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Audrey Roy-Lachapelle
Aquatic Contaminants Research Division, Environment and Climate Change Canada, 105 McGill, Montréal, Québec, H2Y 2E7, Canada

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Journal article
Published: 23 October 2020 in Talanta
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Anabaenopeptins (APs) are bioactive cyanopeptides of emerging concern produced by cyanobacteria. The research for analytical development has recently gained in importance due to their abundance in toxic cyanobacterial blooms. A new commercial enzyme-linked immunosorbent assay kit for the determination of total APs (APtot ELISA) has been released promising a rapid response with good cost efficiency for the routine monitoring of uncommon cyanopeptides. The present study explores the suitability of this new kit in comparison with a validated quantitative analytical method based on liquid chromatography coupled to mass spectrometry (LC-MS). The validation results were comparable with both methods for accuracy, precision, and calibration. Method detection limits were more sensitive using LC-MS specifically evaluated at 0.011 and 0.013 μg L−1 for AP-A and B respectively, compared to APtot ELISA evaluated at 0.10 μg L−1 for total of the two. For APtot ELISA, results were independent from the matrix; however, a systematic signal response was measured in blanks, requiring a blank subtraction in data treatment. Cross-reactivity of APtot ELISA was investigated by analyzing ten cyanopeptides selected for their abundance and diversity. Cyanopeptolin A (CP-A), nodularin-R (NOD), microcystin (MC)-RR, [Asp3]RR, and HilR showed cross-reactivity with an average overestimation going from 25 to 66%. Considering the contribution of cross-reactive cyanopeptides, thirteen lake samples out of fifteen showed higher concentrations using APtot ELISA with overestimation values up to 2261% compared to LC-MS. In light of this study results, LC-MS should still be preconized for the study and monitoring of APs when sensitivity and specificity are needed.

ACS Style

Audrey Roy-Lachapelle; Morgan Solliec; Sébastien Sauvé; Christian Gagnon. Evaluation of ELISA-based method for total anabaenopeptins determination and comparative analysis with on-line SPE-UHPLC-HRMS in freshwater cyanobacterial blooms. Talanta 2020, 223, 121802 .

AMA Style

Audrey Roy-Lachapelle, Morgan Solliec, Sébastien Sauvé, Christian Gagnon. Evaluation of ELISA-based method for total anabaenopeptins determination and comparative analysis with on-line SPE-UHPLC-HRMS in freshwater cyanobacterial blooms. Talanta. 2020; 223 ():121802.

Chicago/Turabian Style

Audrey Roy-Lachapelle; Morgan Solliec; Sébastien Sauvé; Christian Gagnon. 2020. "Evaluation of ELISA-based method for total anabaenopeptins determination and comparative analysis with on-line SPE-UHPLC-HRMS in freshwater cyanobacterial blooms." Talanta 223, no. : 121802.

Journal article
Published: 26 October 2019 in Toxins
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Toxin-producing cyanobacteria are responsible for the presence of hundreds of bioactive compounds in aquatic environments undergoing increasing eutrophication. The identification of cyanotoxins is still emerging, due to the great diversity of potential congeners, yet high-resolution mass spectrometry (HRMS) has the potential to deepen this knowledge in aquatic environments. In this study, high-throughput and sensitive on-line solid-phase extraction ultra-high performance liquid chromatography (SPE-UHPLC) coupled to HRMS was applied to a data-independent acquisition (DIA) workflow for the suspect screening of cyanopeptides, including microcystin and anabaenopeptin toxin classes. The unambiguous characterization of 11 uncommon cyanopeptides was possible using a characterization workflow through extensive analysis of fragmentation patterns. This method also allowed the characterization of four unknown cyanotoxins ([Leu1, Ser7] MC-HtyR, [Asp3]MC-RHar, AP731, and AP803). The quantification of 17 common cyanotoxins along with the semi-quantification of the characterized uncommon cyanopeptides resulted with the identification of 23 different cyanotoxins in 12 lakes in Canada, United Kingdom and France. The concentrations of the compounds varied between 39 and 41,000 ng L−1. To our knowledge, this is the first DIA method applied for the suspect screening of two families of cyanopeptides simultaneously. Moreover, this study shows the great diversity of cyanotoxins in lake water cyanobacterial blooms, a growing concern in aquatic systems.

