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A Simple and Rapid Method for Quantitative HPLC MS/MS Determination of Selected Perfluorocarboxylic Acids and Perfluorosulfonates in Human Serum.

ABSTRACT: Per- and polyfluorinated alkyl substances (PFASs) are ubiquitous environmental contaminants, present in the environment and in the human body. They have raised global concern because of their diffusion in the environment, particularly in water, causing cases of human overexposure due to consumption of contaminated drinking water. Human biomonitoring is the most effective way to characterize human exposure to PFASs, and it is important that as many labs as possible could easily perform this kind of analysis. Analytical methods for quantitation of PFAS mixtures in human serum have been developed, but most of them required materials that are not always easily available in all the laboratories. This paper describes a very simple and accessible HPLC MS/MS method of analysis and quantification of 13 perfluorocarboxylic acids and perfluorosulfonate compounds (belonging to the class of per- and polyfluorinated alkyl substances (PFASs)) in human serum. Method development data provide detailed descriptions of the optimization process in terms of sample preparation, laboratory analysis of human serum samples, determination of analytes by HPLC MS/MS, and describing the pump gradient time, working conditions, and acquisition.

SUBMITTER: Marra V

PROVIDER: S-EPMC7585657 | biostudies-literature | 2020

REPOSITORIES: biostudies-literature

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A Simple and Rapid Method for Quantitative HPLC MS/MS Determination of Selected Perfluorocarboxylic Acids and Perfluorosulfonates in Human Serum.

Marra Valentina V Abballe Annalisa A Dellatte Elena E Iacovella Nicola N Ingelido Anna Maria AM De Felip Elena E

International journal of analytical chemistry 20201016

Per- and polyfluorinated alkyl substances (PFASs) are ubiquitous environmental contaminants, present in the environment and in the human body. They have raised global concern because of their diffusion in the environment, particularly in water, causing cases of human overexposure due to consumption of contaminated drinking water. Human biomonitoring is the most effective way to characterize human exposure to PFASs, and it is important that as many labs as possible could easily perform this kind ...[more]

PMID: 33123200

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Project description:Diacyl glycerophospholipids (GPs) belong to the most abundant lipid species in living organisms and consist of a glycerol backbone with fatty acyl groups in sn-1 and sn-2 and a polar head group in the sn-3 position. Regioisomeric mixed diacyl GPs have the same fatty acyl composition but differ in their allocation to sn-1 or sn-2 of the glycerol unit. In-depth analysis of regioisomeric mixed diacyl GP species composed of fatty acyl moieties that are similar in length and degree of saturation typically requires either chemical derivatization or sophisticated analytical instrumentation, since these types of regioisomers are not well resolved under standard ultra-performance liquid chromatography (UPLC) conditions. Here, we introduce a simple and fast method for diacyl GP regioisomer analysis employing UPLC tandem mass spectrometry (MS/MS). This GP regioisomer analysis is based both on minor chromatographic retention time shifts and on major differences in relative abundances of the two fatty acyl anion fragments observed in MS/MS. To monitor these differences with optimal precision, MS/MS spectra are recorded continuously over the UPLC elution profile of the lipid species of interest. Quantification of relative abundances of the regioisomers was performed by algorithms that we have developed for this purpose. The method was applied to commercially available mixed diacyl GP standards and to total lipid extracts of Escherichia coli (E. coli) and bovine liver. To validate our results, we determined regioisomeric ratios of phosphatidylcholine (PC) standards using phospholipase A2-specific release of fatty acids from the sn-2 position of the glycerol backbone. Our results show that most analyzed mixed diacyl GPs of biological origin exhibit significantly higher regioisomeric purity than synthetic lipid standards. In summary, this method can be implemented in routine LC-MS/MS-based lipidomics workflows without the necessity for additional chemical additives, derivatizations, or instrumentation.

Dataset Information

A Simple and Rapid Method for Quantitative HPLC MS/MS Determination of Selected Perfluorocarboxylic Acids and Perfluorosulfonates in Human Serum.

Publications

A Simple and Rapid Method for Quantitative HPLC MS/MS Determination of Selected Perfluorocarboxylic Acids and Perfluorosulfonates in Human Serum.

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