Preparation of Fe3O4@PPy magnetic nanoparticles as solid-phase extraction sorbents for preconcentration and separation of phthalic acid esters in water by gas chromatography–mass spectrometry

In this work, Chromabond® HLB was evaluated as an extraction sorbent of a group of seven phthalic acid esters (PAEs; i.e., dipropyl phthalate, DPP, dibutyl phthalate, DBP, diisopentyl phthalate, DIPP, di-n-pentyl phthalate, DNPP, butylbenzyl phthalate, BBP, dicyclohexyl phthalate, DCHP, and di(2-ethylhexyl)phthalate, DEHP) and one adipate (di(2-ethylhexyl) adipate, DEHA) from tap and waste water prior to gas chromatography-mass spectrometry. After the optimization of the extraction conditions (200 mg of sorbent conditioned with 10 mL of acetonitrile and 2 mL of Milli-Q water, extraction of 50 mL of water at pH 6.0, vacuum drying for 20 min and elution with 10 mL of ethyl acetate), a recovery study was developed at different concentration levels in each matrix, which revealed that most of the target analytes could be recovered between 75 and 112%, with relative standard deviation values for all of them below 20%. Matrix effect was evaluated, finding that matrix-matched calibration should be developed for most analytes in both matrices. The limits of quantification (LOQs) of the method were in the 0.82–71 ng L−1 range. The developed method was also applied to the extraction of the target PAEs in different water samples finding some of them, in particular, DNPP in tap water samples, and BBP and DCHP in waste water, but below the LOQs of the method.

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Magnetic Graphene Dispersive Solid-Phase Extraction for the Determination of Phthalic Acid Esters in Flavoring Essences by Gas Chromatography Tandem Mass Spectrometry

Journal of Chromatographic Science ◽

10.1093/chromsci/bmaa032 ◽

2020 ◽

Vol 58 (8) ◽

pp. 770-778

Author(s):

Jing Zhu ◽

Binglin Lu ◽

Shanshan Liu ◽

Aifei Xu ◽

Guifang Tang ◽

...

Keyword(s):

Mass Spectrometry ◽

Phthalic Acid ◽

Solid Phase ◽

Tandem Mass ◽

Phase Extraction ◽

Phthalic Acid Esters ◽

Chromatography Tandem Mass Spectrometry ◽

Magnetic Graphene ◽

Acid Esters

Abstract In the present study, a sensitive, efficient and repeatable method for the simultaneous extraction and determination of 13 types of phthalic acid esters (PAEs) in flavoring essence samples using magnetic graphene solid-phase extraction coupled with gas chromatography tandem mass spectrometry was developed. Due to the unique structure of magnetic graphene, it has several advantages, such as large surface area and fast separation ability. This unique structure not only provided strong magnetic responsiveness for the separation but also prevented the self-aggregation of graphene. The large delocalized p-electron system of graphene can form strong π-stacking interactions with the benzene ring. Thus, graphene may be also a good candidate adsorbent for the adsorption of benzenoid-form compounds. Several magnetic soild-phase extraction parameters, such as elution solvents, amounts of sorbents, enrichment time and desorption time were optimized. The optimized procedures for this method were performed by ultrasonication using ethyl acetate as elution solvent for 5 min. Under the optimal conditions, the developed method provided spiked recoveries of 75.0–105.3% with relative standard deviations of ~5.6% and limits of detection were 0.011–0.091 mg/kg. Good linear relationships were observed with the coefficient of determination (R2) > 0.993 for all the analytes. Finally, the validated method was successfully applied to the analysis of PAEs in real samples.

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