ACS Style

Audrey Roy-Lachapelle; Morgan Solliec; Sébastien Sauvé; Christian Gagnon. A Data-Independent Methodology for the Structural Characterization of Microcystins and Anabaenopeptins Leading to the Identification of Four New Congeners. Toxins 2019, 11, 619 .

AMA Style

Audrey Roy-Lachapelle, Morgan Solliec, Sébastien Sauvé, Christian Gagnon. A Data-Independent Methodology for the Structural Characterization of Microcystins and Anabaenopeptins Leading to the Identification of Four New Congeners. Toxins. 2019; 11 (11):619.

Chicago/Turabian Style

Audrey Roy-Lachapelle; Morgan Solliec; Sébastien Sauvé; Christian Gagnon. 2019. "A Data-Independent Methodology for the Structural Characterization of Microcystins and Anabaenopeptins Leading to the Identification of Four New Congeners." Toxins 11, no. 11: 619.

Journal article
Published: 01 September 2017 in Journal of Chromatography A
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A fast and high-throughput method is proposed for the determination of total microcystins (ΣMC) in environmental surface waters. After a 1-h Lemieux-von Rudloff oxidation step to yield the 2-methyl-3-methoxy-4-phenylbutyric acid (MMPB) moiety, samples were quenched, filtered, and directly analyzed. This was achieved via solid phase extraction (SPE) coupled on-line to ultra-high performance liquid chromatography electrospray ionization triple stage quadrupole mass spectrometry. The choice of on-line SPE settings was conducted using experimental designs. Given the matrix complexity of oxidation extracts, the on-line desalting step was found to be a critical parameter to ensure suitable method robustness. The on-line sample loading volume was 5mL, and the wash volume applied for on-line desalting was 3mL. Instrumental analysis was performed in just 8min. The method limit of quantification was 0.5ngL ΣMC (i.e. 2000 times lower than the current World Health Organization - WHO drinking water guideline). Excellent determination coefficients were observed for matrix-free and matrix-based calibration curves alike, and the linearity range tested spanned∼4 orders of magnitude. Accuracy and intermediate precision did not depend on the spike level and proved satisfactory (in the range of 93-110% and 3-6%, respectively). A thorough assessment of instrumental matrix effects was conducted by comparing standard additions curves in several lake and river oxidation extracts with the matrix-free reference. Regardless of the internal standard used (4-PB or D3-MMPB), instrumental matrix effects were efficiently compensated. The matrix effect that may occur at the earlier sample preparation stage was evaluated separately. While the oxidation step was generally not complete (yield ∼65%), the conversion rates of MCs into MMPB remained within a consistent range of values regardless of matrix type. No significant back-pressure was observed upon consecutive injections of oxidation-based samples, while the instrumental sensitivity remained unaffected. The herein described method could therefore be eligible for future large-scale monitoring surveys. The method was applied to a selection of surface water samples (n=30) collected across the province of Québec, Canada, and the results were compared to those achieved by an individual variant analysis of 8 MC congeners and a commercial ELISA kit.

ACS Style

Gabriel Munoz; Sung Vo Duy; Audrey Roy-Lachapelle; Barry Husk; Sébastien Sauvé. Analysis of individual and total microcystins in surface water by on-line preconcentration and desalting coupled to liquid chromatography tandem mass spectrometry. Journal of Chromatography A 2017, 1516, 9 -20.

AMA Style

Gabriel Munoz, Sung Vo Duy, Audrey Roy-Lachapelle, Barry Husk, Sébastien Sauvé. Analysis of individual and total microcystins in surface water by on-line preconcentration and desalting coupled to liquid chromatography tandem mass spectrometry. Journal of Chromatography A. 2017; 1516 ():9-20.

Chicago/Turabian Style

Gabriel Munoz; Sung Vo Duy; Audrey Roy-Lachapelle; Barry Husk; Sébastien Sauvé. 2017. "Analysis of individual and total microcystins in surface water by on-line preconcentration and desalting coupled to liquid chromatography tandem mass spectrometry." Journal of Chromatography A 1516, no. : 9-20.

