Rapid Method For Determination Research Articles

Development of new methods for Determination of Sulpha Drugs with N-Chlorosacchrin Reagent

Sulpha drugs (sulphanilamide and their derivatives) are widely used as antibacterial drugs. An accurate and rapid method for quantitative determination of sulpha drugs and sulphanilamide would be of great importance. In literature several methods have been discussed for determination of sulphanilamide. The previous methods upon the evaluation of their nitrogen and sulphur contents while the latter were based upon the reaction of functional groups present in them.

Gold nanoparticle-enhanced D-shaped optical fiber sensor for mercury ion detection.

Mercury ions (Hg2+) are highly toxic heavy metal ions that pose serious health risks to humans when present at concentrations above the safety threshold. Therefore, the development of a rapid and effective Hg2+ detection method is of significant importance. In this study, based on surface plasmon resonance (SPR) technology integrated with COMSOL simulation analysis, a highly sensitive and selective Hg2+ sensing system is constructed. Initially, gold nanoparticles and the surface of a fiber-optic gold film are modified by sodium sulfide (Na2S). In the presence of Hg2+, the sulfur ions on the modified gold film and gold nanoparticles specifically bind to Hg2+, forming the composite structure Au/S-Hg2+-S/AuNPS. Due to the strong electromagnetic coupling between the gold nanoparticles and the gold film, a significant SPR wavelength shift occurs. These results show that the Hg2+ sensor has high sensitivity and enhanced selectivity. The detection limit for mercury ions was 8.15 nM, and the recovery rate in real environmental samples was up to 90.1-97.3%. This sensing system provides an alternative method for rapid and accurate determination of mercury content.

A high sensitivity adsorptive-electrochemical method for rapid and portable determination of hydroxychloroquine

A high sensitivity adsorptive-electrochemical method for rapid and portable determination of hydroxychloroquine

Method of rapid spectrophotometric determination of iron in dithionite extracts of soils

Amethod for the determination of dithionite iron for soil samples and fractions of the order of 20–25 mg with a spectrophotometric termination has been developed and optimized.Unlike the previously described methods, phenanthroline was used as a chromogen, which made it possible to simplify the analysis by eliminating the combustion stage.The procedure for processing samples with citrate-bicarbonate-dithionite extractant has been optimized.The repeatability and intra-laboratory reproducibility of the technique are investigated.Verification of the proposed methodology by comparison with the standard one showed good convergence of the results.

Development of an electrochemical sensor based on platinum nanoparticles/iron-based metal–organic framework composite for efficient determination of butylated hydroxyanisole

Butylated hydroxyanisole (BHA), a synthetic antioxidant, is widely used in the food industry to prevent the oxidative deterioration of food products. Developing rapid, simple and sensitive methods for BHA determination is of great importance to ensure the safety and quality of food. In this study, we developed an amperometric sensor based on iron-based metal–organic framework and platinum nanoparticle modified glassy carbon electrode (PtNP/Fe-MOF/GCE) for efficient determination of BHA. The Fe-MOF was synthesized by the solvothermal method and characterized using various techniques such as powder X-ray diffraction, thermogravimetric analysis, and differential scanning calorimetry. The synthesized Fe-MOF was modified onto GCE, and platinum nanoparticles were electrodeposited onto the Fe-MOF/GCE. Scanning electron microscopy and energy dispersive X-ray spectroscopy were utilized to enlighten the surface morphologies of the electrodes during the modification steps. Electrochemical characterization of the modified electrodes was performed by cyclic voltammetry and electrochemical impedance spectroscopy. Under the optimum conditions, the PtNP/Fe-MOF/GCE showed excellent electrocatalytic activity towards BHA oxidation due to its large surface area, porosity, and metal sites. The PtNP/Fe-MOF/GCE sensor exhibited a wide linear range from 6.0 × 10-8 to 5.4 × 10-5 M and a low detection limit of 9.4 × 10-9 M. The analytical applicability of the PtNP/Fe-MOF/GCE was tested by the analysis of BHA in potato chips samples.

