Liquid Chromatography Tandem Mass Spectrometry Method for Ultra-Trace Analysis of Organic UV Filters in Environmental Water Samples

Abstract

A liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) method was developed and validated for the simultaneous determination of six organic compounds (2-hydroxy benzophenone, 4hydroxy benzophenone, 2,2',4,4'-tetrahydroxy benzophenone, 2,4-dyhydroxy benzophenone, 4,4'dyhydroxy benzophenone, 2,2'-dyhydroxy-4-methoxy-benzophenone) used as UV filters in personal care products used to protect against UV radiation. The major concern about this type of pollutants is due to their persistence and bioaccumulation potential in the environment and aquatic organisms and for their endocrine disruptor properties. Solid phase extraction was used for sample preparation, followed by liquid chromatography tandem mass spectrometry analysis. Benzophenone derivatives were analyzed on a Phenomenex Luna C18 column (150 x 2.0 mm, 3.0 µm) with the mobile phase run in gradient mode with a mixture of aqueous 0.1% formic acid and acetonitrile as the mobile phase components (at a flow rate of 0.2 mL/min). MS detector response was linear, on the tested concentration domain from 1 to 100 μg/L with correlation coefficient R 2 > 0.998. The recoveries of benzophenone derivatives after solid phase extraction procedure from surface water was found to be >81% for surface water and higher than 79% for wastewater matrix. The standard deviation values for intra-day precision were situated between 7.67% and 9.88% for lower concentration and 7.27% and 8.86% for higher concentration respectively. The limits of quantitation were calculated for both environmental water matrices (1.6-4.1 ng/L for surface water and 3.3-8.2 ng/L for wastewater). This method can be applied for benzophenone derivatives detection in real environmental samples.

Benzophenones in the Environment: Occurrence, Fate and Sample Preparation in the Analysis

“…However, the linear range was rather short (2–10 mg/L) compared with other methods [ 65 ]. In another work, Chiriac et al compared two types of SPE cartridges, in order to determine the optimum for the detection of six BPs and to develop an analytical method [ 66 ]. The authors used Strata C18 cartridges, achieving recoveries between 81.9 and 96.4%, and Strata-X cartridges (pore size of 30μm, polymeric reverse phase), attaining somewhat lower recoveries (74.0–82.6%) [ 66 ].…”

“…In another work, Chiriac et al compared two types of SPE cartridges, in order to determine the optimum for the detection of six BPs and to develop an analytical method [ 66 ]. The authors used Strata C18 cartridges, achieving recoveries between 81.9 and 96.4%, and Strata-X cartridges (pore size of 30μm, polymeric reverse phase), attaining somewhat lower recoveries (74.0–82.6%) [ 66 ]. The developed method achieved enrichment factors (EF) of 200 and 100 for surface water and wastewater, respectively.…”

“…The developed method achieved enrichment factors (EF) of 200 and 100 for surface water and wastewater, respectively. Despite the overall good characteristics, the method was time-consuming, given that 100-200 mL of sample was passed with a flow rate of 5 mL/min (20–40 min extraction time), plus 30 min of solvent evaporation was required [ 66 ]. Kharbouche et al proposed the use of mesoporous silica-based materials MCM-41 and MCM-41-CN(a cyanopropyl derivatized MCM-41) as SPE sorbents, for the extraction of four BPs [ 67 ].…”

Chemometric Optimization of Solid-Phase Extraction Followed by Liquid Chromatography-Tandem Mass Spectrometry and Probabilistic Risk Assessment of Ultraviolet Filters in an Urban Recreational Lake

“…One is gas chromatography with tandem mass spectrometry (GC-MS/MS) (da Silva et al, 2015;Huang et al, 2016;Ramos et al, 2019), which has a huge potential for identification and selectivity in separation. Another technique is liquid chromatography with tandem mass spectrometry (LC-MS/ MS) (Li et al, 2020b;Chiriac et al, 2020;Cadena-Aizaga et al, 2022), which is characterized by exceptional sensitivity and is very suitable for the analysis of lowvolatile and degradable UVFs.…”

Environmental Detection of Brilliant Blue, Sunset Yellow and Tartrazine Using Direct Injection HPLC-DAD Technique

“…A current problem for aquatic ecosystems that can cause a change in the natural balance of flora and fauna is the discharge of industrial and domestic wastewater loaded with various xenobiotic dyes into natural receptors usually represented by rivers and lakes [5]. Among the industrial waters involved are those that come from activities that use dyes in their production cycles.…”