Microwave‐assisted extraction combined with on‐line solid phase extraction followed by ultra‐high‐performance liquid chromatography with tandem mass spectrometric determination of benzotriazole UV stabilizers in marine sediments and sewage sludges

Abstract

Benzotriazole ultra-violet stabilisers are compounds widely used in personal care products, which can reach the environment after passing through wastewater treatment plants. In this work, we develop a novel method to evaluate the presence of seven compounds in marine sediments and sewage sludges using microwave-assisted extraction followed by a clean-up step based in on-line solid phase extraction coupled to ultra-high-performance liquid chromatography with MS/MS detection. This method allows for fast and efficient extraction from the solid matrix, subsequent automatic on-line purification and preconcentration, and analysis. For the optimised method, LOD were from 53.3 to 146 ng/kg and LOQ were in the range of 176-486 ng/kg. The method was validated for different environmental solid samples with satisfactory recoveries and relative standard deviations, between 46.1 and 83.9 and 7.8 and 15.5% (sludges) and 50.1 and 87.1% and 8.83 and 16.3% (sediments), respectively. Finally, the studied analytes were quantified in concentrations between 0.18 and 24.0 ng/g in real samples of marine sediments and sewage sludges from Gran Canaria Island (Spain).

Multi-target determination of organic ultraviolet absorbents in organism tissues by ultrasonic assisted extraction and ultra-high performance liquid chromatography–tandem mass spectrometry

“…Efficient extraction of some benzotriazole UV stabilizers has been a challenge as reported previously [45]. However, satisfactory recoveries were obtained for the benzotriazole UV stabilizers from fish filet and fish belly samples, comparable with those for Table 3 Recoveries (%, mean ± SD, n = 3) of the UV absorbents.…”

“…Montesdeoca-Esponda et al [45] observed co-elution of some benzotriazole UV stabilizers (e.g., UV-326, UV-327 and UV-328) on an octadecyl silica-based RP UHPLC column. Although complete separation is not indispensable in SRM mode, sufficient separation helps to improve detectability and to reduce ion suppression [58], whereas co-elution may impair proper quantification of the analytes due to competitive ionization [34].…”

“…APCI and electronic spray ionization (ESI) have been widely used in determination of various UV absorbents [12,32,34,35,37,[40][41][42][43][45][46][47]49,50]. ESI was reported to provide better sensitivity for compounds of medium to high polarity and APCI is favorable for ionization of compounds with low polarity [47,59].…”

“…It is therefore very likely that various UV absorbents accumulate concurrently in the environment, especially in coastal waters where are usually served for agricultural (e.g., fishing and mariculture), industrial (e.g., shipping and offloading) as well as recreational purposes. In addition, most of the available research focused on water and sediment [30,31,[33][34][35][36][37][38][39][40][41][45][46][47] whereas methods for determination of the UV filters and stabilizers in organism tissues are still limited [4,34,43]. However, many organic UV absorbents have potential for bioaccumulation and biomagnification through trophic web given their strong lipophilicity [14].…”

Microwave-assisted extraction of emerging pollutants in environmental and biological samples before chromatographic determination

“…Both types of UV filter, benzophenone and benzotriazole derivatives, have been extracted from sediments and sludges using MW energy [26,46].…”