A novel colorimetric sensor through peroxymonosulfate activated by CoFe@CN nanozymes for on-site resorcinol detection

The presence of resorcinol (RS) in water contaminated with pollutants may engender environmental and ecosystem risks. In this study, we developed rapid and efficient colorimetric methods for the on-site quantitative determination of RS. Specifically, a synthetic nanozyme composed of nitrogen-doped carbon-coated cobalt-iron (CoFe@CN) was utilized to initiate the oxidation reaction of 3,3′,5,5′-tetramethylbenzidine (TMB) with the activator of peroxymonosulfate (PMS). Compared to the activator of hydrogen peroxide (H2O2), PMS demonstrated a sixfold enhancement in catalytic efficacy, markedly elevating the detection performance. Density Functional Theory calculations indicate that RS can serve as a reducing agent for oxTMB, confirming the theoretical feasibility of this process. A linear relationship between inhibition rate (IR %) of RS concentration and absorbance was established and the colorimetric analysis revealed a linear relationship between RS concentration and gray scale values over the range of 0–45 μM, with a detection limit of 3.39 μM. Furthermore, smartphone-based analysis of color images allows for on-site quantitative analysis of RS concentration, leveraging portability and real-time detection capabilities. This study provides pioneering analytical support for on-site water quality monitoring within the ecological environment.

Chromatographic method for rapid determination of triazoles in ribavirin intermediates synthesis: stationary phase comparison

Chromatographic method for rapid determination of triazoles in ribavirin intermediates synthesis: stationary phase comparison

Development of a rapid method for determination of OchratoxinA in grape mash and wine.

The occurrence of Ochratoxin A (OTA) in wine is commonly known, but there is only limited information about its occurrence in grape mash and wines of German origin. Climate change has led to higher temperatures in the southern regions of Germany, which may increase the growth of fungi associated with the production of OTA and increase the content of this mycotoxin in grapes. A safe and rapid UHPLC-FLD method was developed and validated to assess the contamination of grape mash and wine with OTA. A total of 71 samples of grape mash and 30 wines from various wine producers in Baden-Württemberg, Germany, were analysed for OTA content. The results showed that no samples contained OTA in concentrations above the limit of detection. Further monitoring of samples from different vintages is needed.

A modified pararosaniline hydrochloride method for determination of total and bound sulfur dioxide in wine

An improved pararosaniline hydrochloride (PRA) method for rapid and accurate determination of total and bound sulfur dioxide (SO2) in wine was established. The determination conditions for total SO2 were optimized in model wine systems. The pH of the acidified PRA reagent had a significant effect on the color and the maximum absorption wavelength (λmax) of the reaction system, with its optimum pH 0.48 and a λmax at 549 nm. The addition of ethylene diamine tetraacetic acid (EDTA) could effectively shield the interference of coexisting metal ions present in wine, and a novel approach to double background subtraction was confirmed to remove the matrices interference of red wine color. Under the optimum conditions, the linear range for total SO2 in wine was within 1.00–8.00 mg L−1 (R = 0.9975), with the detection and quantification limits (MDL and MQL) found as 0.02 and 0.06 mg L−1, respectively. The recovery of SO2 ranged from 85.73 % to 105.70 % with the relative standard deviations (RSD) of 0.21 % - 7.78 %, suggesting high sensitivity and accuracy of the method. Combining with the optimized Monier-Williams method, the determination of bound SO2 in wine was also achieved. Sulfite determination can be performed in wine using the rapid, accurate and sensitive method without any pretreatment, and the results were comparable with those of the standard methods.

Deep eutectic solvent-mediated synthesis of ZnCo2O4/MWCNT-COOH: Investigation of electrocatalytic activity for gatifloxacin detection

