Development of an Effective Method for the Determination of p-Hydroxybenzoic Acid Esters (Parabens) in Sediment

Dao Duy Anh, Ta Thuy Nguyen, Nguyen Nu Ha My, Chu Ngoc Chau, Dang Van Long, Hoang Quoc Anh, Tu Binh Minh, Tran Manh Tri

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Published Nov 10, 2025
DOI: https://doi.org/10.25073/2588-1140/vnunst.5870

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ANH, Dao Duy et al. Development of an Effective Method for the Determination of p-Hydroxybenzoic Acid Esters (Parabens) in Sediment. VNU Journal of Science: Natural Sciences and Technology, [S.l.], nov. 2025. ISSN 2588-1140. Available at: <https://js.vnu.edu.vn/NST/article/view/5870>. Date accessed: 27 nov. 2025. doi: https://doi.org/10.25073/2588-1140/vnunst.5870.
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Abstract

This study developed a method for the simultaneous determination of seven paraben compounds in sediment samples using liquid chromatography-tandem mass spectrometry (LC-MS/MS) combined with solid-phase extraction (SPE). Parabens were separated on a C18-column (Kinetex: 150 mm x 2.1 mm, 2.6 µm), with mobile phases (A): 0.05% acetic acid and (B): methanol. One hundred nanograms of each surrogate standard (13C-MeP and 13C-BuP) were added to 500 mg of dried sediment sample. Parabens were then ultrasonically extracted for 10 min with 5 mL of methanol/acetonitrile (1/1, v/v) acidified to pH~3 with formic acid. The sample was centrifuged at 4500 rpm for 5 min, and the supernatant was transferred to a glass tube. The extraction procedure was repeated twice. The extracted solution were then concentrated to ~1.5 mL under a gentle stream of nitrogen. The sample was then added with 10 mL of ultrapure water and passed through an SPE column (Oasis HLB 500 mg), which had been activated respectively with 3 mL of methanol and 3 mL of ultrapure water. The target compounds were eluted with 5 mL of methanol. The eluted solution was concentrated to 1 mL under a stream of nitrogen. The final solution was filtered through a Whatman filter paper (pore size: 0.2 µm) and analyzed on an LC-MS/MS instrument. Calibration curves of the native compounds were constructed in the concentration range of 0.5–200 ng/mL (R2 > 0.997). The recoveries of the surrogate standards (13C-MeP and 13C-BuP) were in the range of 85.5–105% (RSD < 9.5%) and 88.0–110% (RSD < 8.0%), respectively. The method detection limits of parabens in sediment samples ranged from 0.027 to 0.067 ng/g. The standardized method was applied to determine the distribution of parabens in sediment samples collected from To Lich River, Hanoi. Total concentrations of parabens in sediment samples ranged from 12.5 to 81.9 ng/g.

