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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

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Abstract

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.

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Abbreviations

RS :

Residual solvent

GC :

Gas chromatography

DLLME :

Dispersive liquid–liquid microextraction

FID :

Flame ionization detector

HS-SPE :

Headspace solid phase extraction

RSD :

Relative standard deviation

ER :

Enrichment recovery

LOD :

Limit of detection

LOQ :

Limit of quantification

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Acknowledgements

The authors express their thanks to the Research Council of Tabriz University of Medical Science for financial support as grant number of 64800.

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Correspondence to Farnaz Monajjemzadeh or Mohammad Reza Afshar Mogaddam.

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Hassani Aliabad, A., Monajjemzadeh, F., Afshar Mogaddam, M. et al. 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. Chem. Pap. 76, 6451–6460 (2022). https://doi.org/10.1007/s11696-022-02332-8

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