Micro-QuEChERS extraction coupled to GC–MS for a fast determination of Bisphenol A in human urine

Abstract

Bisphenol A (BPA) is considered an endocrine disruptor and public concern over BPA exposure has been raised. Several studies have assessed human exposure to this plasticizer, confirming its ubiquitous presence and highlighting children as a public of special concern. A simple, efficient, cheap and green analytical procedure is reported within this paper. This paper reports, for the first time, the development of a modified Micro-QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method coupled to gas chromatography-mass spectrometry (GC-MS) as a new strategy for the efficient extraction and determination of Bisphenol A in human urine samples. Several parameters that are known to influence extraction were optimized. Good linearity was achieved at the studied concentration range (1-50μg/L), with a correlation coefficient (R) of 0.998. The optimized method proved to be accurate (≥74% recovery), reproducible (<11% relative standard deviation) and sensitive for BPA determination (detection limit of 0.13μg/L and quantification limit of 0.43μg/L). The analytical procedure was applied to the analyses of 12 urine samples collected from children living in the North/Center region of Portugal. BPA was detected in all the analyzed samples in concentrations ranging from 1.5μg/L to 48.9μg/L. The proposed methodology is suitable for the determination of BPA in urine samples in the framework of biomonitoring studies and bioanalytical analyses, applying GC-MS detection.

Determination of four bisphenols in water and urine samples by magnetic dispersive solid‐phase extraction using a modified zeolite/iron oxide composite prior to liquid chromatography diode array detection

“…Regarding to amount of sorbent, this work shows similar amounts of sorbent to previous works, except for methods based on conventional SPE (i.e., 200 and 300 mg) or QuEChERS (i.e., 750 mg) , which consume sorbent amounts that are one order of magnitude greater. Furthermore, the extraction technique developed here presents advantages related to ease of sorbent handling (i.e., magnetic properties) versus other techniques such as SPE and dispersive solid‐phase microextraction (called SPME in publication and micro‐QuEChERS ), avoiding column preparation and centrifugation steps , respectively. Between the different methods based on MDSPE, on the one hand, the magnetic composite employed as sorbent in this work affords easier magnetization synthesis than the other composites (i.e., solvothermal method) and, on the other hand, HDTMA‐ZSM‐5/Fe 2 O 3 composite is more economical than graphene‐based composites (e.g., (3DG)/ZnFe 2 O 4 ) since zeolites are considered low cost materials.…”

“…On the other hand, it is important to highlight that LODs reported in this work are empirical whereas LODs recorded for previous methods were obtained employing statistical methods (i.e., calculated using S/N or the SD of the blank), which provide commonly lower LODs. In addition, the LOD for BPA in this work is comparable to the one obtained using micro‐QuEChERs extraction coupled to GC‐MS employing more economical analytical instrumentation (i.e., LC‐DAD). Regarding to amount of sorbent, this work shows similar amounts of sorbent to previous works, except for methods based on conventional SPE (i.e., 200 and 300 mg) or QuEChERS (i.e., 750 mg) , which consume sorbent amounts that are one order of magnitude greater.…”

“…In addition, the LOD for BPA in this work is comparable to the one obtained using micro‐QuEChERs extraction coupled to GC‐MS employing more economical analytical instrumentation (i.e., LC‐DAD). Regarding to amount of sorbent, this work shows similar amounts of sorbent to previous works, except for methods based on conventional SPE (i.e., 200 and 300 mg) or QuEChERS (i.e., 750 mg) , which consume sorbent amounts that are one order of magnitude greater. Furthermore, the extraction technique developed here presents advantages related to ease of sorbent handling (i.e., magnetic properties) versus other techniques such as SPE and dispersive solid‐phase microextraction (called SPME in publication and micro‐QuEChERS ), avoiding column preparation and centrifugation steps , respectively.…”

“…A comparison between this work and previously reported procedures combining different SPE techniques and sorbents for the determination of several BPs in urine and water samples is summarized in Supporting Information Table S4 . As shown, the proposed method provides LODs comparable with previous works using a shorter extraction time (i.e., 2 min compared to 10 , 15 , and 30 min ).…”

“…As shown, the proposed method provides LODs comparable with previous works using a shorter extraction time (i.e., 2 min compared to 10 , 15 , and 30 min ). The publications that presented slightly lower LODs included additional time‐consuming steps of solvent evaporation and reconstitution in the extraction procedure. On the other hand, it is important to highlight that LODs reported in this work are empirical whereas LODs recorded for previous methods were obtained employing statistical methods (i.e., calculated using S/N or the SD of the blank), which provide commonly lower LODs.…”