Simultaneous determination of fifteen multiclass organic pollutants in human saliva and serum by liquid chromatography–tandem ultraviolet/fluorescence detection: A validated method

Abstract

A quick and inexpensive validated method, based on sample treatment by liquidliquid microextraction followed by liquid chromatography (LC) coupled with ultraviolet tandem fluorescence detection is proposed for the determination of 15 multiclass pollutants both in serum and in saliva, as a simple and easy to draw matrix. The method was set up and validated according to European guidelines. The compounds of interest include some endocrine-disrupting chemicals (i.e. bisphenol A, bisphenol B, bisphenol E, bisphenol F, bisphenol AF, bisphenol A diglycidyl ether, bisphenol M, diethylhexyl phthalate, monoethylhexyl phthalate, triclosan and 4-nonylphenol), as well as other pollutants belonging to the class of volatile organic compounds (2chlorophenol, 1,2 dichlorobenzene, 1,2,4,5-tetrachlorobenzene). The limits of quantifications ranged from 2.28 × 10 −3 μg mL −1 (bisphenol A diglycidyl ether) to 6.29 μg mL −1 (diethylhexyl phthalate), while those of detection ranged from 0.068 × 10 −3 μg mL −1 (bisphenol A diglycidyl ether) to 1.031 μg mL −1 (diethylhexyl phthalate). To test method suitability, it was applied to real saliva and serum samples of healthy human volunteers and was found to meet the demands of the laboratories handling simple and relatively inexpensive equipment for screening oriented at rapid and reliable contamination assessment of a population.

Bisphenol A Diglycidyl Ether (BADGE) and Bisphenol Analogs, but Not Bisphenol A (BPA), Activate the CatSper Ca2+ Channel in Human Sperm

“…The EC 50 -values estimated from these curves ranged from 0.79 to 14.87 µM and the lowest effective dose values (EC 05 ) ranged from 0.18 to 2.37 µM ( Table 2). In the literature, we could only identify human plasma or serum levels for BPAF, BADGE, and BPB out of the six "positive hit" bisphenols (49)(50)(51)(52)(53). A reported maximal human serum concentration of BADGE (3.45 µM) (50) is above the EC 05 estimated in our study (1.82 µM), whereas the reported maximal human serum levels of BPAF (0.05 µM) (50) and BPB (0.59 µM) (50) are below the estimated EC 05 -values of 0.36 µM for BPAF and 2.37 µM for BPB.…”

Monitoring of Pollutants Content in Bottled and Tap Drinking Water in Italy

“…These results indicate that this analytical method provides a reliable response regardless of the concentrations utilized. This is straightforward given that the biological matrices studied in [38] are much more complex than the waters assayed in this work. After running of each sample in triplicate, methanol injections did not show carryover.…”

The occurrence of selected endocrine‐disrupting chemicals in water and sediments from an urban lagoon in Southern Italy

“…Standard calibration curves covered the range indicated in Table 2 and had squared correlation coefficients ( r 2 ) greater than 0.95. The separation and detection of the selected EDCs were accomplished according to an already published method (Russo, Barbato, et al, 2019). All mobile phases were filtered through nylon filters 0.45 μm in pore diameter (Millipore, Burlington, MA USA).…”

“…A systematic QA/QC protocol was adopted to monitor the analysis of chemicals under investigation, including linearity, retention time, limits of detection (LOD) and quantification (LOQ), and recovery. For every batch of samples, a procedural blank and spike sample consisting of all reagents was run to check for interference and cross‐contamination (Russo, Barbato, et al, 2019). The Limit of detection (LOD) indicates method's sensitivity, and it is the lowest concentration, at which the respective compound is just measurable.…”

“…So far, BPs have been detected in food (Cacho et al, 2012; Fattore et al, 2015; Grumetto et al, 2013; Liao & Kannan, 2013), house dust (Liao, Liu, Guo, et al, 2012), water and sediments of seas, rivers, and lakes (Gong et al, 2016; Liao, Liu, Alomirah, et al, 2012; Liu et al, 2017; Noszczynska & Piotrowska‐Seget, 2018; Song et al, 2014; Sun et al, 2017), personal care products (Liao & Kannan, 2014), and thermal paper (Liao et al, 2012; Russo et al, 2017). Furthermore, BPs have also been detected in human biological specimens such as blood, urine, and saliva (Cobellis et al, 2009; Cunha & Fernandes, 2010; Liao, Liu, Alomirah, et al, 2012; Russo et al, 2019; Zhou et al, 2013; Zhou et al, 2014).…”