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monitoring data
Type of information:
experimental study
Adequacy of study:
supporting study
4 (not assignable)
Rationale for reliability incl. deficiencies:
documentation insufficient for assessment

Data source

Reference Type:
Rapid monitoring of residual UV-stabilizers in seawater samples from beaches using fabric phase sorptive extraction and UHPLC-MS/MS
Romualdo B. García-Guerra, Sarah Montesdeoca-Esponda, Zoraida Sosa-Ferrera, Abuzar Kabir, Kenneth G. Furton, José Juan Santana-Rodríguez
Bibliographic source:
Chemosphere 164, 201-207

Materials and methods

Principles of method if other than guideline:
Fabric phase sorption extraction (FPSE) procedure

The following steps were carried out:
1. Immersing FPSE media in 2 mL acetonitrile-methanol (50:50) for 5 min to clean it
2. Rinsing of the FPSE media with 2 mL of distilled water to remove residual organic solvents
3. Combining the clean FPSE media, a magnetic bar and the sample into a vial
4. Stirring at 1000 rpm on a magnetic stirrer during the optimum extraction time
5. Desorption in an appropriate volume of back-extraction solvent during an optimum time for complete back-extraction.
For chromatographic injection the sample will be transferred into a glass vial. After the extraction is completed the first step will be repeated. Then the FPSE media will be dried to eliminate the solvents by putting it on a watch glass for 5 to 10 min and stored in a hermetic glass container for future use.

Three differnt FPSE media were used:
1. sol-gel poly(dimethyldiphenylsiloxane) (PDMDPS)
2. sol-gel poly(tetrahydrofuran) (PTHF)
3. sol-gel poly(ethylene glycol) (PEG)
GLP compliance:
Type of measurement:
other: Residues of UV-stabilizer in seawater

Test material

Specific details on test material used for the study:
The following Benzotriazole UV stabilizer (BUVSs) were investigated:

- 2-(benzotriazol-2-yl)-4-methylphenol (UV P)
- 2-(benzotriazol-2-yl)-4-(2,4,4-trimethylpentan-2-yl) phenol (UV 329)
- 2-tert-butyl-6-(5-chlorobenzotriazol-2-yl)-4-methylphenol (UV 326)
- 2-(benzotriazol-2-yl)-4,6-bis(2-methybutan-2-yl) phenol (UV 328)
- 2,4-ditert-butyl-6-(5-chlorobenzotriazol-2-yl)phenol (UV 327)
- 2-(benzotriazol-2-yl)-6-[[3-(benzotriazol-2-yl)-2-hydroxy-5-(2,4,4-trimethylpentan-2-yl)phenyl]methyl]-4-(2,4,4-trimethylpentan-2-yl)phenol (UV 360)

Study design

Details on sampling:
Seawater samples were collected from three touristic beaches of the Gran Canaria island (Spain) on two different dates. From each beach four samples were taken. Each sample was collected from the surface layer (<10 cm) in glass amber bottles of 1 L. The bottles were filled up completely, transported to the laboratory on ice in absence of light and immediately filtered through a disposable syringe filter with pore size of 0.20 mm. Then the pH was adjusted to pH 3 with formic acid to inhibit microbial activity. All samples were stored in a fridge at 4 °C until their analysis within 48 h.

Results and discussion

Details on results:
UV-360 was the only detected BUVS, found in nine samples. All other BUVSs were not detected. The measured concentrations ranged from 41.12 to 544.9 ng/L. The compound was also detected in two other samples but could not be quantified because the concentration was lower than the LOQ.

Applicant's summary and conclusion

The presented method demonstrated that it is selective and sensitive enoughfor the quantification of the six target BUVSs (UV-P, UV-329, UV-326, UV-327, UV-328 and UV-360) from seawater samples collected from several touristic beaches of Gran canaria. Extraction parameters were optimized to achieve maximum efficiency. LODs and LOQs ranged from 1.06 to 8.96 ng/L and 3.54 to 29.9 ng/L, respectively. After method optimization UV 360 was determined in nine different seawater samples from three beaches of Gran Canary Island in concentrations between 41.12 and 544.9 ng/L.
Executive summary:

In this study the fabric phase sorptive extraction methodology to analyse six BUVSs in twenty-four seawater samples from different coastal areas of Gran Canaria Island was applied. In order to achieve a fast, reliable and sensitive separation and determination of the analytes from different simple matrices extraction was coupled to ultra high performance liquid chromatography with tandem mass spectrometry. With the optimized method UV-360 was the only detectable BUVS with concentrations ranging from 41.12 to 544.9 ng/L.