Simultaneous analysis of multiple mycotoxins in Alpinia oxyphylla by UPLC-MS/MS

2017 ◽  
Vol 10 (1) ◽  
pp. 41-51 ◽  
Author(s):  
X.S. Zhao ◽  
W.J. Kong ◽  
S. Wang ◽  
J.H. Wei ◽  
M.H. Yang

In this study, a reliable and fast method for the simultaneous quantitation of 11 mycotoxins in Alpinia oxyphylla was developed using ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLCMS/ MS). Three different extraction procedures (solid-liquid extraction, solid-phase extraction and modified QuEChERS) were evaluated. Solid-liquid extraction was fast and easy, and also provided the best recovery rate for all mycotoxins, compared to the other extraction procedures. Some crucial factors, including extraction solvent, time and temperature, were carefully optimised. Significant matrix effects were offset using matrix-matched calibration. Under these optimised conditions, our detection approach showed a good, linear dynamic range with correlation coefficients (R2) above 0.9958. The limit of quantification ranged from 0.1 to 20 μg/kg. Accuracy was determined in a selected matrix using blank samples spiked with the target mycotoxins at three different concentration levels. The recoveries ranged from 60% (T-2 toxin) to 111% (HT-2 toxin), with relative standard deviation <20%. The validated method was used to analyse 44 batches of A. oxyphylla purchased from different regions of China. Aflatoxin B1, zearalenone, ochratoxin A, fumonisin B1 and fumonisin B2 were detected in 4 mouldy samples.

2020 ◽  
Vol 17 (3) ◽  
pp. 266
Author(s):  
Julia Martín ◽  
Juan Luis Santos ◽  
José Luis Malvar ◽  
Irene Aparicio ◽  
Esteban Alonso

Environmental contextFollowing stringent regulations, based on environmental health concerns, for controlling the production and usage of bisphenol A, several analogues have been developed as replacement chemicals. These analogues are now found in environmental samples at similar or even higher concentrations than bisphenol A. We report a sensitive and easy-to-perform analytical method for the determination of 11 bisphenols in vegetables. AbstractIn this work, a sensitive, selective, fast and easy-to-perform method has been developed, based on focussed ultrasound solid-liquid extraction (FUSLE) and dispersive solid-phase extraction (d-SPE), for the multiresidue determination of bisphenol A (BPA), its chlorinated derivatives (Clx-BPA) and six structural analogues (S, F, E, B, P, AF) in vegetables. Determination was carried out by gas chromatography–tandem mass spectrometry (GC–MS/MS). A Box–Behnken design was used to optimise the most significant variables. Recoveries in the range from 74 to 105%, precision (relative standard deviation) lower than 12% and limits of quantification in the range from 0.05 to 1ngg−1 d.w. (dry weight) were achieved. The method was successfully applied to the determination of the compounds in carrot, turnip and potato samples purchased from a local market. BPA and Cl-BPA were found in most of the analysed samples at concentrations up to 8.91ngg−1 d.w. The analytical and operational properties of the method make it appropriate to be applied in food monitoring programs.


2007 ◽  
Vol 106 (5) ◽  
pp. 2875-2884 ◽  
Author(s):  
Verónica Calderón ◽  
Felipe Serna ◽  
Félix García ◽  
José L. de la Peña ◽  
José M. García

2020 ◽  
Vol 18 (1) ◽  
pp. 314-324 ◽  
Author(s):  
Mahwash Mahar Gul ◽  
Khuram Shahzad Ahmad

AbstractDetoxification and management of environmental contaminants is an exigent issue of current times. Sulfonylurea herbicide, Bensulfuron-methyl was investigated for its degradation demeanour in soils, through biotic and abiotic modes (biodegradation and hydrolysis). Solid-liquid extraction of the herbicide was followed by GC-MS and UV-visible spectrophotometry analysis. The main metabolites observed were pyrimidinamine [149 m/z] and benzylsulfonamide [182 m/z]. The rate of biodegradation achieved by Aspergillus niger and Penicillium chrysogenum was 95% and 71%, respectively. The maximal decline in Bensulfuron-methyl concentration through hydrolysis was 48%. Furthermore, hydrolytic elimination was also evaluated based on time and pH. Both these parameters had a strong influence on the rate of transformation. Soils with lower pH exhibited an increased rate of degradation while a temperature of 27±2°C gave ideal conditions for herbicide decomposition. Percentage degradation and rate constant (k) followed first order reaction kinetics. Non-inoculated soils displayed less amounts of degradation. Furthermore, relative standard deviations were calculated for the residuals extracted in all soils. Analysis of variance (ANOVA) provided a p value < 0.05 for both strains with R2 closer to 1 signifying the significance of the results. Both fungal strains proved their potential for Bensulfuron-methyl remediation in soils.


2019 ◽  
Vol 65 (2) ◽  
pp. 46-57 ◽  
Author(s):  
Marek Pernica ◽  
Karim C. Piacentini ◽  
Karolina Benešová ◽  
Josef Čáslavský ◽  
Sylvie Běláková

The increasing interest in defining the content of mycotoxins is related to the development of methods for their determination. Several methods of determination have been published. This paper describes analytical procedures such as (a) sample preparation – sampling and homogenization, (b) extraction and purification – solid phase extraction (SPE), a QuEChERS method (acronymic name from quick, easy, cheap, effective, rugged and safe), solid-liquid extraction (SLE) and immuno affinity extraction (IAE). It also provides a review of, (c) instruments, and other analytical methods such as thin layer chromatography (TLC), enzyme linked immune sorbent assay (ELISA) and liquid chromatography (LC), gas chromatography (GC) with different detectors for determination of mycotoxin in barley, malt and beer are discussed.


Foods ◽  
2019 ◽  
Vol 8 (7) ◽  
pp. 273 ◽  
Author(s):  
Nho-Eul Song ◽  
Dong-Ho Seo ◽  
Ji Yeon Choi ◽  
Miyoung Yoo ◽  
Minseon Koo ◽  
...  

The monitoring of food quality and safety requires a suitable analytical method with simultaneous detection in order to control pesticide and herbicide residues. In this study, a novel analytical method, referred to as “dispersive solid–liquid extraction”, was applied to monitor seven sulfonylurea herbicides in strawberries. This method was optimized in terms of the amount of C18 and the volume of added water, and it was validated through satisfactory linearities (R2 > 0.99), recoveries of 70% to 84% with acceptable precisions, and limits of quantification lower than the maximum residue limits for the seven sulfonylurea herbicides in strawberries. The cleanup efficiency of the dispersive solid–liquid extraction technique was compared to that of the QuEChERS- (“quick, easy, cheap, effective, rugged and safe”) based method with dispersive solid phase extraction. The recoveries of the former were found to be comparable to those involving QuEChERS C18 cleanup (recoveries of 74%–87%). The method was used to determine sulfonylurea herbicide residues in ten strawberry samples. None of the samples had herbicide residues higher than that of limit of quantifications (LOQs) or maximum residue limits (MRLs). The results suggest that the dispersive solid–liquid extraction method combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS) is effective for the analysis of sulfonylurea herbicide residues in strawberries.


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