The overuse of gatifloxacin seriously pollutes the environment and cause potential harm to our health. Hence, it is imperative to develop a rapid and sensitive method for gatifloxacin determination. Herein, an efficient electrocatalyst was designed for the voltammetric determination of gatifloxacin based on carboxylated multiwalled carbon nanotubes warped ZnCo2O4 nanoparticles (ZnCo2O4/MWCNT-COOH). The ZnCo2O4 nanoparticles were synthesized by a green deep eutectic solvent-mediated ion-thermal route, and further composited with MWCNTs-COOH. The ZnCo2O4/ MWCNT-COOH combined the catalytic activity of ZnCo2O4 with the high electrical conductivity of MWCNT-COOH, aiming to improve the electrochemical sensing performance toward gatifloxacin. The synergistic interactions between ZnCo2O4 and MWCNT-COOH endowed the ZnCo2O4/MWCNT-COOH with extraordinary catalytic activity for gatifloxacin oxidation. Consequently, the ZnCo2O4/MWCNT-COOH displayed a wide linear response range (0.01–10 μM) for detecting gatifloxacin, with a high sensitivity (29.64 μA μM−1 cm−2) and low detection limit (2.0 nM). The ZnCo2O4/MWCNT-COOH showed robust voltammetric responses against potential interfering species, and maintained highly stable responses for at least two weeks. Moreover, the ZnCo2O4/MWCNT-COOH/GCE was successfully used to detect gatifloxacin in water samples with satisfactory recoveries (97.22 − 104.5 %). Together with its low cost, environment friendly and rapid response, the ZnCo2O4/MWCNT-COOH shows promising prospects in trace detection of gatifloxacin.

Application of a Green Deep Eutectic Solvent for Preconcentration and Determination of Copper and Cadmium in Food, Cosmetic, and Water Samples

Background:: Determination of environmental pollutants is important due to their harmful effects on the health of living organisms. However, direct measurement of many of these pollutants is not possible due to their low concentrations, which necessitates the need for sample preparation methods. One of the rapid and simple sample preparation methods is the Air-Agitated Liquid-Liquid Microextraction (AALLME) method, which requires toxic organic solvents that can lead to environmental pollution. Therefore, finding green solvents like Deep Eutectic Solvents (DESs) to replace them can be investigated. Methods:: A novel Deep Eutectic Solvent (DES) was synthesized from a combination of choline chloride and 2-phenylethanol with a molar ratio of 1:4, and it was examined using FT-IR analysis. This solvent was used in an AALLME method for measuring copper and cadmium heavy metal ions in complex real samples with Flame Atomic Absorption Spectroscopy (FAAS). Results:: The influential parameters of this method, such as solution pH (5.4), extraction cycles (12), and extraction solvent volume (440 μL), were optimized utilizing central composite design (CCD). Underneath the optimized circumstances, the detection limits for Cu2+ and Cd2+ were 0.14 and 0.09 ng mL-1, and the linear dynamic range was 0.47-50.0 and 0.32-22.5 ng mL-1, respectively. The preconcentration factors for these cations were 139.7 and 133.4, respectively. Conclusion:: Combining this novel green solvent and rapid sample preparation method for the preconcentration and determination of the studied heavy metal ions has shown promising results in terms of enrichment factors and detection limit values.

Concepts for a New Rapid and Simple HPLC Method for Simultaneous Determination of Rosuvastatin and Perindopril in Dosage Forms

ABSTRACTSimultaneous determination of a tandem of drugs like perindopril and rosuvastatin with differences in water and organic solvent solubilities, hydrophobicity, polarities, and UV‐absorbing possibilities between them necessitates careful selection of chromatographic conditions. The four specified and different bonded reversed‐phase columns were tested with running mobile phases containing various composition contents concepts; the concept of using diluted trifluoroacetic acid in mobile phase composition with acetonitrile enabled simultaneous acidification and weak ion‐pairing with protonized molecules of analytes, yielding appropriate, short, reasonable run times and resolutions of analytes, satisfying UV‐transparency, and good peak symmetries. These facts especially stand for the peak of perindopril, as a member of the group of proline‐containing moiety in its structure, often and easily prone to peak‐tailing, skewing, or splitting on the high‐performance liquid chromatography chromatograms, which is usually solved by using alkyl‐sulfonate base and ion pairs on higher concentrations of buffering salts with low pH values and with column temperatures increasing by 50°C–60°C. Linearity range was 0.002/004–0.5 mg/mL. The score for method AGREE was 0.73–0.77. The method development approaches, with all columns employing our concepts in mobile phases and experimental conditions, can cover the complete needs and demands of quality control departments and laboratories as simple high‐throughput analysis methods.

