scholarly journals LC–MS/MS Analysis of the Emerging Toxin Pinnatoxin-G and High Levels of Esterified OA Group Toxins in Galician Commercial Mussels

Toxins ◽  
2019 ◽  
Vol 11 (7) ◽  
pp. 394 ◽  
Author(s):  
Paz Otero ◽  
Natalia Miguéns ◽  
Inés Rodríguez ◽  
Luis M. Botana
Keyword(s):  
Potential Risk ◽  
Mytilus Galloprovincialis ◽  
Safety Monitoring ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Standard Calibration ◽  
Commercially Important ◽  
First Time

The occurrence of marine harmful algae is increasing worldwide and, therefore, the accumulation of lipophilic marine toxins from harmful phytoplankton represents a food safety threat in the shellfish industry. Galicia, which is a commercially important EU producer of edible bivalve mollusk have been subjected to recurring cases of mussel farm closures, in the last decades. This work aimed to study the toxic profile of commercial mussels (Mytilus galloprovincialis) in order to establish a potential risk when ingested. For this, a total of 41 samples of mussels farmed in 3 Rías (Ares-Sada, Arousa, and Pontevedra) and purchased in 5 local markets were analyzed by liquid chromatography tandem mass spectrometry (LC–MS/MS). Chromatograms showed the presence of okadaic acid (OA), dinophysistoxin-2 (DTX-2), pectenotoxin-2 (PTX-2), azaspiracid-2 (AZA-2), and the emerging toxins 13-desmethyl spirolide C (SPX-13), and pinnatoxin-G (PnTX-G). Quantification of each toxin was determined using their own standard calibration in the range 0.1%–50 ng/mL (R2 > 0.99) and by considering the toxin recovery (62–110%) and the matrix correction (33–211%). Data showed that OA and DTX-2 (especially in the form of esters) are the main risk in Galician mollusks, which was detected in 38 samples (93%) and 3 of them exceeded the legal limit (160 µg/kg), followed by SPX-13 that was detected in 19 samples (46%) in quantities of up to 28.9 µg/kg. Analysis from PTX-2, AZA-2, and PnTX-G showed smaller amounts. Fifteen samples (37%) were positive for PTX-2 (0.7–2.9 µg/kg), 12 samples (29%) for AZA-2 (0.1–1.8 µg/kg), and PnTX-G was detected in 5 mussel samples (12%) (0.4 µg/kg–0.9 µg/kg). This is the first time Galician mollusk was contaminated with PnTX-G. Despite results indicating that this toxin was not a potential risk through the mussel ingestion, it should be considered in the shellfish safety monitoring programs through the LC–MS/MS methods.

scholarly journals UPLC-MS/MS Profile of Alkaloids with Cytotoxic Properties of Selected Medicinal Plants of the Berberidaceae and Papaveraceae Families

2017 ◽  
Vol 2017 ◽  
pp. 1-7 ◽  
Author(s):  
Anna Och ◽  
Katarzyna Szewczyk ◽  
Łukasz Pecio ◽  
Anna Stochmal ◽  
Daniel Załuski ◽  
...  
Keyword(s):  
Tandem Mass ◽  
Berberis Thunbergii ◽  
Chelidonium Majus ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Macleaya Cordata ◽  
Mahonia Aquifolium ◽  
Fumaria Officinalis ◽  
First Time ◽  
Dicentra Spectabilis

Cancer is one of the most occurring diseases in developed and developing countries. Plant-based compounds are still researched for their anticancer activity and for their quantity in plants. Therefore, the modern chromatographic methods are applied to quantify them in plants, for example, UPLC-MS/MS (ultraperformance liquid chromatography tandem mass spectrometry). Therefore, the aim of the present study was to evaluate the content of sanguinarine, berberine, protopine, and chelidonine in Dicentra spectabilis (L.) Lem., Fumaria officinalis L., Glaucium flavum Crantz, Corydalis cava L., Berberis thunbergii DC., Meconopsis cambrica (L.) Vig., Mahonia aquifolium (Pursh) Nutt., Macleaya cordata Willd., and Chelidonium majus L. For the first time, N,N-dimethyl-hernovine was identified in M. cambrica, B. thunbergii, M. aquifolium, C. cava, G. flavum, and C. majus; methyl-hernovine was identified in G. flavum; columbamine was identified in B. thunbergii; and methyl-corypalmine, chelidonine, and sanguinarine were identified in F. officinalis L. The richest source of protopine among all the examined species was M. cordata (5463.64 ± 26.3 μg/g). The highest amounts of chelidonine and sanguinarine were found in C. majus (51,040.0 ± 1.8 μg/g and 7925.8 ± 3.3 μg/g, resp.), while B. thunbergi contained the highest amount of berberine (6358.4 ± 4.2 μg/g).

scholarly journals First Detection of Tetrodotoxins in the Cotylean Flatworm Prosthiostomum trilineatum

Marine Drugs ◽  
2021 ◽  
Vol 19 (1) ◽  
pp. 40
Author(s):  
Rei Suo ◽  
Maho Kashitani ◽  
Hikaru Oyama ◽  
Masaatsu Adachi ◽  
Ryota Nakahigashi ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
High Performance ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
High Concentrations ◽  
First Time

Several polyclad flatworm species are known to contain high levels of tetrodotoxin (TTX), but currently TTX-bearing flatworms seem to be restricted to specific Planocera lineages belonging to the suborder Acotylea. During our ongoing study of flatworm toxins, high concentrations of TTXs were detected for the first time in the flatworm Prosthiostomum trilineatum, suborder Cotylea, from the coastal area of Hayama, Kanagawa, Japan. Toxin levels were investigated by high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS), revealing that this species contains comparable concentrations of toxins as seen in planocerid flatworms such as Planocera multitentaculata. This finding indicated that there may be other species with significant levels of TTXs. The distribution of TTXs among other flatworm species is thus of great interest.

