scholarly journals Validation of LC-MS/MS Coupled with a Chiral Column for the Determination of 3- or 15-Acetyl Deoxynivalenol Mycotoxins from Fusarium graminearum in Wheat

Toxins ◽  
2021 ◽  
Vol 13 (9) ◽  
pp. 659
Author(s):  
Lan Wang ◽  
Zheng Yan ◽  
Haiyan Zhou ◽  
Yingying Fan ◽  
Cheng Wang ◽  
...  
Keyword(s):  
Fusarium Graminearum ◽  
Chromatographic Separation ◽  
Sample Pretreatment ◽  
Good Stability ◽  
Cereal Grains ◽  
Chiral Column ◽  
Limits Of Detection ◽  
Fusarium Asiaticum

The major causal agents Fusarium graminearum (F. graminearum) and Fusarium asiaticum could produce multiple mycotoxins in infected wheat, which threatens the health of humans and animals. Specifically, deoxynivalenol (DON) and its derivatives 3- and 15-acetyldeoxynivalenol (3-ADON and 15-ADON) are commonly detected mycotoxins in cereal grains. However, the good chromatographic separation of 3-ADON and 15-ADON remains challenging. Here, an LC-MS/MS method for the chemotype determination of Fusarium strains was developed and validated. 3- and 15-ADON could be separated chromatographically in this study with sufficiently low limits of detection (LODs; 4 μg/kg) and limits of quantification (LOQs; 8 μg/kg). The satisfying intraday and interday reproducibility (both %RSDr and %RSDR were <20%) of this method indicated good stability. The recoveries of all analytes were in the range of 80–120%. In addition, three F. graminearum complex (FGC) strains, i.e., PH-1 (chemotype 15-ADON), F-1 (chemotype 3-ADON) and 5035 (chemotype 15-ADON), were selected to verify the accuracy of the method in differentiating phenotypes. The validation results showed that this LC-MS/MS method based on sample pretreatment is effective and suitable for the chromatographic separation of 3-ADON and 15-ADON in wheat.

scholarly journals Pig Urinary Concentration of Mycotoxins and Metabolites Reflects Regional Differences, Mycotoxin Intake and Feed Contaminations

Toxins ◽  
2019 ◽  
Vol 11 (7) ◽  
pp. 378 ◽  
Author(s):  
Lucia Gambacorta ◽  
Monica Olsen ◽  
Michele Solfrizzo
Keyword(s):  
Risk Assessment ◽  
Fusarium Graminearum ◽  
Regional Differences ◽  
Fumonisin B1 ◽  
Cereal Grains ◽  
Aflatoxin M1 ◽  
Urinary Concentration ◽  
Metabolite Concentrations ◽  
Good Agreement

The determination of mycotoxin and metabolite concentrations in human and animal urine is currently used for risk assessment and mycotoxin intake measurement. In this study, pig urine (n = 195) was collected at slaughterhouses in 2012 by the Swedish National Food Agency in three counties representing East, South and West regions of Sweden. Urinary concentrations of four mycotoxins, (deoxynivalenol (DON), zearalenone (ZEA), fumonisin B1 (FB1), and ochratoxin A (OTA)), and four key metabolites, (deepoxy-deoxynivalenol (DOM-1), aflatoxin M1 (AFM1, biomarker of AFB1), α-zearalenol (α-ZOL), and β-zearalenol (β-ZOL)) were identified and measured by UPLC-MS/MS. Statistically significant regional differences were detected for both total DON (DON + DOM-1) and total ZEA (ZEA + α-ZOL + β-ZOL) concentrations in pig urine from the three regions. These regional differences were in good agreement with the occurrence of Fusarium graminearum mycotoxins (DON + ZEA) in cereal grains harvested in 2011 in Sweden. There were no statistically significant differences in FB1, AFM1 and OTA urinary concentrations in pigs from the three regions. The overall incidence of positive samples was high for total ZEA (99–100%), total DON (96–100%) and OTA (85–95%), medium for FB1 (30–61%) and low for AFM1 (0–13%) in the three regions. Urinary mycotoxin biomarker concentrations were used to estimate mycotoxin intake and the level of mycotoxins in feeds consumed by the monitored pigs. The back-calculated levels of mycotoxins in feeds were low with the exception of seven samples that were higher the European limits.

DETERMINATION OF MICRO-AMOUNTS OF 5β-PREGNAN-3α-OL-20-ONE IN URINE USING INFRARED-SPECTROMETRY

1962 ◽  
Vol 41 (2) ◽  
pp. 234-246 ◽  
Author(s):  
H. J. van der Molen
Keyword(s):  
Infrared Spectrum ◽  
Quantitative Determination ◽  
Acid Hydrolysis ◽  
Chromatographic Separation ◽  
Pure Form ◽  
Infrared Spectrometry ◽  
Hydrolysis Of

ABSTRACT A procedure for the quantitative determination of 5β-pregnan-3α-ol-20-one in urine is described. After acid hydrolysis of the pregnanolone-conjugates in urine, the free steroids are extracted with toluene. Pregnanolone is isolated in a pure form as its acetate; after chromatographic separation of the free steroids on alumina, the fraction containing pregnanolone is acetylated and rechromatographed on alumina. Quantitative determination of the isolated pregnanolone-acetate is carried out with the aid of the infrared spectrum recorded by a micro KBr-wafermethod. The reliability of the method under various conditions is discussed under the headings, specificity, accuracy, precision and sensitivity. It is possible to determine 30–40 μg pregnanolone in a 24-hours urine portion with a precision of 25%.

Determination of Sulfite in Beer Based on Fluorescent Derivatives and Liquid Chromatographic Separation

2012 ◽  
Vol 70 (4) ◽  
pp. 296-302 ◽  
Author(s):  
Victor Abrahamsson ◽  
Signe Hoff ◽  
Nikoline J. Nielsen ◽  
Marianne N. Lund ◽  
Mogens L. Andersen
Keyword(s):  
Chromatographic Separation ◽  
Liquid Chromatographic Separation ◽  
Liquid Chromatographic ◽  
Fluorescent Derivatives

scholarly journals Simultaneous determination of iron and copper in children's sera by FAAS

2011 ◽  
Vol 61 (1) ◽  
pp. 93-102 ◽  
Author(s):  
Svjetlana Luterotti ◽  
Tončica Kordić ◽  
Slavica Dodig
Keyword(s):  
Atomic Absorption ◽  
Simultaneous Determination ◽  
Sample Pretreatment ◽  
Single Step ◽  
Design Experiment ◽  
New Approach ◽  
Flame Atomic Absorption ◽  
Reference Methods ◽  
Atomic Absorption Spectrometric

Simultaneous determination of iron and copper in children's sera by FAASA new and simple flame atomic-absorption spectrometric (FAAS) method is proposed for simultaneous determination of iron and copper in children's sera. It is based on single-step sample pretreatment (deproteinization with 3 mol L-1HCl, ratio 1:1) and single-step calibration using 1.5 mol L-1HCl standard. During method's optimization a short multifactorial design experiment was used. The proposed method assures accuracy, sensitivity and precision comparable to that of the reference methods. The new approach is simple and time-, labour- and serum-saving, the latter being especially important in pediatric diagnostics.

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