Food Analytical Methods

, Volume 12, Issue 2, pp 489–502 | Cite as

Ultrasound-Assisted Low-Density Solvent-Based Dispersive Liquid–Liquid Microextraction Coupled to Spectrophotometry for the Determination of Low Levels of Histamine in Fish and Meat Products

  • Adil Elik
  • Nail AltunayEmail author
  • Ramazan Gürkan


In this study, a new low-density solvent-based dispersive liquid–liquid microextraction strategy coupled to spectrophotometry has been developed for the determination of the trace levels of histamine in fish and meat products. The method is based on the formation of a charge transfer complex between a histamine and a phenothiazine group dye, promethazine (PMZ) in the presence of greener ionic liquid (IL), 1-butyl-3-methylimidazilium octylsulfate, C4mim octylOSO3, exhibiting a surfactant-like micellar behavior at pH 7.0, and then microextraction of the complex into the floating organic drops of 1-heptanol, which is water-immiscible and lighter than water. Ultrasound or sonication was used to improve the microextraction efficiency as well as to reduce the analysis time and cost. Variables affecting the microextraction efficiency were evaluated and optimized. Under optimal conditions, a calibration plot, which is prepared from solvent-based calibration solutions, was linear in the range of 5–750 μg L−1, with a sensitivity enhancement of 95-fold. In addition, the satisfactory extraction recoveries ranging from 95.2 to 102.8% were obtained. The method has been found to have excellent detection sensitivity, with a detection limit of 1.35 μg L−1 and intra- and inter-day precisions of 3.5–5.6% (as RSDs; n, 5 and 3 × 5). A preconcentration factor of 107-fold from the preconcentration of a 75-mL sample was obtained. The method was statistically validated by analysis of two quality control samples, including accuracy and precision studies after spiking. The method may be accepted as a simple, easy-to-use, low-cost, fast, sensitive, accurate, and reliable approach, even better than conventional DLLME and similar techniques. The results indicated that this methodology was suitable for the analysis of low levels of histamine in selected food matrices.


Histamine Low-density solvent-based dispersive liquid–liquid microextraction Ultrasound Fish and meat products Spectrophotometry 



This study was supported by Cumhuriyet University Scientific Research Projects Commission as the research projects with the F-535 code.

Compliance with Ethical Standards

The authors have no financial relationship with the organization that sponsored the research.

Conflict of Interest

Adil Elik declares that he has no conflict of interest. Nail Altunay declares that he has no conflict of interest. Ramazan Gürkan declares that he has no conflict of interest.

Ethical Approval

This article does not contain any studies with human or animal subjects.

Informed Consent

On behalf of other authors, informed consent was obtained from all individual participants included in the study.


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© Springer Science+Business Media, LLC, part of Springer Nature 2018

Authors and Affiliations

  1. 1.Department of Chemistry, Faculty of SciencesCumhuriyet UniversitySivasTurkey

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