via this new approach has been proven effective by comparing them with nuclear magnetic resonance (NMR). This novel approach can replace heavy-duty instruments such as high-pressure liquid chromatography (HPLC), gas chromatography (G.C.), and NMR due to its extraordinary selectivity and rapidity.

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