scholarly journals Accurate Determination, Matrix Effect Estimation, and Uncertainty Evaluation of Three Sulfonamides in Milk by Isotope Dilution Liquid Chromatography-Tandem Mass Spectrometry

2021 ◽  
Vol 2021 ◽  
pp. 1-7
Author(s):  
Chaonan Han ◽  
Xiuqin Li ◽  
Hui Jiao ◽  
Yan Gao ◽  
Qinghe Zhang
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Matrix Effect ◽  
Mobile Phase ◽  
Accurate Determination ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass

Liquid chromatography-tandem mass spectrometry (LC-MS/MS) is the most commonly used method for sulfonamide determination. Its accuracy, however, can be affected by many factors. In this study, sulfadiazine (SDZ), sulfadimidine (SMZ), and sulfadimethoxine (SDM) in milk were selected to investigate an accurate determination method and the potential influencing factors in the use of ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Milk samples were extracted by 25 mL perchloric acid solution (pH = 2) and cleaned up using HLB solid-phase extraction (SPE) cartridges. Four kinds of filters, including PTFE, GHP, nylon, and glass fiber, were compared, and PTFE was selected since it had the best recoveries of target sulfonamides (SAs). Three quantitative methods, including external standard (ES), matrix matching (MM), and isotope dilution mass spectrometry (IDMS), were compared, among which IDMS exhibited the best accuracy. The matrix effect under different mobile phase compositions and of different sample matrices were evaluated and discussed. Ion suppression effects were observed during the determination of all SAs, which got stronger with the increase of the methanol composition percent in the mobile phase. After correction by IDMS, the matrix effect could be neglected. Matrix spiked recoveries at three spiked levels (1 μg/kg, 10 μg/kg, and 20 μg/kg) ranged from 96.8% to 103.8% by IDMS. The expanded relative uncertainties were in the range of 2.02% to 5.75%. The method exhibited wide application range, high accuracy, good stability, and high sensitivity.

A selective and robust UPLC-MS/MS method for the simultaneous quantitative determination of anlotinib, ceritinib and ibrutinib in rat plasma and its application to a pharmacokinetic study

The Analyst ◽  
2019 ◽  
Vol 144 (18) ◽  
pp. 5462-5471 ◽  
Author(s):  
Ping Du ◽  
Yin Guan ◽  
Zhuoling An ◽  
Pengfei Li ◽  
Lihong Liu
Keyword(s):  
Mass Spectrometry ◽  
Kinase Inhibitors ◽  
Rat Plasma ◽  
Tandem Mass ◽  
Spectrometry Method ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Ultrahigh Performance Liquid Chromatography ◽  
First Time

A selective, robust ultrahigh performance liquid chromatography tandem mass spectrometry method was developed for the first time for the simultaneous determination of next-generation antitumor tyrosine kinase inhibitors in rat plasma using protein precipitation extraction.

Detection of mephedrone and its metabolites in fingerprints from a controlled human administration study by liquid chromatography-tandem mass spectrometry and paper spray-mass spectrometry

The Analyst ◽  
2020 ◽  
Vol 145 (8) ◽  
pp. 3038-3048 ◽  
Author(s):  
Joanna Czerwinska ◽  
Min Jang ◽  
Catia Costa ◽  
Mark C. Parkin ◽  
Claire George ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Tandem Mass ◽  
Paper Spray ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
First Time

Mephedrone and one of its metabolites have been detected for the first-time in fingerprints collected from a controlled human mephedrone administration study.

scholarly journals Development and Validation of Liquid Chromatography-Tandem Mass Spectrometry Methods for the Quantification of Cefquinome, Ceftiofur, and Desfuroylceftiofuracetamide in Porcine Feces with Emphasis on Analyte Stability

Molecules ◽  
2021 ◽  
Vol 26 (15) ◽  
pp. 4598
Author(s):  
Sofie Rutjens ◽  
Siska Croubels ◽  
Siegrid De Baere ◽  
Mathias Devreese
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
The Impact ◽  
Porcine Feces

Cefquinome and ceftiofur are β-lactam antibiotics used for the treatment of bacterial infections in swine. Although these antimicrobials are administered intramuscularly, the exposure of the gut microbiota to these cephalosporins is not well described. This exposure can contribute to the emergence and spread of antimicrobials in the environment and to the possible spread of antimicrobial resistance genes. To assess the impact of drug administration on the intestinal excretion of these antimicrobials it is essential to measure the amounts of native compound and metabolites in feces. Two (ultra)-high-performance liquid chromatography-tandem mass spectrometry ((U)HPLC–MS/MS) methods were developed and validated, one for the determination of cefquinome and ceftiofur and the other for the determination of ceftiofur residues, measured as desfuroylceftiofuracetamide, in porcine feces. The matrix-based calibration curve was linear from 5 ng g−1 to 1000 ng g−1 for cefquinome (correlation coefficient (r) = 0.9990 ± 0.0007; goodness of fit (gof) = 3.70 ± 1.43) and ceftiofur (r = 0.9979 ± 0.0009; gof = 5.51 ± 1.14) and quadratic from 30 ng g−1 to 2000 ng g−1 for desfuroylceftiofuracetamide (r = 0.9960 ± 0.0020; gof = 7.31 ± 1.76). The within-day and between-day precision and accuracy fell within the specified ranges. Since β-lactam antibiotics are known to be unstable in feces, additional experiments were conducted to adjust the sampling protocol in order to minimize the impact of the matrix constituents on the stability of the analytes. Immediately after sampling, 500 µL of an 8 µg mL−1 tazobactam solution in water was added to 0.5 g feces, to reduce the degradation in matrix.

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