scholarly journals Development of the High Sensitivity and Selectivity Method for the Determination of Histamine in Fish and Fish Sauce from Vietnam by UPLC-MS/MS

2020 ◽  
Vol 2020 ◽  
pp. 1-9
Author(s):  
Quang Hieu Tran ◽  
Thanh Tan Nguyen ◽  
Kim Phuong Pham
Keyword(s):  
Limit Of Detection ◽  
High Sensitivity ◽  
Fish Sauce ◽  
Limit Of Quantification ◽  
Fish Samples ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Sensitivity And Selectivity ◽  
Liquid Chromatographic

A selective, sensitive, and rapid method by using ultraperformance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for the determination of histamine in fish and fish sauce was developed. The optimal conditions of liquid chromatographic separation and mass spectroscopy of histamine have also been investigated. The linear ranges of the method were 20.0 ÷ 1000 ng/mL, and the corresponding correlation coefficient was 0.9993. Mean recoveries of the analyte at three spike levels (low, medium, and high) were within the range of 98.5% ÷ 102.5% (n = 7). The limit of detection (LOD) and limit of quantification (LOQ) values were 3.83 and 11.50 ng/mL for the fish sauce sample and 4.71 and 14.12 ng/mL for the fish sample, respectively. The influence of the matrix effect on the accuracy, repeatability, and recovery of the method was negligible. The recommended method was applied to determine the content of this substance in 21 fish sauce samples and 4 kinds of fish samples, which were collected from Ho Chi Minh City, Vietnam, in 2019.

scholarly journals Determination of 77 Multiclass Pesticides and Their Metabolitesin Capsicum and Tomato Using GC-MS/MS and LC-MS/MS

Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 1837
Author(s):  
Harischandra Naik Rathod ◽  
Bheemanna Mallappa ◽  
Pallavi Malenahalli Sidramappa ◽  
Chandra Sekhara Reddy Vennapusa ◽  
Pavankumar Kamin ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Solid Phase ◽  
Graphitized Carbon Black ◽  
Limit Of Quantification ◽  
Gas And Liquid Chromatography ◽  
Relative Standard ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Primary Secondary Amine

A quick, sensitive, and reproducible analytical method for the determination of 77 multiclass pesticides and their metabolites in Capsicum and tomato by gas and liquid chromatography tandem mass spectrometry was standardized and validated. The limit of detection of 0.19 to 10.91 and limit of quantification of 0.63 to 36.34 µg·kg−1 for Capsicum and 0.10 to 9.55 µg·kg−1 (LOD) and 0.35 to 33.43 µg·kg−1 (LOQ) for tomato. The method involves extraction of sample with acetonitrile, purification by dispersive solid phase extraction using primary secondary amine and graphitized carbon black. The recoveries of all pesticides were in the range of 75 to 110% with a relative standard deviation of less than 20%. Similarly, the method precision was evaluated interms of repeatability (RSDr) and reproducibility (RSDwR) by spiking of mixed pesticides standards at 100 µg·kg−1 recorded anRSD of less than 20%. The matrix effect was acceptable and no significant variation was observed in both the matrices except for few pesticides. The estimated measurement uncertainty found acceptable for all the pesticides. This method found suitable for analysis of vegetable samples drawn from market and farm gates.

scholarly journals Optimization of Method for Pesticide Detection in Honey by Using Liquid and Gas Chromatography Coupled with Mass Spectrometric Detection

Foods ◽  
2020 ◽  
Vol 9 (10) ◽  
pp. 1368
Author(s):  
Mariana O. Almeida ◽  
Silvia Catarina S. Oloris ◽  
Vanessa Heloisa F. Faria ◽  
Márcia Cassimira M. Ribeiro ◽  
Daniel M. Cantini ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Limit Of Detection ◽  
High Sensitivity ◽  
Mass Spectrometric ◽  
Mass Spectrometric Detection ◽  
Tandem Mass ◽  
Limit Of Quantification ◽  
Liquid Chromatography Tandem Mass ◽  
Tandem Mass Spectrometric ◽  
Liquid Chromatographic