Journal article
Published: 25 February 2017 in Toxins
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Algae dietary supplements are marketed worldwide as natural health products. Although their proprieties have been claimed as beneficial to improve overall health, there have been several previous reports of contamination by cyanotoxins. These products generally contain non-toxic cyanobacteria, but the methods of cultivation in natural waters without appropriate quality controls allow contamination by toxin producer species present in the natural environment. In this study, we investigated the presence of total microcystins, seven individual microcystins (RR, YR, LR, LA, LY, LW, LF), anatoxin-a, dihydroanatoxin-a, epoxyanatoxin-a, cylindrospermopsin, saxitoxin, and β-methylamino-l-alanine in 18 different commercially available products containing Spirulina or Aphanizomenon flos-aquae. Total microcystins analysis was accomplished using a Lemieux oxidation and a chemical derivatization using dansyl chloride was needed for the simultaneous analysis of cylindrospermopsin, saxitoxin, and β-methylamino-l-alanine. Moreover, the use of laser diode thermal desorption (LDTD) and ultra-high performance liquid chromatography (UHPLC) both coupled to high resolution mass spectrometry (HRMS) enabled high performance detection and quantitation. Out of the 18 products analyzed, 8 contained some cyanotoxins at levels exceeding the tolerable daily intake values. The presence of cyanotoxins in these algal dietary supplements reinforces the need for a better quality control as well as consumer’s awareness on the potential risks associated with the consumption of these supplements.

ACS Style

Audrey Roy-Lachapelle; Morgan Solliec; Maryse F. Bouchard; Sébastien Sauvé. Detection of Cyanotoxins in Algae Dietary Supplements. Toxins 2017, 9, 76 .

AMA Style

Audrey Roy-Lachapelle, Morgan Solliec, Maryse F. Bouchard, Sébastien Sauvé. Detection of Cyanotoxins in Algae Dietary Supplements. Toxins. 2017; 9 (3):76.

Chicago/Turabian Style

Audrey Roy-Lachapelle; Morgan Solliec; Maryse F. Bouchard; Sébastien Sauvé. 2017. "Detection of Cyanotoxins in Algae Dietary Supplements." Toxins 9, no. 3: 76.

Journal article
Published: 01 February 2016 in Science of The Total Environment
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The fate of antimicrobial active compound residues in the environment, and especially antibiotics used in swine husbandry are of particular interest for their potential toxicity and contribution to antibiotic resistance. The presence of relatively high concentrations of bioactive compounds has been reported in agricultural areas but few information is available on their degradation products. Veterinary antibiotics reach terrestrial environments through many routes, including application of swine manure to soils. The objectives of this project were first, to develop an analytical method able to quantify and identify veterinary antibiotics and their degradation products in manure, soil and water samples; and second, to study the distribution of these target compounds in soils and drainage waters. A brief evaluation of their potential toxicity in the environment was also made. In order to achieve these objectives, liquid chromatography coupled to high-resolution mass spectrometry was used for its ability to quantify contaminants with sensitivity and selectivity, and its capacity to identify degradation products. Samples of manure, soil and water came from a long-term experimental site where swine manure containing veterinary antibiotics has been applied for many years. In this study, tetracycline antibiotics were found at several hundred μg L− 1 in the swine manure slurry used for fertilization, several hundred of ng L− 1 in drainage waters and several ng g− 1 in soils, while degradation products were sometimes found at concentrations higher than the parent compounds.

ACS Style

Morgan Solliec; Audrey Roy-Lachapelle; Marc-Olivier Gasser; Caroline Coté; Mylène Généreux; Sébastien Sauvé. Fractionation and analysis of veterinary antibiotics and their related degradation products in agricultural soils and drainage waters following swine manure amendment. Science of The Total Environment 2016, 543, 524 -535.

AMA Style

Morgan Solliec, Audrey Roy-Lachapelle, Marc-Olivier Gasser, Caroline Coté, Mylène Généreux, Sébastien Sauvé. Fractionation and analysis of veterinary antibiotics and their related degradation products in agricultural soils and drainage waters following swine manure amendment. Science of The Total Environment. 2016; 543 ():524-535.

