TY - JOUR

T1 - Vacuum-assisted headspace solid-phase microextraction in food analysis

T2 - basics and applications

AU - Syrgabek, Yerkanat

AU - Alimzhanova, Mereke

AU - Haque, Shaikh Manirul

AU - Psillakis, Elefteria

AU - Fuente-Ballesteros, Adrián

N1 - Publisher Copyright: © 2025 Elsevier B.V.

PY - 2026/2/8

Y1 - 2026/2/8

N2 - Background: Vacuum-assisted headspace solid-phase microextraction (Vac-HSSPME) is increasingly recognized as a powerful and environmentally friendly technique for extracting volatile and semi-volatile compounds from complex food matrices. While conventional HSSPME has been widely applied, its limitations in extracting low-volatility and matrix-bound compounds have spurred interest in vacuum-assisted approaches. In this review, we provide a comprehensive summary of Vac-HSSPME basics, applications, and limitations in food analysis. Results: This review evaluates recent advances and applications of Vac-HSSPME across seven main food categories: (i) dairy products; (ii) edible oils and fats; (iii) honey; (iv) meat, fish, and high-protein samples; (v) fruits and vegetables; (vi) beverages and drinking water; and (vii) grains and plant-based products. Compared to conventional HSSPME, vacuum conditions consistently improve detection limits, extraction efficiency, and analyte coverage. Key operational parameters, including extraction time, temperature, sample volume, agitation, and vacuum level, are discussed in relation to their influence on performance and matrix effects. The review also highlights persistent challenges such as analyte losses during vacuum application, pronounced matrix effects in viscous samples, and the need for careful optimization. Recent developments in SPME fiber materials, automation, and coupling with high-resolution mass spectrometry are expanding the technique's applicability and analytical throughput. Moreover, the integration of machine learning offers promising avenues for optimizing conditions and predicting analyte behavior based on sample characteristics. Significance: Vac-HSSPME is expected to gain wider adoption in food, environmental, and pharmaceutical analysis, supporting high-throughput, sensitive, and green analytical workflows. This review provides an up-to-date perspective of Vac-HSSPME's advantages, limitations, and emerging perspectives in the context of food analysis.

AB - Background: Vacuum-assisted headspace solid-phase microextraction (Vac-HSSPME) is increasingly recognized as a powerful and environmentally friendly technique for extracting volatile and semi-volatile compounds from complex food matrices. While conventional HSSPME has been widely applied, its limitations in extracting low-volatility and matrix-bound compounds have spurred interest in vacuum-assisted approaches. In this review, we provide a comprehensive summary of Vac-HSSPME basics, applications, and limitations in food analysis. Results: This review evaluates recent advances and applications of Vac-HSSPME across seven main food categories: (i) dairy products; (ii) edible oils and fats; (iii) honey; (iv) meat, fish, and high-protein samples; (v) fruits and vegetables; (vi) beverages and drinking water; and (vii) grains and plant-based products. Compared to conventional HSSPME, vacuum conditions consistently improve detection limits, extraction efficiency, and analyte coverage. Key operational parameters, including extraction time, temperature, sample volume, agitation, and vacuum level, are discussed in relation to their influence on performance and matrix effects. The review also highlights persistent challenges such as analyte losses during vacuum application, pronounced matrix effects in viscous samples, and the need for careful optimization. Recent developments in SPME fiber materials, automation, and coupling with high-resolution mass spectrometry are expanding the technique's applicability and analytical throughput. Moreover, the integration of machine learning offers promising avenues for optimizing conditions and predicting analyte behavior based on sample characteristics. Significance: Vac-HSSPME is expected to gain wider adoption in food, environmental, and pharmaceutical analysis, supporting high-throughput, sensitive, and green analytical workflows. This review provides an up-to-date perspective of Vac-HSSPME's advantages, limitations, and emerging perspectives in the context of food analysis.

KW - Food analysis

KW - Green analytical chemistry

KW - Headspace solid-phase microextraction

KW - Sustainable sample preparation

KW - Vac-HSSPME

KW - Vacuum-assisted headspace solid-phase microextraction

KW - Chemistry

UR - https://www.scopus.com/pages/publications/105023484887

U2 - 10.1016/j.aca.2025.344939

DO - 10.1016/j.aca.2025.344939

M3 - Scientific review articles

C2 - 41545131

AN - SCOPUS:105023484887

VL - 1386

JO - Analytica Chimica Acta

JF - Analytica Chimica Acta

SN - 0003-2670

M1 - 344939

ER -