A Low-cost and Rapid Method for Determination of Five Flavonoids in Herbal Medicines with Rutin by HPLC-UV at Equal Absorption Wavelength

Background: Flavonoid is a type of active constituent in herbs and always used as the quality control markers of herbal medicines. Owing to the extensive diversity of flavonoids, numerous reference compounds are necessitated for the analysis of flavonoids, and some are usually very expensive, which engenders challenges in the analysis of flavonoids in herbal medicines. Consequently, the development of a simple, rapid, and reference compounds saving method is important for the determination of flavonoids in herbal medicines. Objective: In order to develop a high-performance liquid chromatography (HPLC) method for the determination of 5 flavonoids (mangiferin, hesperidin, baicalin, buddleoside, and rutin) in five herbal medicines (Anemarrhenae rhizome, Sophorae flos, Citri reticulatae pericarpium, Scutellariae radix, and Chrysanthemi indici flos) with rutin. Methods: Five herbal medicine samples were prepared according to the Chinese Pharmacopoeia which includes ultrasound and reflux methods. The separation of the sample was performed on a PoroShell 120 EC-C18 (4.6 mm×100 mm, 2.7 µm) by gradient elution with 0.1% formic acid and acetonitrile at a flow rate of 1.0 mL/min. The wavelengths were set as follows: Anemarrhenae rhizome (363 nm), Sophorae flos (256 nm), Citri reticulatae pericarpium (236 nm), Scutellariae radix (263 nm), Chrysanthemi indici flos (354 nm). Results: The method validation showed that the established HPLC method was accurate and stable for quantitative analysis of flavonoids in five herbal medicines. The comparative analysis revealed that the determination results of the current HPLC method and Chinese Pharmacopoeia method are consistent, exhibiting less than 1% relative error. Remarkably, the developed HPLC method needs one cheapest reference compound (rutin) and costs 8 min for sample HPLC analysis. Conclusion: The developed HPLC method for quantitative analysis of five flavonoids in five herbal medicines is simple, rapid, and reference compound saving, which provides a good alternative method for quality control of flavonoids in herbal medicines.

Bismuth Film along with dsDNA-Modified Electrode Surfaces as Promising (bio)Sensors in the Analysis of Heavy Metals in Soils.

Heavy metals constitute pollutants that are particularly common in air, water, and soil. They are present in both urban and rural environments, on land, and in marine ecosystems, where they cause serious environmental problems since they do not degrade easily, remain almost unchanged for long periods, and bioaccumulate. The detection and especially the quantification of metals require a systematic process. Regular monitoring is necessary because of seasonal variations in metal levels. Consequently, there is a significant need for rapid and low-cost metal determination methods. In this study, we compare and analytically validate absorption spectrometry with a sensitive voltammetric method, which uses a bismuth film-plated electrode surface and applies stripping voltammetry. Atomic absorption spectroscopy (AAS) represents a well-established analytical technique, while the applicability of anodic stripping voltammetry (ASV) in complicated sample matrices such as soil samples is currently unknown. This sample-handling challenge is investigated in the present study. The results show that the AAS and ASV methods were satisfactorily correlated and showed that the metal concentration in soils was lower than the limit values but with an increasing trend. Therefore, continuous monitoring of metal levels in the urban complex of a city is necessary and a matter of great importance. The limits of detection of cadmium (Cd) were lower when using the stripping voltammetry (SWASV) graphite furnace technique compared with those obtained with AAS when using the graphite furnace. However, when using flame atomic absorption spectroscopy (flame-AAS), the measurements tended to overestimate the concentration of Cd compared with the values found using SWASV. This highlights the differences in sensitivity and accuracy between these analytical methods for detecting Cd. The SWASV method has the advantage of being cheaper and faster, enabling the simultaneous determination of heavy elements across the range of concentrations that these elements can occur in Mediterranean soils. Additionally, a dsDNA biosensor is suggested for the discrimination of Cu(I) along with Cu(II) based on the oxidation peak of guanine, and adenine residues can be applied in the redox speciation analysis of copper in soil, which represents an issue of great importance.

