Development of an Immunofluorescence Assay Module for Determination of the Mycotoxin Zearalenone in Water

Project Aquafluosense is designed to develop prototypes for a fluorescence-based instrumentation setup for in situ measurements of several characteristic parameters of water quality. In the scope of the project an enzyme-linked fluorescent immunoassay (ELFIA) method has been developed for the detection of several environmental xenobiotics, including mycotoxin zearalenone (ZON). ZON, produced by several plant pathogenic Fusarium species, has recently been identified as an emerging pollutant in surface water, presenting a hazard to aquatic ecosystems. Due to its physico-chemical properties, detection of ZON at low concentrations in surface water is a challenging task. The 96-well microplate-based fluorescence instrument is capable of detecting ZON in the concentration range of 0.09–400 ng/mL. The sensitivity and accuracy of the analytical method has been demonstrated by a comparative assessment with detection by high-performance liquid chromatography and by total internal reflection ellipsometry. The limit of detection of the method, 0.09 ng/mL, falls in the low range compared to the other reported immunoassays, but the main advantage of this ELFIA method is its efficacy in combined in situ applications for determination of various important water quality parameters detectable by induced fluorimerty—e.g., total organic carbon content, algal density or the level of other organic micropollutants detectable by immunofluorimetry. In addition, the immunofluorescence module can readily be expanded to other target analytes if proper antibodies are available for detection.

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Fast UHPLC-MS/MS for the Simultaneous Determination of Azithromycin, Erythromycin, Fluoxetine and Sotalol in Surface Water Samples

Applied Sciences ◽

10.3390/app11188316 ◽

2021 ◽

Vol 11 (18) ◽

pp. 8316

Author(s):

Mira Azzi ◽

Sylvain Ravier ◽

Assem Elkak ◽

Bruno Coulomb ◽

Jean-Luc Boudenne

Keyword(s):

Surface Water ◽

Simultaneous Determination ◽

Surface Waters ◽

Water Samples ◽

High Performance ◽

Chemical Properties ◽

Environmental Water ◽

Butyl Ether ◽

Flight Mass Spectrometry

Chromatographic development for the determination of pharmaceuticals in environmental water samples is particularly challenging when the analytes have significantly different physico-chemical properties (solubility, polarity, pKa) often requiring multiple chromatographic methods for each active component. This paper presents a method for the simultaneous determination of azithromycin, erythromycin (antibiotics), fluoxetine (anti-depressant) and sotalol (b-blocker) in surface waters by ultra-high-performance liquid chromatography coupled with ultra-high-resolution time-of-flight mass spectrometry. These pharmaceuticals—presenting a broad spectrum of polarity (0.24 ≤ log Kow ≤ 4.05)—were separated on a C-18 analytical column, after a simple filtration step for freshwater samples or after a liquid–liquid extraction with Methyl-tertio-butyl ether (MTBE) for seawater samples. The optimized separation method (in terms of nature of column and eluent, elution gradient, and of mass spectrometric parameters), enable one to reach limits of detection ranging between 2 and 7 ng L−1 and limits of quantification between 7 and 23 ng L−1 for the four targeted molecules, within a three minute run. This method was validated using samples collected from three different surface waters in Lebanon (freshwater and seawater) and analytical results were compared with those obtained in surface waters sampled in a French river, equivalent in terms of human activities. Using this method, we report the highest concentration of pharmaceuticals found in surface water (up to 377 ng L−1 and 268 ng L−1, respectively, for azithromycin and erythromycin, in the Litani river, Lebanon).

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Optimum HPLC Conditions for Determination of Dibucaine HCL, Fluocortolone Pivalate and Fluocortolone Caproate by Using Experimental Design

Current Pharmaceutical Analysis ◽

10.2174/1573412913666170707113025 ◽

2018 ◽

Vol 15 (1) ◽

pp. 32-38 ◽

Cited By ~ 1

Author(s):

Bürge Aşçı ◽

Mesut Koç

Keyword(s):

Experimental Design ◽

Flow Rate ◽

Mobile Phase ◽

High Performance ◽

Limit Of Detection ◽

Pharmaceutical Preparations ◽

Acid Mixture ◽

Solution Stability ◽

Uv Detector

Introduction:This paper presents the development and validation of a novel, fast, sensitive and accurate high performance liquid chromatography (HPLC) method for the simultaneous quantitative determination of dibucaine HCl, fluocortolone pivalate and fluocortolone caproate in pharmaceutical preparations.Experiment:Development of the chromatographic method was based on an experimental design approach. A five-level-three-factor central composite design requiring 20 experiments in this optimization study was performed in order to evaluate the effects of three independent variances including mobile phase ratio, flow rate and amount of acid in the mobile phase.Conclusion:The optimum composition for mobile phase was found as a methanol:water:acetic acid mixture at 71.6 : 26.4 : 2 (v/v/v) ratio and optimum separation was acquired by isocratic elution with a flow rate of 1.3 mL/min. The analytes were detected using a UV detector at 240 nm. The developed method was validated in terms of linearity, precision, accuracy, limit of detection/quantitation and solution stability and successfully applied to the determination of dibucaine HCl, fluocortolone pivalate and fluocortolone caproate in pharmaceutical topical formulations such as suppositories and ointments.