Chicago/Turabian Style

Morgan Solliec; Audrey Roy-Lachapelle; Marc-Olivier Gasser; Caroline Coté; Mylène Généreux; Sébastien Sauvé. 2016. "Fractionation and analysis of veterinary antibiotics and their related degradation products in agricultural soils and drainage waters following swine manure amendment." Science of The Total Environment 543, no. : 524-535.

Journal article
Published: 01 December 2015 in Toxicon
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An analytical method based on on-line SPE-LC-HESI-MS/MS has been developed for the detection and quantification of eight selected cyanotoxins in algal bloom waters that include mycrocystins, anatoxin-a and cylindrospermopsin. The injection volume was 2 mL according to the expected concentration of cyanotoxins in matrix. The method provides an analysis time of 7 min per sample, acceptable recovery values (91–101%), good precision (RSD < 13%) and method limits of detection at the sub-microgram per liter levels (0.01–0.02 μg L−1). A detailed discussion on optimization parameters that have an impact on the overall performance of the method are presented. In particular, method optimization permitted the chromatographic separation of anatoxin-a and phenylalanine, an isobaric interference with a similar chromatographic characteristics. All optimization and validation experiments for the on-line SPE method and chromatographic separation were performed in environmentally relevant algal bloom water matrices. The applicability of the method was tested on several algal bloom water samples from monitored lakes across the province of Québec (Québec, Canada) known to produce cyanotoxins. All of the targeted cyanotoxins were detected with the exception of cylindrospermopsin. In addition, it was found that total microcystin concentrations in several surface water samples exceeded the proposed guidelines established by the province of Québec in Canada of 1.5 μg L−1 as well as the World Health Organization of 1 μg L−1 for both free and cell-bound microcystin-LR equivalent.

ACS Style

Paul B. Fayad; Audrey Roy-Lachapelle; Sung Vo Duy; Michèle Prévost; Sébastien Sauvé. On-line solid-phase extraction coupled to liquid chromatography tandem mass spectrometry for the analysis of cyanotoxins in algal blooms. Toxicon 2015, 108, 167 -175.

AMA Style

Paul B. Fayad, Audrey Roy-Lachapelle, Sung Vo Duy, Michèle Prévost, Sébastien Sauvé. On-line solid-phase extraction coupled to liquid chromatography tandem mass spectrometry for the analysis of cyanotoxins in algal blooms. Toxicon. 2015; 108 ():167-175.

Chicago/Turabian Style

Paul B. Fayad; Audrey Roy-Lachapelle; Sung Vo Duy; Michèle Prévost; Sébastien Sauvé. 2015. "On-line solid-phase extraction coupled to liquid chromatography tandem mass spectrometry for the analysis of cyanotoxins in algal blooms." Toxicon 108, no. : 167-175.

Research article
Published: 10 November 2015 in Rapid Communications in Mass Spectrometry
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Rationale Swine manure can contain a wide range of veterinary antibiotics, which could enter the environment via manure spreading on agricultural fields. A suspect and non‐target screening method was applied to swine manure samples to attempt to identify veterinary antibiotics and pharmaceutical compounds for a future targeted analysis method. Methods A combination of suspect and non‐target screening method was developed to identify various veterinary antibiotic families using liquid chromatography coupled with high‐resolution mass spectrometry (LC/HRMS). The sample preparation was based on the physicochemical parameters of antibiotics for the wide scope extraction of polar compounds prior to LC/HRMS analysis. The amount of data produced was processed by applying restrictive thresholds and filters to significantly reduce the number of compounds found and eliminate matrix components. Results The suspect and non‐target screening was applied on swine manure samples and revealed the presence of seven common veterinary antibiotics and some of their relative metabolites, including tetracyclines, β‐lactams, sulfonamides and lincosamides. However, one steroid and one analgesic were also identified. The occurrence of the identified compounds was validated by comparing their retention times, isotopic abundance patterns and fragmentation patterns with certified standards. Conclusions This identification method could be very useful as an initial step to screen for and identify emerging contaminants such as veterinary antibiotics and pharmaceuticals in environmental and biological matrices prior to quantification. Copyright © 2015 John Wiley & Sons, Ltd.

