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Accelerated solvent extraction combined with solid phase extraction for the determination of organophosphate esters from sewage sludge compost by UHPLC–MS/MS

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Abstract

Organophosphate esters (OPEs), widely used as flame retardants and plasticizers, are regarded as emerging pollutants. OPEs are prone to concentrate into residual activated sludge, which might cause secondary pollution if not suitably treated. Composting is an economical and effective approach to make sewage sludge stable and harmless. Therefore, it is essential to develop a novel method for analyzing OPEs in sewage sludge compost samples. However, in the composting process, large amounts of amendments are doped into the sludge to adjust the carbon-nitrogen ratio. Amendment has a strong capacity for adsorption and thus induces a decrease of extraction efficiency. This study developed a novel procedure for determining OPEs in compost samples. Accelerated solvent extraction (ASE) and solid phase extraction (SPE) were used for extracting and concentrating the OPEs from sewage sludge compost samples, and then analyzed by UHPLC–MS/MS. Some parameters were optimized in this study, mainly including the extraction solvent type, extraction temperature, static extraction time, extraction cycles, and flush volume. Under the optimal conditions, the proposed method showed good linearity between 0.50 and 100 μg kg−1 with regression coefficients in the range of 0.9984–0.9998. Detection limits were in the range of 0.02–3 μg kg−1 with standard deviations ranging from 2 to 6%. Acceptable recoveries between 56 and 119% for samples spiked at different concentration levels were achieved. In contrast, the recoveries merely ranged from 24 to 58% by using ultrasonic-assisted extraction.

A comparison of recoveries between ultrasonic-assisted extraction (UAS) and accelerated solvent extraction (ASE) for organophosphate esters from sewage sludge compost samples

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Acknowledgments

This study was supported by the Open foundation Major Science and Technology Program for Water Pollution Control and Treatment (2015ZX07204-002-003), Collaborative Innovation Center of Environmental Pollution Control and Ecological Restoration, Henan Province (XTCX-010), and Major Science Program for University of Henan Province (15A180063).

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Authors and Affiliations

  1. Department of Material and Chemical Engineering, Collaborative Innovation Center of Environmental Pollution Control and Ecological Restoration, Zhengzhou University of Light Industry, Zhengzhou, Henan, 450001, China

    Long Pang, Peijie Yang, Liming Ge, Jingjing Du & Hongzhong Zhang

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  1. Long Pang
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  2. Peijie Yang
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  3. Liming Ge
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Correspondence to Long Pang.

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Pang, L., Yang, P., Ge, L. et al. Accelerated solvent extraction combined with solid phase extraction for the determination of organophosphate esters from sewage sludge compost by UHPLC–MS/MS. Anal Bioanal Chem 409, 1435–1440 (2017). https://doi.org/10.1007/s00216-016-0078-8

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