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Determination of antibiotic resistance genes in a WWTP-impacted river in surface water, sediment, and biofilm: Influence of seasonality and water quality

The Science of The Total Environment ◽

10.1016/j.scitotenv.2020.144526 ◽

2021 ◽

pp. 144526

Author(s):

Gabriela Reichert ◽

Stephan Hilgert ◽

Johannes Alexander ◽

Júlio César Rodrigues de Azevedo ◽

Tobias Morck ◽

...

Keyword(s):

Water Quality ◽

Antibiotic Resistance ◽

Surface Water ◽

Resistance Genes ◽

Antibiotic Resistance Genes

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Determination of amino acids in human biological fluids by high-performance liquid chromatography: critical review

Amino Acids ◽

10.1007/s00726-021-03002-x ◽

2021 ◽

Author(s):

Grażyna Gałęzowska ◽

Joanna Ratajczyk ◽

Lidia Wolska

Keyword(s):

Amino Acids ◽

Amino Acid ◽

High Performance ◽

Hplc Analysis ◽

Limit Of Detection ◽

Biological Fluids ◽

Analytical Techniques ◽

Epidemiological Studies ◽

Preparation Conditions

AbstractThe quantitation and qualification of amino acids are most commonly used in clinical and epidemiological studies, and provide an excellent way of monitoring compounds in human fluids which have not been monitored previously, to prevent some diseases. Because of this, it is not surprising that scientific interest in evaluating these compounds has resurfaced in recent years and has precipitated the development of a multitude of new analytical techniques. This review considers recent developments in HPLC analytics on the basis of publications from the last few years. It helps to update and systematize knowledge in this area. Particular attention is paid to the progress of analytical methods, pointing out the advantages and drawbacks of the various techniques used for the preparation, separation and determination of amino acids. Depending on the type of sample, the preparation conditions for HPLC analysis change. For this reason, the review has focused on three types of samples, namely urine, blood and cerebrospinal fluid. Despite time-consuming sample preparation before HPLC analysis, an additional derivatization technique should be used, depending on the detection technique used. There are proposals for columns that are specially modified for amino acid separation without derivatization, but the limit of detection of the substance is less beneficial. In view of the fact that amino acid analyses have been performed for years and new solutions may generate increased costs, it may turn out that older proposals are much more advantageous.

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DETERMINATION OF 10-GINGEROL IN INDIAN GINGER BY VALIDATED HPTLC METHOD OF SAMPLES COLLECTED ACROSS SUBCONTINENT OF INDIA

International Journal of Pharmacy and Pharmaceutical Sciences ◽

10.22159/ijpps.2016v8i12.14953 ◽

2016 ◽

Vol 8 (12) ◽

pp. 190

Author(s):

Kamran Ashraf ◽

Syed Adnan Ali Shah ◽

Mohd Mujeeb

Keyword(s):

Thin Layer ◽

Thin Layer Chromatography ◽

High Performance ◽

Limit Of Detection ◽

Limit Of Quantification ◽

Chromatography Method ◽

Aluminum Plates ◽

Layer Chromatography ◽

Hptlc Method

Objective: A simple, sensitive, precise, and accurate stability indicating HPTLC (high-performance thin-layer chromatography) method for analysis of 10-gingerol in ginger has been developed and validated as perICH guidelines.Methods: The separation was achieved on TLC (thin layer chromatography) aluminum plates pre-coated with silica gel 60F254 using n-hexane: ethyl acetate 55:45 (%, v/v) as a mobile phase. Densitometric analysis was performed at 569 nm.Results: This system was found to have a compact spot of 10-gingerol at RF value of 0.57±0.03. For the proposed procedure, linearity (r2 = 0.998±0.02), limit of detection (18ng/spot), limit of quantification (42 ng/spot), recovery (ranging from 98.35%–100.68%), were found to be satisfactory.Conclusion: Statistical analysis reveals that the content of 10-gingerol in different geographical region varied significantly. The highest and lowest concentration of 10-gingerol in ginger was found to be present in a sample of Patna, Lucknow and Surat respectively which inferred that the variety of ginger found in Patna, Lucknow are much superior to other regions of India.