This study aimed to optimize and validate a multi-residue method for identifying and quantifying pesticides in honey by using both gas and liquid chromatographic separation followed by mass spectrometric detection. The proposed method was validated to detect 168 compounds, 127 of them by LC-MS/MS (liquid chromatography tandem mass spectrometric detection) and 41 by GC-MS/MS (gas chromatography tandem mass spectrometric detection). The limit of detection (LOD) and limit of quantification (LOQ) values for the analytes determined by LC-MS/MS were 0.0001–0.0004 mg/kg and 0.0002–0.0008 mg/kg, respectively. For GC-MS/MS analyses, the LOD and LOQ values were 0.001–0.004 mg/kg and 0.002–0.008 mg/kg. In total, 33 samples of commercial honey produced by apiaries in six Brazilian states were analyzed with the validated method. Residual amounts of 15 analytes were detected in 31 samples (93.9%). The method described in the present study was able to detect an extensive and broad range of pesticides with very high sensitivity.

scholarly journals Liquid Chromatographic Method for the Analysis of Brimonidine in Ophthalmic Formulations

2012 ◽  
Vol 9 (3) ◽  
pp. 1327-1331 ◽  
Author(s):  
A. Narendra ◽  
D. Deepika ◽  
M. Mathrusri Annapurna
Keyword(s):  
Limit Of Detection ◽  
Detector Response ◽  
Eye Drops ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Acid Sodium Salt ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

A reverse phase LC method was developed for the determination of Brimonidine in eye drops. Chromatography was carried on an Inertsil ODS 3V column (C18) using a mixture of Octane 1- sulfonic acid sodium salt (0.02M) (pH 3.5 ± 0.05) and acetonitrile (64:36 v/v) as mobile phase at a flow rate of 1 mL/min with UV detection at 254 nm. The drug was eluted at 4.636 min. The detector response was linear in the concentration range of 0.4–72 μg/mL. The limit of detection and limit of quantification were found to be 0.0561 and 0.1848 μg/mL respectively. The proposed method was validated as per the ICH guidelines and can be applied for the routine analysis of Brimonidine in eye drops.

scholarly journals Micellar Liquid Chromatographic Determination of Carbaryl and 1-Naphthol in Water, Soil, and Vegetables

2012 ◽  
Vol 2012 ◽  
pp. 1-7 ◽  
Author(s):  
Mei-Liang Chin-Chen ◽  
Maria Rambla-Alegre ◽  
Abhilasha Durgbanshi ◽  
Devasish Bose ◽  
Sandeep K. Mourya ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Cetylpyridinium Chloride ◽  
Sodium Dodecyl ◽  
Chromatographic Determination ◽  
Limit Of Quantification ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

A liquid chromatographic procedure has been developed for the determination of carbaryl, a phenyl-N-methylcarbamate, and its main metabolite 1-naphthol, using a C18 column (250’mm’ × ’4.6’mm) with a micellar mobile phase and fluorescence detection at maximum excitation/emission wavelengths of 225/333’nm, respectively. In the optimization step, surfactants sodium dodecyl sulphate (SDS), Brij-35 andN-cetylpyridinium chloride monohydrate, and organic solvents propanol, butanol, and pentanol were considered. The selected mobile phase was 0.15’M SDS-6% (v/v)-pentanol-0.01’M NaH2PO4buffered at pH 3. Validation studies, according to the ICH Tripartite Guideline, included linearity (r>0.999), limit of detection (5 and 18’ng mL-1, for carbaryl and 1-naphthol, resp.), and limit of quantification (15 and 50’ng mL-1, for carbaryl and 1-naphthol, resp.), with intra- and interday precisions below 1%, and robustness parameters below 3%. The results show that the procedure was adequate for the routine analysis of these two compounds in water, soil, and vegetables samples.

RAPID HIGH PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE DETERMINATION OF RALTEGRAVIR IN HUMAN SALIVA

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (09) ◽  
pp. 68-73
Author(s):  
K Vijaya Sri ◽  
M. Shiva Kumar ◽  
M. A. Madhuri ◽  
Suresha K. ◽  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Human Saliva ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Liquid Chromatography Method ◽  
Liquid Chromatographic

In this study, a high-performance liquid chromatographic method (HPLC) was developed, validated and applied for the determination of raltegravir in biological sample like saliva. Liquid- liquid extraction was performed for isolation of the drug and elimination of saliva interferences. Samples of saliva was extracted with 50µL of ortho phosphoric acid and 3ml of methanol was added and spiked with raltegravir. The chromatographic separation was performed on Agilent Eclipse C18 (100 mm × 4.6 mm, 3.5µm) column, by using 80:20 v/v acetonitrile: water as a mobile phase under isocratic conditions at a flow rate of 1.0 mL/min for UV detection at 240 nm. Retention time of raltegravir was found to be 1.030 min. Linearity was found to be in the range of 25-1000 ng/mL with regression equation y = 13864x + 40495 and correlation coefficient 0.999. The low % RSD value indicates the method is accurate and precise. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.76 and 2.28 ng/mL, respectively. It can be concluded that this validated HPLC method is easy, precise, accurate, sensitive and selective for determination of raltegravir in saliva.

