scholarly journals Screening of Danish traffic cases for synthetic cannabinoids in whole blood by LC-MS/MS

2013 ◽  
Vol 19 (2) ◽  
pp. 45-51 ◽  
Author(s):  
Niels Bjerre Holm ◽  
Rebeca Sequera Pineda ◽  
David Wederkinck Andersen ◽  
Brian Schou Rasmussen ◽  
Petur Weihe Dalsgaard ◽  
...  
Keyword(s):  
Whole Blood ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Synthetic Cannabinoids ◽  
Screening Method ◽  
Driving Under The Influence ◽  
Reaction Monitoring ◽  
Multiple Reaction Monitoring Mode ◽  
Target Screening

ABSTRACT A target screening method for the detection of 13 synthetic cannabinoids in whole blood was developed and validated. Samples underwent automated solid-phase extraction, and sample extracts were analyzed by liquid chromatography-positive electrospray ionization-tandem mass spectrometry using two transitions in multiple reaction monitoring mode. The limit of detection was between 0.1-2.5 ng/mL for the compounds except HU-210, and extraction recovery ranged from 59 to 78%. The method was used to screen 393 Danish traffic cases from 2012, where the driver was suspected of driving under the influence of drugs. No synthetic cannabinoids were identified in these samples. Additionally, the method was applied to a clinical intoxication case, and the synthetic cannabinoid AM- 2201 was identified in serum. We conclude that the prevalence of driving under the influence of synthetic cannabinoids in Denmark is likely to be low, and that synthetic cannabinoids are most likely to be encountered in the clinical setting.

scholarly journals A bioanalytical screening method for Enterococcus faecalis RNPP-type quorum sensing peptides in murine feces

Bioanalysis ◽  
2022 ◽  
Author(s):  
Frederick Verbeke ◽  
Nathan Debunne ◽  
Yorick Janssens ◽  
Bart De Spiegeleer ◽  
Evelien Wynendaele
Keyword(s):  
Quorum Sensing ◽  
Enterococcus Faecalis ◽  
High Performance ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Screening Method ◽  
Phase Extraction ◽  
Reaction Monitoring ◽  
Wild Type ◽  
Fit For Purpose

Background: Bacteria coordinate their behavior as a group via communication with their peers, known as ‘ quorum sensing’. Enterococcus faecalis employs quorum sensing via RNPP-peptides which were not yet reported to be present in mammalian biofluids. Results: Solid phase extraction of murine feces was performed, followed by ultra high performance liquid chromatography (UHPLC–MS/MS) in multiple reaction monitoring (MRM) mode (in total <90 min/sample) for the nine known RNPP peptides. Limits of detection ranged between 0.045 and 52 nM. Adequate identification criteria allowed detection of RNPP quorum sensing peptides in 2/20 wild-type murine feces samples (i.e., cAM373 and cOB1). Conclusion: A fit-for-purpose UHPLC–MS/MS method detected these RNPP peptides in wild-type murine feces samples.

scholarly journals Determination of Erythromycin and Tylosin Residues in Honey by LC/MS/MS

2009 ◽  
Vol 92 (3) ◽  
pp. 975-980 ◽  
Author(s):  
Rodrigo Granja ◽  
Alfredo Montes Nio ◽  
Roberto Zucchetti ◽  
Rosario Montes Nio ◽  
Raj Patel ◽  
...  
Keyword(s):  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Monitoring Program ◽  
Reaction Monitoring ◽  
Development Of Resistance ◽  
Drug Concentrations ◽  
Prevention And Treatment ◽  
Multiple Reaction Monitoring Mode ◽  
Detection Capabilities

Abstract Antibiotics are used in apiculture to protect bees against a variety of brood diseases. As a result of the development of resistance to oxytetracycline, erythromycin and tylosin are increasingly used for the prevention and treatment of these diseases. Therefore, Brazilian authorities have added these antibiotics to the National Regulatory Monitoring Program for the control of residues in honey. An analytical method has been developed for the determination of residues of erythromycin and tylosin in honey. The procedure involves solid-phase extraction of diluted honey samples with Bond Elut cartridges, followed by LC/MS with electrospray positive ionization in the multiple reaction monitoring mode. Two characteristic transitions were monitored for both drugs. Average analyte recoveries of erythromycin and tylosin ranged from 99 to 109 from sets of replicate honey samples fortified with drug concentrations of 5, 10, 15, and 20 g/kg. The method decision limits were determined to be 1.27 and 0.59 g/kg for erythromycin and tylosin, respectively. The detection capabilities were 5 and 5.2 g/kg for erythromycin and tylosin, respectively.

scholarly journals Simultaneous Determination of Some Phenothiazine Derivatives in Human Blood by Headspace Solid-Phase Microextraction and Gas Chromatography with Nitrogen-Phosphorus Detection