ACS Style

Morgan Solliec; Audrey Roy-Lachapelle; Sébastien Sauvé. Development of a suspect and non-target screening approach to detect veterinary antibiotic residues in a complex biological matrix using liquid chromatography/high-resolution mass spectrometry. Rapid Communications in Mass Spectrometry 2015, 29, 2361 -2373.

AMA Style

Morgan Solliec, Audrey Roy-Lachapelle, Sébastien Sauvé. Development of a suspect and non-target screening approach to detect veterinary antibiotic residues in a complex biological matrix using liquid chromatography/high-resolution mass spectrometry. Rapid Communications in Mass Spectrometry. 2015; 29 (24):2361-2373.

Chicago/Turabian Style

Morgan Solliec; Audrey Roy-Lachapelle; Sébastien Sauvé. 2015. "Development of a suspect and non-target screening approach to detect veterinary antibiotic residues in a complex biological matrix using liquid chromatography/high-resolution mass spectrometry." Rapid Communications in Mass Spectrometry 29, no. 24: 2361-2373.

Research article
Published: 12 August 2015 in Journal of Agricultural and Food Chemistry
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Microcystins (MCs) are cyanobacterial toxins encountered in aquatic environments worldwide. Over 100 MC variants have been identified and have the capacity to covalently bind to animal tissue. This study presents a new approach for cell-bound and free microcystin analysis in fish tissue using sodium hydroxide as a digestion agent and Lemieux oxidation to obtain the 2-methyl-3-methoxy-4-phenylbutyric acid (MMPB) moiety, common to all microcystin congeners. The use of laser diode thermal desorption-atmospheric pressure chemical ionization coupled with Q-Exactive mass spectrometry (LDTD-APCI-HRMS) led to an analysis time of approximately 10 s per sample and high-resolution detection. Digestion/oxidation and solid phase extraction recoveries ranged from 70 to 75% and from 86 to 103%, respectively. Method detection and quantification limits values were 2.7 and 8.2 μg kg(-1), respectively. Fish samples from cyanobacteria-contaminated lakes were analyzed, and concentrations ranging from 2.9 to 13.2 μg kg(-1) were reported.

ACS Style

Audrey Roy-Lachapelle; Morgan Solliec; Marc Sinotte; Christian Deblois; Sébastien Sauvé. Total Analysis of Microcystins in Fish Tissue Using Laser Thermal Desorption–Atmospheric Pressure Chemical Ionization–High-Resolution Mass Spectrometry (LDTD-APCI-HRMS). Journal of Agricultural and Food Chemistry 2015, 63, 7440 -7449.

AMA Style

Audrey Roy-Lachapelle, Morgan Solliec, Marc Sinotte, Christian Deblois, Sébastien Sauvé. Total Analysis of Microcystins in Fish Tissue Using Laser Thermal Desorption–Atmospheric Pressure Chemical Ionization–High-Resolution Mass Spectrometry (LDTD-APCI-HRMS). Journal of Agricultural and Food Chemistry. 2015; 63 (33):7440-7449.

Chicago/Turabian Style

Audrey Roy-Lachapelle; Morgan Solliec; Marc Sinotte; Christian Deblois; Sébastien Sauvé. 2015. "Total Analysis of Microcystins in Fish Tissue Using Laser Thermal Desorption–Atmospheric Pressure Chemical Ionization–High-Resolution Mass Spectrometry (LDTD-APCI-HRMS)." Journal of Agricultural and Food Chemistry 63, no. 33: 7440-7449.

