An In Situ Dansylation Ultrasound-Assisted Dispersive Liquid-Liquid Microextraction Based on Ionic Liquid for Determination of Biogenic Amines in Foods

  • Solehatun Mhd Bani
  • Mardiana SaaidEmail author
  • Bahruddin Saad


An in situ derivatization combined with ionic liquid-based ultrasound-assisted dispersive liquid-liquid microextraction (IL-USADLLME) method was developed for the extraction of seven biogenic amines (BAs) namely putrescine, cadaverine, histamine, tryptamine, tyramine, spermidine, and spermine in foods. BAs were derivatized in situ with dansyl chloride and 1-butyl-3-methylimidazolium hexafluorophosphate, [C4MIM][PF6] (extraction solvent) was dispersed into the aqueous sample solution as fine droplets by ultrasonication. Acetonitrile was used as a disperser solvent. Factors affecting the extraction efficiency, such as the dansylation conditions, volume of ionic liquid, ultrasonication time, and extraction temperature have been optimized. BAs were analyzed using C18 monolithic column of high performance liquid chromatography coupled with diode array detector after the extraction and centrifugation. The proposed method was linear over 1–100 mg/L with a correlation coefficient of 0.9871–0.9992. The limit of detection and quantification based on signal to noise ratio of 3 and 10 ranges from 0.06 to 0.3 mg/L and 0.19 to 0.99 mg/L, respectively. The relative standard deviations (RSDs) for intra-day and inter-day assay were less than 3.6%. Relative recoveries ranging from 70.7-118.4% were established using mango juice, local delicacies (tempe, budu), and canned sardine fish samples with %RSD less than 5.5%. The developed method was eco-friendly and was found to be sensitive, rapid, and cost-effective for the determination of BAs in a wide range of food sample matrices.


Biogenic amines In situ dansylation Ionic liquid HPLC 



This work was conducted at Faculty of Applied Sciences, Universiti Teknologi MARA, Shah Alam, Selangor. We thank Mr. Mohamad Shukri Kamarudin for the material supplied.

Funding Information

This study was funded by a Fundamental Research Grant Scheme (FRGS) (Grant no: 600-RMI/ST/FRGS 5/3/Fst (13/2010)) of the Ministry of Higher Education Malaysia.

Compliance with Ethical Standards

Conflict of Interest

Mardiana Saaid declares that she has no conflict of interest. Solehatun Md Bani declares that she has no conflict of interest. Bahruddin Saad declares that he has no conflict of interest.

Ethical Approval

This article does not contain any studies with human participants or animals performed by any of the authors.

Informed Consent

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 2019

Authors and Affiliations

  1. 1.Faculty of Applied SciencesUniversiti Teknologi MARAShah AlamMalaysia
  2. 2.School of Chemical SciencesUniversiti Sains MalaysiaPulau PinangMalaysia
  3. 3.Fundamental and Applied Sciences DepartmentUniversiti Teknologi PETRONASPerak Darul RidzuanMalaysia

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