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Some indicators of water quality of the Tamis river

Chemical Industry and Chemical Engineering Quarterly ◽

10.2298/ciceq100712060b ◽

2011 ◽

Vol 17 (1) ◽

pp. 107-115 ◽

Cited By ~ 3

Author(s):

Nada Babovic ◽

Dejan Markovic ◽

Vojkan Dimitrijevic ◽

Dragan Markovic

Keyword(s):

Water Quality ◽

Ph Value ◽

Ammonium Nitrogen ◽

Field Analysis ◽

Total Hardness ◽

Chemical Parameters ◽

Physico Chemical

This paper shows the results obtained in field analysis performed at the Tamis River, starting from the settlement Jasa Tomic - border between Serbia and Romania to Pancevo - confluence of Tamis into the Danube. The Tamis is a 359 km long river rising in the southern Carpathian Mountains. It flows through the Banat region and flows into the Danube near Pancevo. During the years the water quality of the river has severely deteriorated and badly affected the environment and the river ecosystem. In situ measurements enabled determination of physico-chemical parameters of water quality of the Tamis River on every 400 m of the watercourse, such as: water temperature, pH value, electrical conductivity, contents of dissolved oxygen and oxygen saturation. The main reason of higher pollution of Tamis is seen in connection to DTD hydro system. Sampling was performed at 7 points with regard to color, turbidity, total hardness, alkalinity, concentration of ammonium nitrogen, nitrite nitrogen, nitrate nitrogen, iron, chlorides and sulphates in samples. The aim of the present work was to evaluate water quality in the Tamis River taking into account significant pollution, which originates from settlements, industry and agriculture, and to suggest appropriate preventive measures to further pollution decreasing of the river's water.

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Determination of Potential Genotoxic Impurity, 5-Amino-2-Chloropyridine, in Active Pharmaceutical Ingredient Using the HPLC-UV System

Journal of Chromatographic Science ◽

10.1093/chromsci/bmaa100 ◽

2020 ◽

Author(s):

Murat Soyseven ◽

Rüstem Keçili ◽

Hassan Y Aboul-Enein ◽

Göksel Arli

Keyword(s):

Analytical Method ◽

High Performance ◽

Orthophosphoric Acid ◽

Limit Of Detection ◽

Detection System ◽

Active Pharmaceutical Ingredient ◽

Limit Of Quantification ◽

Column Temperature ◽

Water Ph

Abstract A novel analytical method, based on high-performance liquid chromatography with a UV (HPLC-UV) detection system for the sensitive detection of a genotoxic impurity (GTI) 5-amino-2-chloropyridine (5A2Cl) in a model active pharmaceutical ingredient (API) tenoxicam (TNX), has been developed and validated. The HPLC-UV method was used for the determination of GTI 5A2Cl in API TNX. The compounds were separated using a mobile phase composed of water (pH 3 adjusted with orthophosphoric acid): MeOH, (50:50: v/v) on a C18 column (150 × 4.6 mm i.d., 2.7 μm) at a flow rate of 0.7 mL min−1. Detection was carried out in the 254 nm wavelength. Column temperature was maintained at 40°C during the analyses and 10 μL volume was injected into the HPLC-UV system. The method was validated in the range of 1–40 μg mL−1. The obtained calibration curves for the GTI compound was found linear with equation, y = 40766x − 1125,6 (R2 = 0.999). The developed analytical method toward the target compounds was accurate, and the achieved limit of detection and limit of quantification values for the target compound 5A2Cl were 0.015 and 0.048 μg mL−1, respectively. The recovery values were calculated and found to be between 98.80 and 100.03%. The developed RP-HPLC-UV analytical method in this research is accurate, precise, rapid, simple and appropriate for the sensitive analysis of target GTI 5A2Cl in model API TNX.

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Determination of tigecycline in turkey plasma by LC-MS/MS: validation and application in a pharmacokinetic study

Polish Journal of Veterinary Sciences ◽

10.1515/pjvs-2017-0029 ◽

2017 ◽

Vol 20 (2) ◽

pp. 241-249 ◽

Cited By ~ 2

Author(s):

A. Jasiecka-Mikołajczyk ◽

J.J. Jaroszewski

Keyword(s):