2008 ◽  
Vol 91 (6) ◽  
pp. 1354-1362 ◽  
Author(s):  
Natsuko Shinmen ◽  
Xiao-Pen Lee ◽  
Takeshi Kumazawa ◽  
Chika Hasegawa ◽  
Yasuhiro Ishiwata ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Whole Blood ◽  
Solid Phase Microextraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Regression Equations ◽  
Phenothiazine Derivatives ◽  
Headspace Solid Phase Microextraction ◽  
Coefficients Of Variation

Abstract Chlorpromazine, levomepromazine, promazine, triflupromazine, and trimeprazine were simultaneously determined in human whole blood and plasma by combining headspace solid-phase microextraction and gas chromatography with nitrogenphosphorus detection. Extraction efficiency for the phenothiazine derivatives was 0.0130.117 for both sample types. Regression equations were linear [correlation coefficient (r) 0.99510.9999] within the range 2.5200 ng/0.5 mL for triflupromazine and trimeprazine, and 6.3200 ng/0.5 mL for chlorpromazine, levomepromazine, and promazine. The limit of detection for each compound was 0.23.9 ng/0.5 mL whole blood and plasma. Intraday and interday coefficients of variation for all phenothiazines in both human samples were commonly &lt;15 and 20, respectively. We also report the determination of levomepromazine in human plasma after oral administration.

scholarly journals A Rapid and Selective LC-MS/MS Method for Quantification of Quetiapine in Human Plasma and its Application to Pharmacokinetic Study on Indian Schizophrenia Patients

2011 ◽  
Vol 8 (4) ◽  
pp. 1802-1814 ◽  
Author(s):  
S. Ravinder ◽  
A. T. Bapuji ◽  
K. Mukkanti ◽  
M. Nagesh ◽  
H. L. V. Ravikiran
Keyword(s):  
Mass Spectrometry ◽  
Human Plasma ◽  
Pharmacokinetic Study ◽  
Dynamic Range ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Plasma Samples ◽  
Standard Curve ◽  
Multiple Reaction Monitoring Mode

A rapid, robust and selective high pressure liquid chromatography–positive electrospray ionization tandem mass spectrometry method has been developed and validated for the quantification of quetiapine (QUE) in human plasma with K2EDTA using oxcarbazepine (IS) as an internal standard. Analyte and internal standard were extracted from human plasma by solid-phase extraction using acetonitrile. The eluted samples were chromatographed on a C18 column by using a 10:75:15v/v mixture of ammonium formate buffer (5 mM, pH 4.50) and acetonitrile and methanol as an isocratic mobile phase at a flow rate of 0.4 mL/min and analyzed by mass spectrometry in the multiple reaction monitoring mode using the respective [M+H]+ions,m/z384.3/253.2 for Quetiapine andm/z253.1/208.1 for the internal standard. The assay exhibited a linear dynamic range of 5.01 - 2501.04 ng/mL for quetiapine in human plasma. Acceptable precision and accuracy were obtained for concentrations over the standard curve range. A run time of 2.5 min for each sample made it possible to analyze 300 patient plasma samples per day. The validated method has been successfully used for the estimation of quetiapine in real time schizophrenia patient’s plasma samples for pharmacokinetic study.

scholarly journals Determination of Pharmaceutical Residues by UPLC-MS/MS Method: Validation and Application on Surface Water and Hospital Wastewater

2021 ◽  
Vol 2021 ◽  
pp. 1-12
Author(s):  
Bui Van Hoi ◽  
Cam-Tu Vu ◽  
Lan-Anh Phung-Thi ◽  
Thao Thi Nguyen ◽  
Phuong Thanh Nguyen ◽  
...  
Keyword(s):  
Surface Water ◽  
Analytical Method ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Hospital Wastewater ◽  
Esi Ms ◽  
Pharmaceutical Residues ◽  
Detection Frequency

In this study, an analytical method for the simultaneous determination of 7 major pharmaceutical residues in Vietnam, namely, carbamazepine, ciprofloxacin, ofloxacin, ketoprofen, paracetamol, sulfamethoxazole, and trimethoprim, in surface water and hospital wastewater has been developed. The method includes enrichment and clean-up steps by solid phase extraction using mix-mode cation exchange, followed by identification and quantification using an ultrahigh-performance liquid chromatography and tandem mass spectrometry and employing electrospray ionization (UPLC-ESI-MS/MS). Seven target compounds were separated on the reversed phase column and detected in multiple reaction monitoring (MRM) mode within 6 minutes. The present study also optimized the operating parameters of the mass spectrometer to achieve the highest analytical signals for all target compounds. All characteristic parameters of the analytical method were investigated, including linearity range, limit of detection, limit of quantification, precision, and accuracy. The important parameter in UPLC-ESI-MS/MS, matrix effect, was assessed and implemented via preextraction and postextraction spiking experiments. The overall recoveries of all target compounds were in the ranges from 55% to 109% and 56 % to 115% for surface water and hospital wastewater, respectively. Detection limits for surface water and hospital wastewater were 0.005–0.015 µg L−1 and 0.014–0.123 µg L−1, respectively. The sensitivity of the developed method was allowed for determination of target compounds at trace level in environmental water samples. The in-house validation of the developed method was performed by spiking experiment in both the surface water and hospital wastewater matrix. The method was then applied to analyze several surface water and hospital wastewater samples taken from West Lake and some hospitals in Vietnam, where the level of these pharmaceutical product residues was still missed. Sulfamethoxazole was present at a high detection frequency in both surface water (33% of analyzed samples) and hospital wastewater (81% of analyzed samples) samples.

