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Extraction and preconcentration of residual solvents from herbal medicines by headspace-micro solid phase extraction combined with deep eutectic solvent-based dispersive liquid–liquid microextraction

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Abstract

In this study, a headspace-micro solid phase extraction method combined with dispersive liquid–liquid microextraction was utilized in the extraction of residual solvents from herbal-based medicine samples. A home-made extraction device was used for headspace-micro solid phase extraction by transferring a proper amount of the samples into the device and adsorption of the analytes onto octadecylsilane from the headspace of sample solution. The adsorbed analytes were eluted by dimethylformamide. The eluate was mixed with a few microliters of tetrabutylammonium chloride: p-aminophenol: linalool deep eutectic solvent [1:1:1, mol: mol: mol]. It was used in the microextraction step to preconcentrate the analytes. The enriched analytes were determined by gas chromatography equipped with flame ionization detector. Under optimized conditions, the method validation was done by International Council of Harmonization protocol and the limits of detection and quantification were in the ranges of 0.81–1.2 and 2.8–4.1 ng g−1, respectively. Wide linearity was obtained with a correlation coefficient ≥ 0.994 for the calibration curves. Relative standard deviation values for the repeated analyses in the same day (n = 6) and different days (n = 4) were ≤ 4.9% at a concentration of 5.0 ng g−1 of each analyte. The method was successful in determination of the analytes in herbal medicines at trace levels (ng g−1).

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Abbreviations

ChCl:

Choline chloride

RS:

Residual solvent

LOD:

Limit of detection

FID:

Flame ionization detector

DLLME:

Dispersive liquid–liquid microextraction

HS-µSPE:

Headspace-micro solid phase extraction

TBAC:

Tetrabutylammonium chloride

ER:

Enrichment factor

LOQ:

Limit of quantification

GC:

Gas chromatography

RSD:

Relative standard deviation

ODS:

Octadecylsilane

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Funding

The funding was provided by Tabriz University of Medical Sciences as the grant number of 64800.

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Authors and Affiliations

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

    Alireza Hassani Aliabad

  2. Food and Drug Safety Research Center, Tabriz University of Medical Sciences, Tabriz, Iran

    Alireza Hassani Aliabad & Mohammad Reza Afshar Mogaddam

  3. Pharmaceutical Analysis Research Center, Tabriz University of Medical Sciences, Tabriz, Iran

    Mohammad Reza Afshar Mogaddam

  4. Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz, Iran

    Mir Ali Farajzadeh

  5. Engineering Faculty, Near East University, 99138, North Cyprus, Mersin 10, Nicosia, Turkey

    Mir Ali Farajzadeh

Authors
  1. Alireza Hassani Aliabad
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  2. Mohammad Reza Afshar Mogaddam
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  3. Mir Ali Farajzadeh
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Corresponding author

Correspondence to Mohammad Reza Afshar Mogaddam.

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Hassani Aliabad, A., Afshar Mogaddam, M.R. & Farajzadeh, M.A. Extraction and preconcentration of residual solvents from herbal medicines by headspace-micro solid phase extraction combined with deep eutectic solvent-based dispersive liquid–liquid microextraction. J IRAN CHEM SOC 20, 1039–1048 (2023). https://doi.org/10.1007/s13738-022-02723-4

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