Ceftobiprole quantification in human serum by HPLC-UV to implement routine TDM in clinical practice

Background and aimsCeftobiprole is a recent 5th generation parenteral cephalosporin with antibacterial activity against a large range Gram+ and Gram− bacteria. Therapeutic drug monitoring (TDM) is an essential tool for maintaining plasma concentrations of antibiotics above the MIC by the end of the dosing interval, thus preventing the resistant strain diffusion. TDM is already recommended for other cephalosporins, and it is a reasonable tool contributing to the safety and efficacy of these drugs. During the treatment of patients in real-life, a number of pharmacokinetic (PK) changes not normally seen in healthy volunteers can occur which can impair the pharmacokinetic/pharmacodynamic target attainment.We aimed to develop simple and rapid HPLC-UV method for determination of ceftobiprole in human serum to implement TDM in clinical practice and support PKs and pharmacokinetic/pharmacodynamic (PK/PD) studies. Materials and methodsSamples preparation of calibration standards, QC, and anonymous patients serum samples was performed by protein precipitation by adding 0.01 ml of sulphosalicylic acid at 30 % to 0.1 ml of each sample. Then samples were vortexed and the centrifuged at 12,000 rpm for 10 min at 4 °C. Fifty microlitres of clear supernatant were diluted 1:1 with mobile phase and transferred into HPLC autosampler held at 8 °C. Chromatographic separation was carried out in a gradient mode at 35 °C on an ultra-Biphenyl column using a Thermo Scientific chromatographic system with a Diode array. Data management was performed with Chromeleon 7.4 software. ResultsThe HPLC-UV method proved to be linear over wide concentration ranges (0.5–50.0 mg/L) and was accurate and reproducible in the absence of matrix effects, allowing for robust, specific, and rapid quantification of ceftobiprole from a low amount of serum (0.1 mL). The mean steady state Ctrough and Cend values measured in the anonymous patients’ samples were 6.26 ± 3.81 mg/L and 22.56 ± 15.69 mg/L, respectively. ConclusionsWe report a broadened simple and fast HPLC with UV detection method for quantification of ceftobiprole in human serum to implement ceftobiprole TDM as clinical routine, and support future (PK/PD) studies in special patients’ population.

Development of a Rapid Method for Simultaneous Determination of Pesticides in Plant Oil Using GC-MS/MS

Development of a Rapid Method for Simultaneous Determination of Pesticides in Plant Oil Using GC-MS/MS

Rapid quantitative determination method of four heavy metals in strawberry

A rapid quantitative determination method of mercury, arsenic and arsenic, cadmium and chromium in strawberry was established. The sample to be tested was prepared into the solution to be tested, and the content of mercury, arsenic, cadmium and chromium were determined respectively on the machine. The results showed that the correlation coefficient of the standard curves of the four heavy metals was within 0.9961.000, and the detection limit was 0 mercury 0.028 g / kg, arsenic 0.062 g / kg, cadmium 0.14 g / kg, chromium 4.76 g / kg; the recovery was 80.2% 108.3% and 1.58% 26.34%; the test results of the standard samples were within the standard value. The method established in this experiment can determine the four heavy metals of mercury, arsenic, cadmium and chromium, etc. It has good linear correlation, low detection limit, good accuracy, high safety, simple operation, batch processing, and saves reagent consumables and detection time.

Rapid analysis method for process parameter determination of transient thermal tensioning during welding buckling distortion mitigation

The effect of transient thermal tensioning (TTT) on mitigating buckling distortion is significantly influenced by the process parameters. TTT and conventional welding (CW) experiments were both performed on butt welded joints using induction heating as an additional heat source. The thermal elastic plastic (TEP) FE simulation was then carried out with consideration of material nonlinearity and geometrical nonlinearity to investigate the temperature, buckling distortion fields of the butt welded joints. A good agreement between computational results and the measurement was represented, and the buckling distortion of the butt welded joints with TTT was much smaller than that with CW. Based on the validated FE simulation, the sensitivity of process parameters (amount, sizes, tensioning temperature Ttmax, locations of induction heating) for TTT was examined in detail. The results show that amount and sizes exerted an evident impact on buckling distortion mitigation, which were determined by equipment. Tensioning temperature Ttmax and the offset from weld centerline d1 are more important parameters on effectively mitigating welding buckling distortion of thin plate structures than the offset from welding arc d2. Through optimizing Ttmax and d1, buckling distortion of examined butt welded joint can be reduced by more than 80 %. Moreover, a method for determining the process parameters of TTT towards engineering applications was proposed. Firstly, the amount and sizes of additional heat sources are maximized per the available equipment. Secondly, Ttmax is recommended as yield temperature to implement TTT and d1 is optimized through an experiment or TEP FE simulation. Eventually, the offset from welding arc d2 is further optimized when the manufacturing precisions are not reached.