Validation study
Published: 03 May 2015 in Analytical and Bioanalytical Chemistry
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A new analytical method was developed for the detection of alkaloid cyanotoxins in harmful algal blooms. The detection of the nonproteinogenic amino acid β-N-methylamino-L-alanine (BMAA) and two of its conformation isomers, 2,4-diaminobutyric acid (DAB) and N-(2-aminoethyl) glycine (AEG), as well as three alkaloid cyanotoxins, anatoxin-a (ANA-a), cylindrospermopsin (CYN), and saxitoxin (STX), is presented. The use of a chemical derivatization with dansyl chloride (DNS) allows easier separation with reversed phase liquid chromatography. Detection with high-resolution mass spectrometry (HRMS) with the Q-Exactive enables high selectivity with specific fragmentation as well as exact mass detection, reducing considerably the possibilities of isobaric interferences. Previous to analysis, a solid phase extraction (SPE) step is used for purification and preconcentration. After DNS derivatization, samples are submitted to ultra high-performance liquid chromatography coupled with heated electrospray ionisation and the Q-Exactive mass spectrometer (UHPLC-HESI-HRMS). With an internal calibration using isotopically-labeled DAB-D3, the method was validated with good linearity (R (2) > 0.998), and method limits of detection and quantification (MLD and MLQ) for target compounds ranged from 0.007 to 0.01 μg L(-1) and from 0.02 to 0.04 μg L(-1), respectively. Accuracy and within-day/between-days variation coefficients were below 15%. SPE recovery values ranged between 86 and 103%, and matrix effects recovery values ranged between 75 and 96%. The developed analytical method was successfully validated with 12 different lakes samples, and concentrations were found ranging between 0.009 and 0.3 μg L(-1) except for STX which was not found in any sample.

ACS Style

Audrey Roy-Lachapelle; Morgan Solliec; Sébastien Sauvé. Determination of BMAA and three alkaloid cyanotoxins in lake water using dansyl chloride derivatization and high-resolution mass spectrometry. Analytical and Bioanalytical Chemistry 2015, 407, 5487 -5501.

AMA Style

Audrey Roy-Lachapelle, Morgan Solliec, Sébastien Sauvé. Determination of BMAA and three alkaloid cyanotoxins in lake water using dansyl chloride derivatization and high-resolution mass spectrometry. Analytical and Bioanalytical Chemistry. 2015; 407 (18):5487-5501.

Chicago/Turabian Style

Audrey Roy-Lachapelle; Morgan Solliec; Sébastien Sauvé. 2015. "Determination of BMAA and three alkaloid cyanotoxins in lake water using dansyl chloride derivatization and high-resolution mass spectrometry." Analytical and Bioanalytical Chemistry 407, no. 18: 5487-5501.

Journal article
Published: 01 January 2015 in Talanta
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A new innovative analytical method combining ultra-fast analysis time with high resolution/accurate mass detection was developed to eliminate the misidentification of anatoxin-a (ANA-a), a cyanobacterial toxin, from the natural amino acid phenylalanine (PHE). This was achieved by using the laser diode thermal desorption-atmospheric pressure chemical ionization (LDTD-APCI) coupled to the Q-Exactive, a high resolution/accurate mass spectrometer (HRMS). This novel combination, the LDTD-APCI-HRMS, allowed for an ultra-fast analysis time (0.999). Enhancement of signal to noise ratios relative to a standard triple-quadrupole method was demonstrated with lower detection and quantification limit values of 0.2 and 0.6 μg/L using the Q-Exactive. Accuracy and interday/intraday relative standard deviations were below 15%. The new method was applied to 8 different lake water samples with signs of cyanobacterial blooms. This work demonstrates the possibility of using an ultra-fast LDTD-APCI sample introduction system with an HRMS hybrid instrument for quantitative purposes with high selectivity in complex environmental matrices.

ACS Style

Audrey Roy-Lachapelle; Morgan Solliec; Marc Sinotte; Christian Deblois; Sébastien Sauvé. High resolution/accurate mass (HRMS) detection of anatoxin-a in lake water using LDTD–APCI coupled to a Q-Exactive mass spectrometer. Talanta 2015, 132, 836 -844.

AMA Style

Audrey Roy-Lachapelle, Morgan Solliec, Marc Sinotte, Christian Deblois, Sébastien Sauvé. High resolution/accurate mass (HRMS) detection of anatoxin-a in lake water using LDTD–APCI coupled to a Q-Exactive mass spectrometer. Talanta. 2015; 132 ():836-844.