Keywords: Parabens; LC-MS/MS; SPE; Sediment

References

[1] Q. Zhu, J. Jia, Y. Wang, K. Zhang, H. Zhang, C. Liao, G. Jiang, Spatial distribution of parabens, triclocarban, triclosan, bisphenols, and tetrabromo bisphenol A and its alternatives in municipal sewage sludges in China, Sci. Total Environ. Vol. 679, 2019, 61–69. https://doi.org/10.1016/j.scitotenv.2019.05.059.
[2] D. A. Brose, K. Kumar, A. Liao, L. S. Hundal, G. Tian, A. Cox, H. Zhang, E. W. Podczerwinski, A reduction in triclosan and triclocarban in water resource recovery facilities’ influent, effluent, and biosolids following the U.S. Food and Drug Administration’s 2013 proposed rulemaking on antibacterial products, Water Environ. Res. Vol. 91, 2019, 715–721. https://doi.org/10.1002/wer.1101.
[3] X. Xu, Y. Xu, N. Xu, B. Pan, J. Ni, Pharmaceuticals and personal care products (PPCPs) in water, sediment and freshwater mollusks of the Dongting Lake downstream the Three Gorges Dam, Chemosphere Vol. 301, 2022, 134721. https://doi.org/10.1016/j.chemosphere.2022.134721.
[4] A. C. Johnson, R. L. Donnachie, J. P. Sumpter, M. D. Jurgens, C. Moeckel, M. G. Pereira, An alternative approach to risk rank compounds on the threat they pose to the aquatic environment, Sci. Total Environ. Vol. 599–600, 2017, 1372–1381. https://doi.org/10.1016/j.scitotenv.2017.05.039.
[5] Y. Wang, D. Cun, Z. Zhang, D. Pu, X. Li, W. Liang, T. Fang, Occurrence and risk assessment of triclosan in freshwater lakes in the middle Yangtze River basin (Wuhan, Central China), Water Biol. Secur. Vol. 1, 2022, 100063. https://doi.org/10.1016/j.watbs.2022.100063.
[6] J. Feng, J. Zhao, N. Xi, W. Guo, J. Sun, Parabens and their metabolite in surface water and sediment from the Yellow River and the Huai River in Henan Province: Spatial distribution, seasonal variation and risk assessment, Ecotoxicol. Environ. Saf. Vol. 172, 2019, 480–487. https://doi.org/10.1016/j.ecoenv.2019.01.102.
[7] A. R. Wahab, T. F. T. Omar, Y. M. Nurulnadia, A. N. N. Rozulan, Occurrence, distribution, and risk assessment of parabens in the surface water of Terengganu River, Malaysia, Mar. Pollut. Bull. Vol. 192, 2023, 115036. https://doi.org/10.1016/j.marpolbul.2023.115036.
[8] N.B. Bolujoko, O. O. Ogunlaja, M. O. Alfred, D. M. Okewole, A. Ogunlaja, O. D. Olukanni, T. A. M. Msagati, E. I. Unuabonah, Occurrence and human exposure assessment of parabens in water sources in Osun State, Nigeria, Sci. Total Environ. Vol. 814, 2022, 152448. https://doi.org/10.1016/j.scitotenv.2021.152448.
[9] G. Nandikes, P. Pathak, A. S. Razak, V. Narayanamurthy, L. Singh, Occurrence, environmental risks and biological remediation mechanisms of triclosan in wastewaters: Challenges and perspectives, J. Water Process Eng. 2022, 49, 103078. https://doi.org/10.1016/j.jwpe.2022.103078.
[10] M. J. S. Chaves, S. C. Barbosa, M. M. Malinowski, D. Volpato, I. B. Castro, T. Franco, E. G. Primel, Pharmaceuticals and personal care products in a Brazilian wetland of international importance: Occurrence and environmental risk assessment, Sci. Total Environ. Vol. 734, 2020, 139374. https://doi.org/10.1016/j.scitotenv.2020.139374.
[11] P. Kumkar, C. R. Verma, S. Hysek, M. Pise, S. Zoltowska, S. M. Gosavi, F. Mercl, M. Božik, L. Praus, K. Hanková, R. Rinn, P. Kloucek, M. Petrtyl, L. Kalous, Contaminants and their ecological risk assessment in beach sediments and water along the Maharashtra coast of India: A comprehensive approach using microplastics, heavy metal(loid)s, pharmaceuticals, personal care products and plasticizers, Sci. Total Environ. Vol. 892, 2023, 164712. http://dx.doi.org/10.1016/j.scitotenv.2023.164712.
[12] D. Sadutto, V. Andreu, T. Ilo, J. Akkanen, Y. Pico, Pharmaceuticals and personal care products in a Mediterranean coastal wetland: Impact of anthropogenic and spatial factors and environmental risk assessment, Environ. Pollut. Vol. 271, 2021, 116353. https://doi.org/10.1016/j.envpol.2020.116353.
[13] T. M. Tran, M. B. Tu, K. A. Taha, K. Kannan, Occurrence of phthalate diesters (phthalates), p-hydroxybenzoic acid esters (parabens), bisphenol A diglycidyl ether (BADGE) and their derivatives in indoor dust from Vietnam: Implications for exposure, Chemosphere, Vol. 144, 2016, 1553–1559. https://doi.org/10.1016/j.chemosphere.2015.10.028.
[14] A. Q. Hoang, M. B. Tu, S. T. Nguyen, N. M. T. Le, T. M. Tran, H. D. Phung, K. Kannan, Determination and risk assessment of p-hydroxybenzoate esters (parabens) in indoor dust from some northern cities in Vietnam, J. Anal. Sci. Vol. 31, No. 3, 2016, 109–115.
[15] T. M. Tran, T. L. T. Thien, M. T. H. Hang, B. T. H. Lan, N. N. M Ha, T. T. Hue, D. T. Lieu, M. B. Tu, Q. C. Thuy, H. Q. Anh, Parabens in personal care products and indoor dust from Hanoi, Vietnam: Temporal trends, emission sources, and non-dietary exposure through dust ingestion, Sci. Total Environ. Vol. 761, 2021, 143274. https://doi.org/10.1016/j.scitotenv.2020.143274.
[16] T. M. Le, P. T. Phuong, N. Q. Truong, N. Q. Trung, B. Q. Minh, N. Q. Hoa, V. D. Nam, K. Kannan, T. M. Tran, A survey of parabens in aquatic environments in Hanoi, Vietnam and its implications for human exposure and ecological risk, Environ. Sci. Pollut. Res. Vol. 29, 2022, 46767–46777. https://doi.org/10.1007/s11356-022-19254-3.
[17] P. T. Phuong, Q. C. Thuy, L. T. Quynh, B. Q. Minh, A. H. Tran, A. T. T. Phung, A. Q. Hoang, M. B. Tu, T. L. T. Thien, H. N. Tran, T. M. Tran, Quantification of parabens in marine fish samples by a rapid, simple, effective sample preparation method, Environ. Sci. Pollut. Res. Vol. 31, No. 11, 2024, 16571–16582. https://doi.org/10.1007/s11356-024-32321-1.
[18] Y. Guo, L. Wang, K. Kannan, Phthalates and parabens in personal care products from China: Concentrations and human exposure, Arch. Environ. Contam. Toxicol. Vol. 66, 2014, 113–119. https://doi.org/10.1007/s00244-013-9937-x.
[19] T. Wu, X. Li, Z. Zheng, Z. Liu, M. Yang, N. Zhang, J. Cui, B. Zhang, Hexabromocyclododecanes in surface soil-maize system around Baiyangdian Lake in North China: Distribution, enantiomer-specific accumulation, transport, temporal trend and dietary risk, J. Hazard. Mater. Vol. 451, 2023, 131180. https://doi.org/10.1016/j.jhazmat.2023.131180.
[20] C. M. Gopal, K. Bhat, B. R. Ramaswamy, V. Kumar, R. K. Singhal, H. Basu, H. N. Udayashankar, S. G. Vasantharaju, Y. Praveenkumarreddy, Y. Lino, K. Balakrishna, Seasonal occurrence and risk assessment of pharmaceutical and personal care products in Bengaluru rivers and lakes, India, J. Environ. Chem. Eng. Vol. 9, 2021, 105610. https://doi.org/10.1016/j.jece.2021.105610.