The complexation color development—visible spectrophotometry method for rapid determination of Ca2+ concentration in mine wastewater and its mechanism

Ca2+ is an important cation in coagulants used in the treatment of mine wastewater such as coal slime water, and its concentration directly affects the settling and flotation of coal slime water. The rapid determination of Ca2+ concentration is of great significance to guiding industrial production. Herein, the complexation color development—visible spectrophotometry (CCDVS) method was proposed to obtain the concentration information of Ca2+, wherein 1-(1-Hydroxy-4-methyl-2-phenylazo)-2-naphthol-4-sulfonic acid (Calmagite) was used as an indicator and the mechanism of complexation between the indicator and Ca2+ was explored. The strong correlation between spectral data and Ca2+ concentration (R2 = 0.997) indicated that this method could be used for Ca2+ detection, thereby a quantitative model was proposed to predict Ca2+ concentration by using the complexation color development—visible light absorption data. The chemical element and bonding analysis confirmed that Ca2+ was complexed with the sulfonic acid group on the indicator skeleton in the form of Ca(OH)+ intermediate in an alkaline environment. The generated complexation product (-S-O-Ca(OH)+) could stably absorb 620 nm light energy, and its absorption performance remained 99.8% after standing for 60 min. The relative standard deviation of the detection results of Ca2+ in different calcium source solutions was as low as 1.24%, which confirmed the strong calcium source compatibility of the proposed method. More importantly, the successful application of this method in the determination of Ca2+ concentration at different points in industrial coal slime water system proved its advantages of high accuracy (relative error is as low as 5.01%), low cost and simple operation. The LOD of this method is 0.038 mg/L. Therefore, the complexation color development—visible spectrophotometry method can maximize the potential for cost reduction and efficiency improvement in mine wastewater treatment.

Mechanical Method for Rapid Determination of Step Count Sensor Settings.

With the increased push for personalized medicine, researchers and clinicians have begun exploring the use of wearable sensors to track patient activity. These sensors typically prioritize device life over robust onboard analysis, which results in lower accuracies in step count, particularly at lower cadences. To optimize the accuracy of activity-monitoring devices, particularly at slower walking speeds, proven methods must be established to identify suitable settings in a controlled and repeatable manner prior to human validation trials. Currently, there are no methods for optimizing these low-power wearable sensor settings prior to human validation, which requires manual counting for in-laboratory participants and is limited by time and the cadences that can be tested. This article proposes a novel method for determining sensor step counting accuracy prior to human validation trials by using a mechanical camshaft actuator that produces continuous steps. Sensor error was identified across a representative subspace of possible sensor setting combinations at cadences ranging from 30 steps/min to 110 steps/min. These true errors were then used to train a multivariate polynomial regression to model errors across all possible setting combinations and cadences. The resulting model predicted errors with an R2 of 0.8 and root-mean-square error (RMSE) of 0.044 across all setting combinations. An optimization algorithm was then used to determine the combinations of settings that produced the lowest RMSE and median error for three ranges of cadence that represent disabled low-mobility ambulators, disabled high-mobility ambulators, and healthy ambulators (30-60, 20-90, and 30-110 steps/min, respectively). The model identified six setting combinations for each range of interest that achieved a ±10% error in cadence prior to human validation. The anticipated range of errors from the optimized settings at lower walking speeds are lower than the reported errors of wearable sensors (±30%), suggesting that pre-human-validation optimization of sensors may decrease errors at lower cadences. This method provides a novel and efficient approach to optimizing the accuracy of wearable activity monitors prior to human validation trials.