Malays. J. Anal. Sci. Volume 29 Number 5 (2025): 1636

 

Research Article

 

Headspace micro-solid phase extraction of pyrene in tea infusions and beverages

 

Chang Sen Chai1, Wan Mohd Afiq Wan Mohd Khalik1,2, Hafiza Mohamed Zuki1, and Saw Hong Loh1*

 

1Faculty of Science and Marine Environment, Universiti Malaysia Terengganu, 21030 Kuala Nerus, Terengganu, Malaysia

2Water Analysis Research Centre, Faculty of Science and Technology, Universiti Kebangsaan Malaysia, 43600 Bangi, Selangor, Malaysia

 

*Corresponding author: lohsh@umt.edu.my

 

Received: 31 July 2025; Revised: 18 September 2025; Accepted: 23 September 2025; Published: 16 October 2025

 

Abstract

Tea is a significant beverage in many cultures and often serves a purpose beyond mere consumption. However, pyrene raises concerns regarding lung health and cancer risks for humans. Therefore, a sensitive and environmentally friendly headspace micro-solid phase extraction (Hs-μ-SPE) combined with fluorescence spectrophotometry (Fs) was examined and evaluated for analysing pyrene in tea infusions and beverages. The extraction of pyrene was performed using a commercial adsorbent termed MonotrapTM. Microextraction parameters, such as extraction temperature, extraction time, stirring rate, type of desorption solvent, desorption time, and volume of desorption solvent, were investigated and optimised. The limit of detection (LOD) and limit of quantification (LOQ) of Hs-μ-SPE-Fs for determining pyrene were 12 and 15 µg L-1, respectively, indicating the method's high sensitivity, despite the absence of chromatography instrumentation. A negligible matrix effect was observed, as indicated by the relative recovery of pyrene from spiked tea infusions and beverages, which ranged from 77.9 to 99.9%. Pyrene, at concentrations ranging from 29 to 99 µg L-1, was detected in some commercially available tea infusions and beverages, potentially posing a health risk to regular consumers. The environmental impact of Hs-μ-SPE-Fs was then assessed using the analytical greenness metric for sample preparation (AGREEprep), a tool designed to evaluate the sustainability and environmental friendliness of sample preparation methods. With a total AGREEprep score of 0.61, the proposed Hs-μ-SPE-Fs method demonstrated above-average environmental performance. However, further improvements could be performed in areas such as on-site applicability and the use of renewable materials. Despite these limitations, the method offers a sensitive and accurate approach for detecting pyrene in tea infusions and beverages that is beneficial to tea lovers.

 

Keywords: AGREEprep, fluorescence, μ-SPE, PAH, tea

 

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