scholarly journals New Method for Simultaneous Determination of Microcystins and Cylindrospermopsin in Vegetable Matrices by SPE-UPLC-MS/MS

Toxins ◽  
2018 ◽  
Vol 10 (10) ◽  
pp. 406 ◽  
Author(s):  
Leticia Díez-Quijada ◽  
Remedios Guzmán-Guillén ◽  
Ana Prieto Ortega ◽  
María Llana-Ruíz-Cabello ◽  
Alexandre Campos ◽  
...  
Keyword(s):  
Chemical Structure ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Simultaneous Detection ◽  
Ultra Performance Liquid Chromatography ◽  
Limit Of Quantification ◽  
Worldwide Distribution ◽  
Exposure Estimation ◽  
Liquid Chromatography Tandem Mass

Cyanotoxins are a large group of noxious metabolites with different chemical structure and mechanisms of action, with a worldwide distribution, producing effects in animals, humans, and crop plants. When cyanotoxin-contaminated waters are used for the irrigation of edible vegetables, humans can be in contact with these toxins through the food chain. In this work, a method for the simultaneous detection of Microcystin-LR (MC-LR), Microcystin-RR (MC-RR), Microcystin-YR (MC-YR), and Cylindrospermopsin (CYN) in lettuce has been optimized and validated, using a dual solid phase extraction (SPE) system for toxin extraction and ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for analysis. Results showed linear ranges (5–50 ng g−1 f.w.), low values for limit of detection (LOD) (0.06–0.42 ng g−1 f.w.), and limit of quantification (LOQ) (0.16–0.91 ng g−1 f.w.), acceptable recoveries (41–93%), and %RSDIP values for the four toxins. The method proved to be robust for the three variables tested. Finally, it was successfully applied to detect these cyanotoxins in edible vegetables exposed to cyanobacterial extracts under laboratory conditions, and it could be useful for monitoring these toxins in edible vegetables for better exposure estimation in terms of risk assessment.

scholarly journals High performance liquid chromatographic method for the determination of guaifenesin in pharmaceutical syrups and in environmental samples

2013 ◽  
Vol 10 (3) ◽  
pp. 1014-1022
Author(s):  
Baghdad Science Journal
Keyword(s):  
High Performance ◽  
Chromatographic Method ◽  
Limit Of Detection ◽  
Industrial Effluent ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Limit Of Quantification ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

A simple, precise, rapid, and accurate reversed – phase high performance liquid chromatographic method has been developed for the determination of guaifenesin in pure from pharmaceutical formulations.andindustrial effluent. Chromatography was carried out on supelco L7 reversed- phase column (25cm × 4.6mm), 5 microns, using a mixture of methanol –acetonitrile-water: (80: 10 :10 v/v/v) as a mobile phase at a flow rate of 1.0 ml.min-1. Detection was performed at 254nm at ambient temperature. The retention time for guaifenesin was found 2.4 minutes. The calibration curve was linear (r= 0.9998) over a concentration range from 0.08 to 0.8mg/ml. Limit of detection (LOD) and limit of quantification ( LOQ) were found 6µg/ml and 18µg/ml respectively. The method was validated for its linearity, precision and accuracy .The proposed method was successfully applied for the determination of guaifenesin in syrups and industrial effluent samples.

scholarly journals Schiff-Based Fluorescent-ON Sensor L Synthesis and Its Application for Selective Determination of Cerium in Aqueous Media

2020 ◽  
Vol 2020 ◽  
pp. 1-10
Author(s):  
Maria Sadia ◽  
Jehangir Khan ◽  
Robina Naz ◽  
Muhammad Zahoor ◽  
Ezzat Khan ◽  
...  
Keyword(s):  
Metal Ion ◽  
Limit Of Detection ◽  
Fluorescent Sensor ◽  
Aqueous Media ◽  
High Sensitivity ◽  
Transition Metal Ions ◽  
Acetonitrile Solution ◽  
Selective Determination ◽  
Sensitivity And Selectivity