Pharmacokinetic Study ◽

High Performance ◽

Limit Of Detection ◽

Internal Standard ◽

Reversed Phase ◽

Selected Reaction Monitoring ◽

Limit Of Quantification ◽

Complicated Skin ◽

Intravenous And Oral Administration

Abstract Tigecycline (TIG), a novel glycylcycline antibiotic, plays an important role in the management of complicated skin and intra-abdominal infections. The available data lack any description of a method for determination of TIG in avian plasma. In our study, a selective, accurate and reversed-phase high performance liquid chromatography-tandem mass spectrometry method was developed for the determination of TIG in turkey plasma. Sample preparation was based on protein precipitation and liquid-liquid extraction using 1,2-dichloroethane. Chromatographic separation of TIG and minocycline (internal standard, IS) was achieved on an Atlantis T3 column (150 mm × 3.0 mm, 3.0 μm) using gradient elution. The selected reaction monitoring transitions were performed at 293.60 m/z → 257.10 m/z for TIG and 458.00 m/z → 441.20 m/z for IS. The developed method was validated in terms of specificity, selectivity, linearity, lowest limit of quantification, limit of detection, precision, accuracy, matrix effect, carry-over effect, extraction recovery and stability. All parameters of the method submitted to validation met the acceptance criteria. The assay was linear over the concentration range of 0.01-100 μg/ml. This validated method was successfully applied to a TIG pharmacokinetic study in turkey after intravenous and oral administration at a dose of 10 mg/kg at various time-points.

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SENSITIVE DETERMINATION OF RELATED SUBSTANCES IN PIOGLITAZONE HYDROCHLORIDE BY HPLC

International Journal of Applied Pharmaceutics ◽

10.22159/ijap.2017v9i2.16828 ◽

2017 ◽

Vol 9 (2) ◽

pp. 34

Author(s):

N. Balaji ◽

Sayeeda Sultana

Keyword(s):

Mobile Phase ◽

High Performance ◽

Limit Of Detection ◽

High Performance Liquid Chromatographic ◽

Hplc Method ◽

Internal Diameter ◽

Related Substances ◽

Relative Standard ◽

Limit Of Quantitation

Objective: An efficient, high performance liquid chromatographic method has been developed and validated for the quantification of related substances in pioglitazone hydrochloride drug substance.Methods: This method includes the determination of three related substances in pioglitazone hydrochloride. The mobile phase A is 0.1% w/v triethylamine in water with pH 2.5 adjusted by dilute phosphoric acid. The mobile phase B is premixed and degassed mixtures of acetonitrile and methanol. The flow rate was 1 ml/min. The elution used was gradient mode. The HPLC column used for the analysis was symmetry C18 with a length of 250 mm, the internal diameter of 4.6 mm and particle size of 5.0 microns.Results: The developed method was found to be linear with the range of 0.006-250% with a coefficient of correlation 0.99. The precision study revealed that the percentage relative standard deviation was within the acceptable limit. The limit of detection and limit of quantitation of the impurities was less than 0.002%and 0.006% with respect to pioglitazone hydrochloride test concentration of 2000 µg/ml respectively. This method has been validated as per ICH guidelines Q2 (R1).Conclusion: A reliable, economical HPLC method was magnificently established for quantitative analysis of related substances of pioglitazone hydrochloride drug substance.

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Development and validation of reversed phase high performance liquid chromatography (RP-HPLC) for quantification of captopril in rabbit plasma

Acta Chromatographica ◽

10.1556/1326.2020.00816 ◽

2020 ◽

Author(s):

Muhammad Fawad Rasool ◽

Umbreen Fatima Qureshi ◽

Nazar Muhammad Ranjha ◽

Imran Imran ◽

Mouqadus Un Nisa ◽

...

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

Mobile Phase ◽

High Performance ◽

Limit Of Detection ◽

Reversed Phase ◽

Rabbit Plasma ◽

Rp Hplc ◽

Relative Standard

AbstractTh accurate rapid, simple and selective reversed phase high performance liquid chromatography (RP-HPLC) has been established and validated for the determination of captopril (CAP). Chromatographic separation was accomplished using prepacked ODSI C18 column (250 mm × 4.6 mm with 5 μm particle size) in isocratic mode, with mobile phase consisting of water: acetonitrile (60:40 v/v), pH adjusted to 2.5 by using 85% orthophosphoric acid at a flow rate of 1 mL/min and UV detection was performed at 203 nm. RP-HPLC method used for the analysis of CAP in mobile phase and rabbit plasma was established and validated as per ICH-guidelines. It was carried out on a well-defined chromatographic peak of CAP was established with a retention time of 4.9 min and tailing factor of 1.871. The liquid–liquid extraction method was used for extraction of CAP from the plasma. Excellent linearity (R2 = 0.999) was shown over range 3.125–100 µg/mL with mean percentage recoveries ranges from 97 to 100.6%. Parameters of precision and accuracy of the developed method meet the established criteria. Intra and inter-day precision (% relative standard deviation) study was also performed which was less than 2% which indicate good reproducibility of the method. The limit of detection (LOD) and quantification for the CAP in plasma were 3.10 and 9.13 ng/mL respectively. The method was suitably validated and successfully applied to the determination of CAP in rabbit plasma samples.

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