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Combination of headspace solid phase extraction with lighter than water organic solvent-based dispersive liquid-liquid microextraction for the extraction of residual solvents from herbal laxative medicine prior to gas chromatography-flame ionization detection

Alireza Hassani Aliabad, Farnaz Monajjemzadeh, Mohammad Reza Afshar Mogaddam, and Mir Ali Farajzadeh

Department of Pharmaceutical and Food Control , Faculty of Pharmacy, Tabriz University of Medical Sciences, Tabriz, Iran



Received: 23 February 2022  Accepted: 15 June 2022


A combined headspace solid phase extraction-dispersive liquid–liquid microextraction method was developed for the extraction of residual solvents (dichloromethane, chloroform, methanol, ethanol, acetone, 2-propanol, 1-butanol, tetrahydrofuran, and pyridine) from herbal laxative medicines. The headspace solid phase extraction procedure was performed by a home-made device. For this purpose, the sample was placed into the extraction device and after dilution with sodium chloride solution, the analytes were forced to inter the headspace of samples and adsorbed onto the sorbent. After extraction, the analytes were eluted by a suitable solvent and more concentrated by a lighter than water organic solvent-based dispersive liquid–liquid microextraction. The enriched analytes were determined by gas chromatography-flame ionization detector. The validation parameters confirmed good sensitivity (limits of detection, 0.59–0.94 ng g−1) and repeatability (relative standard deviations, ≤ 3.9%), broad linear ranges and high extraction recovery (89–98%). The method was successful used in determination of the analytes in herbal laxative medicines and only methanol and dichloromethane were found in three samples.

Keywords: Headspace solid phase extraction; Gas chromatography; Residual solvent; Dispersive liquid–liquid microextraction; Herbal medicines

Full paper is available at

DOI: 10.1007/s11696-022-02332-8


Chemical Papers 76 (10) 6451–6460 (2022)

Monday, June 17, 2024

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