In the present study, a fluorescent sensor L for sensing of Ce3+ ion was designed and characterized by XRD, 1HNMR, and FTIR. Its fluorescence behavior towards metal ion was examined by fluorescence spectroscopy. Chelation-enhanced fluorescence was shown by the sensor L upon interaction with Ce3+ ion. This fluorescent sensor exhibits high sensitivity and selectivity towards Ce3+ ion in acetonitrile solution, forming 2 : 1 (L : M) complex as determined by Job’s plot. Association constant was found to be 1×107 M−1 estimated from the Benesi-Hildebrand plot. No significant interference was observed in the presence of other studied alkali, alkaline, and transition metal ions. A rapid response was observed when employed for the determination of Ce3+ ion in spiked water samples with a limit of detection equal to 3.4×10−8 M.

scholarly journals Potentiometric Signal Transduction for Selective Determination of 1-(3-Chlorophenyl)piperazine “Legal Ecstasy” Through Biomimetic Interaction Mechanism

Chemosensors ◽  
2019 ◽  
Vol 7 (3) ◽  
pp. 46
Author(s):  
Eman El-Naby
Keyword(s):  
Dynamic Range ◽  
Limit Of Detection ◽  
Interaction Mechanism ◽  
High Sensitivity ◽  
Fast Response ◽  
Polymeric Membrane ◽  
Selective Determination ◽  
Sensitivity And Selectivity ◽  
Pharmacologically Active

1-(3-chlorophenyl)piperazine (mCPP) is a wide spread new psychoactive substance produces stimulant and hallucinogenic effects similar to those sought from ecstasy. Hence, in the recent years, mCPP has been introduced by the organized crime through the darknet as a part of the illicit ecstasy market with a variable complex profile of pharmacologically active substances that pose problematic risk patterns among people who take these seized products. Accordingly, the design of selective sensors for the determination of mCPP is a very important demand. In this respect, a supramolecular architecture; [Na(15-crown-5)][BPh4] from the assembly of 15-crown-5 and sodium tetraphenylboron has been utilized as an ionophore, for the first time in the selective recognition of mCPP in conjunction with potassium tetrakis(p-chlorophenyl)borate and dioctylphthalate through polymeric membrane ion sensors. The ionophore exhibited a strong binding affinity that resulted in a high sensitivity with a slope closed to the ideal Nernstian value; 58.9 ± 0.43 mV/decade, a larger dynamic range from 10−6 to 10−2 M, a lower limit of detection down to 5.0 × 10−7 M and a fast response time of 5 s. Very important also is it was afforded excellent selectivity towards mCPP over psychoactive substances of major concern, providing a potentially useful system for the determination of mCPP in the illicit market. On comparison with the natural β-cyclodextrin as an ionophore, it exhibited more sensitivity and selectivity estimated to be the superior.

Determination of ethyl glucuronide and ethyl sulfate in human whole blood and vitreous humor by LC-MS/MS and applications to the interpretation of postmortem ethanol findings

2020 ◽  
Author(s):  
Hao Wang ◽  
Beixu Li ◽  
Fanglin Wang ◽  
Jing Chang ◽  
Yunfeng Zhang ◽  
...  
Keyword(s):  
Whole Blood ◽  
High Sensitivity ◽  
Vitreous Humor ◽  
Ethyl Glucuronide ◽  
Ethyl Sulfate ◽  
Human Whole Blood ◽  
Ethanol Formation ◽  
Liquid Chromatography Tandem Mass ◽  
Sensitivity And Selectivity

Abstract Identifying the source of ethanol in a decedent remained a complicated problem for forensic toxicologists because of postmortem ethanol formation. As ethanol’s non-oxidative metabolites, ethyl glucuronide (EtG) and ethyl sulfate (EtS) have the potential to distinguish between antemortem ethanol consumption and postmortem ethanol formation, due to their high sensitivity and selectivity. In the current study, a simple and quick liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed for the determination of EtG and EtS in human whole blood and vitreous humor (VH). A total of 20 μL of the sample was precipitated by methanol, and the analytes were detected by LC-MS/MS in a run of 6 min. This method achieved high sensitivity (limits of detection: 2 ng/mL for both EtG and EtS), with linearity in the range of 5–10,000 ng/mL in both whole blood and VH. Deviations in accuracy, inter- and intra-day precision were all lower than 15% at three quality control levels. Subsequently, this method was applied to 62 real forensic cases. Only blood samples were available in 52 cases. Paired blood and VH samples were present in 10 cases. The concentrations of EtG and EtS in blood were in the range of 0–22,264.8 ng/mL and 0–2,126.0 ng/mL, respectively. In one case with both blood and VH, the blood ethanol concentration was 1.22 mg/mL, with EtG and EtS both below limits of quantification (5 ng/mL) in VH, and no EtG and EtS found in whole blood. The results suggested that EtG and EtS were useful markers for the interpretation of ethanol resource in postmortem blood and VH.

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