Search results for " mass spectrometry"

Producing SI-traceable reference values for Cd, Cr and Pb amount contents in polyethylene samples from the Polymer Elemental Reference Material (PERM…

2000

The present paper describes the certification of the amount content of Cd, Cr and Pb in two different polyethylene materials within the third phase of the Polyethylene Elemental Reference Material (PERM) project. The analytical procedure to establish the reference values for Cd, Cr and Pb amount contents in these materials is based on isotope dilution mass spectrometry used as a primary method of measurement. Cd and Pb were measured with inductively coupled plasma-mass spectrometry and Cr with positive thermal ionization-mass spectrometry. The decomposition of the polymer matrix was carried out using a high pressure asher. Reference values for amount content, traceable to the SI-system, hav…

Development of microextraction techniques in combination with GC-MS/MS for the determination of mycotoxins and metabolites in human urine.

2017

Simple and highly efficient sample preparation procedures, namely, dispersive liquid–liquid microextraction and salting-out liquid–liquid extraction for the analysis of ten Fusarium mycotoxins and metabolites in human urine were compared. Various parameters affecting extraction efficiency were carefully evaluated. Under optimal extraction conditions, salting-out liquid–liquid extraction showed a better accuracy (84–96%) and precision (<14%) than dispersive liquid–liquid microextraction. Hence, a multibiomarker method based on salting-out liquid–liquid extraction followed by gas chromatography with tandem mass spectrometry was proposed. Satisfactory results in terms of validation were achiev…

230Th/U-dating of a late Holocene low uranium speleothem from Cuba

2010

We present 22 U-series ages for a stalagmite from north-western Cuba based on multi-collector inductively coupled plasma mass spectrometry (MC-ICPMS) and thermal ionisation mass spectrometry (TIMS). Our results reveal that the stalagmite continuously grew within the last ~1400a. Low uranium content of the sample and thus, extremely low 230Th concentrations limit the precision and accuracy of 230Th/U-dating by TIMS. Samples measured by MC-ICPMS show a high variability of 232Th content along the growth axis with some sections significantly affected by initial 230Th from a detrital phase. An a-priori bulk earth ratio for (238U/232Th) cannot be used to accurately account for this initial 230Th.…

Quantitative evaluation of the phenolic profile in fruits of six avocado (Persea americana) cultivars by ultra-high-performance liquid chromatography…

2016

The phenolic profiles of six varieties of avocado (Persea americana) grown in Sicily were investigated. The ultra-high-performance liquid chromatography-heated electrospray-mass spectrometry method was developed to determine qualitative and quantitative changes in fruits at two different ripening stage. Nineteen individual phenolic compounds were detected in avocado pulp extracts. Gallic acid, sinapinic acid, vanillin, p-coumaric acid, and gentisic acid were present only in ripe fruits. On the contrary, epicatechin decreased with fruit ripening, whereas protocatechuic acid, 4-hydroxybenzoic acid, chlorogenic acid, and benzoic acid were relatively stable or exhibited erratic changes with fru…

Development of a GC–MS/MS strategy to determine 15 mycotoxins and metabolites in human urine

2014

The widespread mycotoxins contamination of food commodities has made the monitoring of their levels essential. To overcome the disadvantages of the indirect approach by food analysis, detection of mycotoxin as biomarkers in urine provides a useful and specific data for exposure assessment to these food contaminants. In this work, a sensitive, rapid and accurate method based on gas chromatography-tandem mass spectrometry procedure to determine 15 mycotoxins and metabolites in human urine was optimized and validated taking into consideration the guidelines specified in Commission Decision 2002/657/EC and 401/2006/EC. A salting-out assisted acetonitrile-based extraction was used for sample pre…

Multi-mycotoxin analysis in wheat semolina using an acetonitrile-based extraction procedure and gas chromatography–tandem mass spectrometry

2012

A new analytical method for the rapid and simultaneous determination of ten mycotoxins including patulin, zearalenone and eight trichothecenes (nivalenol, fusarenon-X, diacetoxyscirpenol, 3-acetyl-deoxynivalenol, neosolaniol, deoxynivalenol, T-2 and HT-2) in wheat semolina has been developed and optimized. Sample extraction and purification were performed with a modified QuEChERS-based (acronym of Quick, Easy, Cheap, Effective, Rugged and Safe) procedure and determined by gas chromatography (GC) coupled to triple quadrupole instrument (QqQ). This is the first paper on the application of GC-QqQ-MS/MS to analysis of mycotoxins. Careful optimization of the gas chromatography-tandem mass spectr…

Room temperature acid sonication ICP-MS multielemental analysis of milk

2005

Abstract Room temperature acid sonication of milk samples is proposed as a fast alternative methodology for the determination of the total content of 45 elements (Li, Al, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Rb, Sr, Y, Mo, Ag, Cd, In, Sn, U, Sb, Te, Cs, Ba, Hg, Pb, Bi, Th, La, Ce, Pr, Nd, Sm, Eu, Gd, Dy, Ho, Er, Tm, Yb, Lu, Hf and Ta) in milk by inductively coupled plasma mass spectrometry (ICP-MS). The aforementioned procedure involves a 10 min sample pre-treatment. Measurements were made in quantitative and semiquantitative (Totalquant ® ) modes of analysis using Rh as internal standard and Be, Ge, Tb and Re for internal calibration of the equipment in the semiquantitative mode. The…

Exposure assessment of Spanish lactating mothers to acrylamide via human biomonitoring.

2021

Abstract Acrylamide (AA) is an organic compound classified as “Probably carcinogenic to humans” (Group 2 A) that can be found principally in processed carbohydrate-rich foods and tobacco smoke. In humans, after exposure, AA is rapidly metabolized and excreted in urine, predominantly as N-acetyl-S-(2-carbamoylethyl)-l-cysteine (AAMA), N-acetyl-S-(2-carbamoyl-2-hydroxyethyl)-l-cysteine (GAMA3) and N-Acetyl-3-[(3-amino-3-oxopropyl)sulfinyl]-L-alanine (AAMA-Sul), which can be used as short-term biomarkers of exposure to AA. In this study, the presence of AA metabolites in urine samples of lactating mothers living in Spain (n = 114) was analyzed by “dilute and shoot” and liquid chromatography co…

Proteomic investigations to unravel molecular physiology of the lantibiotic producer Microbispora sp. ATCC‐PTA‐5024

2013

Application of LA-ICP-MS as a rapid tool for analysis of elemental impurities in active pharmaceutical ingredients.

2014

The control of inorganic contaminants in active pharmaceutical ingredients has a significant role in the quality control of drug products. The concentration limits for metal residues in drug products have been defined by various regulatory guidelines. Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is a powerful and fast analytical technique for multi-elemental analysis. A disadvantage in using LA-ICP-MS method is the lack of matrix reference materials for validation and calibration purposes. This article focuses on the handling strategy of laboratory-made matrix calibration standards for the quantification of elemental impurities in an active pharmaceutical ingredie…