Chicago/Turabian Style

Audrey Roy-Lachapelle; Morgan Solliec; Marc Sinotte; Christian Deblois; Sébastien Sauvé. 2015. "High resolution/accurate mass (HRMS) detection of anatoxin-a in lake water using LDTD–APCI coupled to a Q-Exactive mass spectrometer." Talanta 132, no. : 836-844.

Journal article
Published: 01 January 2015 in Analytica Chimica Acta
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The presence of antibiotics in the environment is of increased interest and, as modern mass spectrometers become more efficient, we are increasingly aware of traces of pharmaceuticals appearing in a wide range of environmental and biological matrices. The Q-Exactive mass spectrometer is part of these innovative hybrid high-resolution mass spectrometers (HRMS) which is often associated with peptide sequencing or metabolomics but with a limited number of studies focusing on its application to the quantification of small molecules in environmental and biological matrices. It combines the high resolving power (RP) performance of the Orbitrap with the high performance selectivity of the quadrupole. Tetracyclines (TCs) are a family comprising some of the most widely used antibiotics in veterinary medicine. This study presents the quantitative performances of the Q-Exactive by illustrating a new approach to quantify TCs using liquid chromatography coupled to a HRMS in a complex matrix, i.e., swine manure. The Q-Exactive was used at high-resolution in both full scan (FS) and targeted ion fragmentation (tMS(2)) modes. These two modes were optimized and compared to determine the most reliable and efficient approach to quantify TCs with good accuracy. The proposed method was optimized to obtain the best selectivity and sensitivity, thus eliminating false positive and allowing the detection of trace levels of analyte. The TCs were extracted from the matrix by sonication using McIlvaine buffer followed by an off-line solid phase extraction method to concentrate and clean the extracts. Both FS and tMS(2) modes presented good linearity (R(2)>0.991) and repeatability (RSD<15%). Mass accuracy was acceptable with values below 2 ppm. The method detection limits (MLD) calculated from the calibration curves ranged from 2.0 to 12 ng g(-1) for FS mode and from 1.5 to 3.6 ng g(-1) for tMS(2) mode. Accuracy and interday/intraday relative standard deviations were below 21% for both modes studied. TCs were quantified in real samples of swine manure with concentrations ranging from 29 to 75 ng g(-1). This study showed the possibility of using hybrid HRMS for trace detection and quantification of TCs in a complex matrix, thus avoiding false positive while achieving good selectivity and sensitivity.

ACS Style

Morgan Solliec; Audrey Roy-Lachapelle; Sébastien Sauvé. Quantitative performance of liquid chromatography coupled to Q-Exactive high resolution mass spectrometry (HRMS) for the analysis of tetracyclines in a complex matrix. Analytica Chimica Acta 2015, 853, 415 -424.

AMA Style

Morgan Solliec, Audrey Roy-Lachapelle, Sébastien Sauvé. Quantitative performance of liquid chromatography coupled to Q-Exactive high resolution mass spectrometry (HRMS) for the analysis of tetracyclines in a complex matrix. Analytica Chimica Acta. 2015; 853 ():415-424.

Chicago/Turabian Style

Morgan Solliec; Audrey Roy-Lachapelle; Sébastien Sauvé. 2015. "Quantitative performance of liquid chromatography coupled to Q-Exactive high resolution mass spectrometry (HRMS) for the analysis of tetracyclines in a complex matrix." Analytica Chimica Acta 853, no. : 415-424.

Journal article
Published: 01 April 2014 in Analytica Chimica Acta
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A new approach for the analysis of the cyanobacterial microcystins (MCs) in environmental water matrices has been developed. It offers a cost efficient alternative method for the fast quantification of total MCs using mass spectrometry. This approach permits the quantification of total MCs concentrations without requiring any derivatization or the use of a suite of MCs standards. The oxidation product 2-methyl-3-methoxy-4-phenylbutyric acid (MMPB) was formed through a Lemieux oxidation and represented the total concentration of free and bound MCs in water samples. MMPB was analyzed using laser diode thermal desorption-atmospheric pressure chemical ionization coupled to tandem mass spectrometry (LDTD-APCI-MS/MS). LDTD is a robust and reliable sample introduction method with ultra-fast analysis time (0.999). Limits of detection and quantification were 0.2 and 0.9 μg L(-1), respectively. These values are comparable with the WHO (World Health Organization) guideline of 1 μg L(-1) for total microcystin-LR congener in drinking water. Accuracy and interday/intraday variation coefficients were below 15%. Matrix effect was determined with a recovery of 91%, showing no significant signal suppression. This work demonstrates the use of the LDTD-APCI-MS/MS interface for the screening, detection and quantification of total MCs in complex environmental matrices.

