Key Takeaways & Executive Findings
- •• • Achieved simultaneous quantification of 11 OUVs in coral tissue with method detection limits (MDLs) of 0.020–0.133 ng·g−1 and quantification limits (MQLs) of 0.080–0.532 ng·g−1, enabling trace-level monitoring essential for assessing bioaccumulation in marine organisms. • • The optimized extraction protocol (sequential methanol and ethyl acetate, vortexing 20 min, ultrasonication 20 min at 30 °C) yielded recoveries of 60.5%–120.3% across three spiking levels (1, 10, 50 ng·g−1) with RSDs ≤10.7%, demonstrating robustness for complex biological matrices. • • Chromatographic separation on CAPCELL PAK MG C18 (5 μm, 2.1 mm × 100 mm) at 40 °C with a methanol–0.1% formic acid gradient achieved baseline separation within 15 min, balancing resolution and throughput for routine monitoring. • • Field application to 89 coral samples from Xidao Island detected five target OUVs, confirming the method's practical utility for environmental surveillance and risk assessment in coral reef ecosystems.
Abstract
An analytical method was developed for the simultaneous determination of 11 organic ultraviolet absorbents (OUVs) in coral tissues using ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Target analytes included benzophenones (BP, BP-2, BP-3, BP-8) and other common UV filters. Sample pretreatment and chromatographic conditions were systematically optimized. Coral tissue samples were extracted by combined vortexing and ultrasonication, separated on a CAPCELL PAK MG C18 column using a mobile phase of methanol-0.1% formic acid aqueous solution under gradient elution, and determined by multiple reaction monitoring (MRM) with internal standard quantification. Method validation demonstrated good linearity for all target compounds over the range of 0.1–500 μg·L−1 (R2 > 0.990), with method detection limits ranging from 0.020 to 0.133 ng·g−1. The mean recoveries at low, medium, and high spiking levels ranged from 60.5% to 120.3%, with relative standard deviations (RSDs) of 1.6%–10.7%. The method offers advantages of simple pretreatment, good repeatability, and high accuracy, making it suitable for high-throughput determination of OUVs in complex biological matrices such as corals. The method was applied to analyze 89 coral samples collected from Xidao Island, Sanya, and five target OUVs were detected in the samples. This method provides reliable technical support for elucidating the accumulation characteristics of OUVs in corals and assessing their potential ecological risks.
1. Introduction
Organic ultraviolet absorbents (OUVs) are emerging contaminants widely used in personal care products, sunscreens, plastics, and coatings. Their environmental persistence, bioaccumulation potential, and endocrine-disrupting effects pose significant risks to marine ecosystems, particularly coral reefs. While OUVs have been detected in water, sediment, and biota, existing analytical methods primarily target environmental matrices, leaving a gap in techniques for complex biological tissues such as coral. The high lipid content and diverse matrix components in coral tissues challenge conventional extraction and detection, necessitating a robust and sensitive method for accurate quantification.
This study addresses the bottleneck by developing a UHPLC-MS/MS method with systematic optimization of sample preparation and chromatographic conditions. The sequential extraction using methanol and ethyl acetate, combined with vortexing and ultrasonication, effectively recovers both polar and moderately polar OUVs. The method achieves low detection limits (0.020–0.133 ng·g−1) and high recoveries (60.5%–120.3%) in coral tissue, enabling high-throughput analysis. Application to field samples from Sanya demonstrates its practical utility, providing a reliable tool for monitoring OUV contamination and assessing ecological risks in coral reef ecosystems.
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SU Hao, LIN Jiamin, HU Shanhu, GUO Ziyu, WU Xiaochen, CAO Xiaocong, ZHOU Zhi (2026). Simultaneous Determination of Eleven Organic Ultraviolet Absorbents in Coral by Ultra-High Performance Liquid Chromatography-Mass Spectrometry. Environmental Chemistry. https://doi.org/10.0000/202604-1
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Frequently Asked Questions
What are the method detection limits (MDLs) and quantification limits (MQLs) for the 11 OUVs in coral tissue, and how do they compare to typical environmental concentrations?
The MDLs range from 0.020 to 0.133 ng·g−1, and MQLs from 0.080 to 0.532 ng·g−1. These limits are sufficiently low to detect OUVs at trace levels found in coral tissues, as evidenced by the detection of five OUVs in field samples from Xidao Island.
How was the extraction protocol optimized to ensure high recoveries for a diverse set of OUVs with varying polarities?
We compared single-solvent extraction (methanol or ethyl acetate) versus sequential extraction. The sequential method using 5 mL methanol followed by 5 mL ethyl acetate, combined with vortexing for 20 min and ultrasonication at 30 °C for 20 min, provided the highest and most consistent recoveries (60.5%–120.3%) across all compounds.
What chromatographic conditions were selected to achieve baseline separation of 11 OUVs within a reasonable runtime?
A CAPCELL PAK MG C18 column (5 μm, 2.1 mm × 100 mm) maintained at 40 °C was used with a mobile phase of methanol and 0.1% formic acid aqueous solution under gradient elution. This setup achieved effective separation within 15 minutes at a flow rate of 0.4 mL·min−1 and an injection volume of 5 μL.
How was the method validated in terms of precision and accuracy, and what were the acceptance criteria?
Validation was performed at three spiking levels (1, 10, 50 ng·g−1) with six replicates each. Mean recoveries ranged from 60.5% to 120.3%, with relative standard deviations (RSDs) between 1.6% and 10.7%, meeting the criteria for trace analysis in complex matrices.
What is the practical applicability of this method for large-scale monitoring of OUVs in coral reef ecosystems?
The method was successfully applied to 89 coral samples from Xidao Island, detecting five target OUVs. Its simple pretreatment, good repeatability, and high accuracy make it suitable for high-throughput screening, enabling comprehensive risk assessment of OUV contamination in coral reefs.
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