scholarly journals Comparison of Liquid-Liquid Partition, HS-SPME and Static HS GC/MS Analysis for the Quantification of (–)-Linalool in Human Whole Blood Samples

2010 ◽  
Vol 5 (9) ◽  
pp. 1934578X1000500 ◽  
Author(s):  
Susanne Mirjam Friedl ◽  
Katharina Oedendorfer ◽  
Simone Kitzer ◽  
Gottfried Reznicek ◽  
Guenther Sladek ◽  
...  
Keyword(s):  
Whole Blood ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Internal Standard ◽  
Pharmacokinetic Studies ◽  
Pharmacokinetic Data ◽  
Blood Samples ◽  
Human Whole Blood ◽  
Quantitative Results ◽  
Incubation Temperatures

The aim of this investigation was to develop a fast and convenient method for the determination of (–)-linalool in human whole blood to facilitate pharmacokinetic studies. Analytical protocols were elaborated for three different GC/MS sampling techniques, i.e., static headspace ( S-HS), headspace solid phase micro extraction (HS-SPME), and liquid-liquid partition. In principle, all tested methods were feasible, but s-HS had the greatest benefit because of the easy handling of the blood samples and its short analysis time. For s-HS two different incubation temperatures were tested (40°C and 60°C). The limit of detection was slightly lower when samples were incubated at 60°C, but the same quantitative results were achieved using α–terpineol as internal standard. An accurate and sensitive method for the quantification of (–)-linalool in blood samples after either inhalation or percutaneous application, as well as pharmacokinetic data are presented.

A New Method Using Liquid Chromatography Tandem Mass Spectrometry to Detect NDMA in Water

2013 ◽  
Vol 742 ◽  
pp. 355-358
Author(s):  
Chao Jie Zhang ◽  
Geng Zhang ◽  
Lu Ting Chen ◽  
Qian Chen ◽  
Qi Zhou
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Tandem Mass ◽  
Reaction Monitoring ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Trace Concentrations

This study focused on using liquid Chromatography Tandem Mass Spectrometry to detect N-Nitrosodimethylamine (NDMA) at trace concentrations in water. The water sample was preconcentrated by solid-phase extraction method. To find an elution which can obtain higher recovery, three reagents with different organic solvents were examined. After comparing the recoveries and the standard deviation of the elution, finally the dichloromethane was determined as the elution of the experiment. Then the concentrated sample was analyzed by a method combining SPE pretreatment and LC separation with tandem mass spectrometry using multiple reaction monitoring (MRM).

Quantification and confirmation of four aflatoxins using a LC–MS/MS QTRAP system in multiple reaction monitoring, enhanced product ion scan, and MS3 modes

2019 ◽  
Vol 26 (1) ◽  
pp. 63-77
Author(s):  
Shencong Lv ◽  
Henghui Wang ◽  
Yong Yan ◽  
Miaohua Ge ◽  
Jian Guan
Keyword(s):  
Formic Acid ◽  
Ion Trap ◽  
Multiple Reaction Monitoring ◽  
Correlation Coefficients ◽  
Gradient Elution ◽  
Reaction Monitoring ◽  
Liquid Chromatography Tandem Mass ◽  
Multiple Reaction Monitoring Mode ◽  
Derivative Products

A simple, rapid, and efficient liquid chromatography tandem mass spectrometry (LC–MS/MS) method, operated in electrospray ionization and quadrupole linear ion trap modes, has been developed for the identification and structural characterization of aflatoxins in peanuts and its derivative products or bean sauce. Samples (5 g) were extracted with acetonitrile/water/formic acid (79:20:1, v/v). After centrifugation and dilution, the extracts were separated on a C18 analytical column by gradient elution (acetonitrile/0.2% formic acid) and analyzed by UPLC–MS/MS. External calibration was used for qualification. The developed multiple reaction monitoring–information-dependent acquisition–enhanced product ion method enabled quantification and confirmation of the analytes in a single run. Enhanced product ion mode was used for qualitative analysis, while multiple reaction monitoring mode was used for quantitative analysis. An in-house library was constructed for identification. Calibration curves showed good linearity with correlation coefficients (r) higher than 0.994. Limits of detection were determined to be below 0.26 µg kg−1 for most analytes. The recoveries for those substances were in the acceptable range of 80.2%–119.1%. A new LC–MS3 method was established for further confirmation. One pickled pepper peanut was found to contain aflatoxins B1, B2, and G1 with contents of 90.93, 26.64, and 1.92 µg kg−1, respectively.

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