ACS Style

Audrey Roy-Lachapelle; Paul B. Fayad; Marc Sinotte; Christian Deblois; Sébastien Sauvé. Total microcystins analysis in water using laser diode thermal desorption-atmospheric pressure chemical ionization-tandem mass spectrometry. Analytica Chimica Acta 2014, 820, 76 -83.

AMA Style

Audrey Roy-Lachapelle, Paul B. Fayad, Marc Sinotte, Christian Deblois, Sébastien Sauvé. Total microcystins analysis in water using laser diode thermal desorption-atmospheric pressure chemical ionization-tandem mass spectrometry. Analytica Chimica Acta. 2014; 820 ():76-83.

Chicago/Turabian Style

Audrey Roy-Lachapelle; Paul B. Fayad; Marc Sinotte; Christian Deblois; Sébastien Sauvé. 2014. "Total microcystins analysis in water using laser diode thermal desorption-atmospheric pressure chemical ionization-tandem mass spectrometry." Analytica Chimica Acta 820, no. : 76-83.

Journal article
Published: 01 January 2013 in Toxicon
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A novel approach for the analysis of the cyanobacterial toxin, anatoxin-a (ANA-a), in an environmentally relevant matrix, using laser diode thermal desorption-atmospheric pressure chemical ionization-tandem mass spectrometry (LDTD-APCI-MS/MS) is presented. The ultra-fast analysis time (15 s/sample) provided by the LDTD-APCI interface is strengthened by its ability to remove interference from phenylalanine (PHE), an isobaric interference in ANA-a analysis by MS/MS. Thus the LDTD-APCI interface avoids the time consuming steps of derivatization, chromatographic separation or solid-phase extraction prior to analysis. Method development and instrumental parameter optimizations were focused toward signal enhancement of ANA-a, and signal removal of a PHE interference as high as 500 μg/L. External calibration in a complex matrix gave detection and quantification limit values of 1 and 3 μg/L respectively, as well as good linearity (R(2) > 0.999) over nearly two orders of magnitude. Internal calibration with clomiphene (CLO) is possible and method performance was similar to that obtained by external calibration. This work demonstrated the utility of the LDTD-APCI source for ultra-fast detection and quantification of ANA-a in environmental aqueous matrices, and confirmed its ability to suppress the interference of PHE without sample preparation or chromatographic separation.

ACS Style

Pascal Lemoine; Audrey Roy-Lachapelle; Michèle Prévost; Patrice Tremblay; Morgan Solliec; Sébastien Sauvé. Ultra-fast analysis of anatoxin-A using laser diode thermal desorption-atmospheric pressure chemical ionization-tandem mass spectrometry: Validation and resolution from phenylalanine. Toxicon 2013, 61, 165 -174.

AMA Style

Pascal Lemoine, Audrey Roy-Lachapelle, Michèle Prévost, Patrice Tremblay, Morgan Solliec, Sébastien Sauvé. Ultra-fast analysis of anatoxin-A using laser diode thermal desorption-atmospheric pressure chemical ionization-tandem mass spectrometry: Validation and resolution from phenylalanine. Toxicon. 2013; 61 ():165-174.

Chicago/Turabian Style

Pascal Lemoine; Audrey Roy-Lachapelle; Michèle Prévost; Patrice Tremblay; Morgan Solliec; Sébastien Sauvé. 2013. "Ultra-fast analysis of anatoxin-A using laser diode thermal desorption-atmospheric pressure chemical ionization-tandem mass spectrometry: Validation and resolution from phenylalanine." Toxicon 61, no. : 165-174.