Malaysian Journal of Analytical Sciences, Vol 28 No 3 (2024): 645 – 663

 

EXPLORING DEEP EUTECTIC SOLVENTS AS A POTENTIAL SOLVENT FOR THE EXTRACTION OF FOOD ADDITIVE ALLURA RED IN FOOD TECHNOLOGY APPLICATION

 

(Mengeksplorasi Pelarut Eutektik Mendalam sebagai Pelarut Berpotensi untuk Pengekstrakan Pewarna Makanan Merah Allura dalam Aplikasi Teknologi Makanan)

 

Thanussha Elangovan1, Nor Munira Hashim1, Nurina Izzah Mohd Husani1, Noorfatimah Yahaya1,

Farhanini Yusoff 2, and Nur Nadhirah Mohamad Zain1*

 

1Department of Toxicology, Advanced Medical, and Dental Institute, Universiti Sains Malaysia, 13200 Kepala Batas, Penang, Malaysia.

2Faculty of Science and Marine Environment, Universiti Malaysia Terengganu, 21030 Kuala Terengganu, Terengganu, Malaysia.

 

*Corresponding author: nurnadhirah@usm.my

 

 

Received: 4 January 2024; Accepted: 16 Apr 2024; Published:  29 June 2024

 

 

Abstract

In recent years, synthetic food dyes have gained significant popularity as additives, replacing natural dyes, with azo dyes comprising approximately 65% of the commercial dye market. However, concerns regarding the toxic effects of azo dyes used in food colouring have prompted the development of advanced analytical methods to detect them in various food matrices. These methods typically involve intricate pre-concentration processes, time-consuming steps, and the use of expensive instruments, thus emphasising the need for highly sensitive and selective approaches. Hence, this study aims to explore the application of deep eutectic solvent (DES) as a potential solvent for the extraction of Allura Red AC (ARAC). First, the synthesised magnetic nanoparticles functionalised with DES (silicone surfactant: dodecanoic acid) (SS: DoAc@Fe3O4) adsorbent was successfully characterised using attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR) for the identification of functional bonds. This adsorbent was subsequently applied in the magnetic solid phase extraction (MSPE) technique to extract ARAC in soft drink samples. In contrast to pure Fe3O4 particles, the targeted ARAC can be easily adsorbed onto the SS: DoAc@Fe3O4 surface due to the formation of strong hydrophobic interaction between ARAC and the adsorbents, thus amplifying the extraction efficiency. Further optimisation was done via one-variable-at-a-time (OVAT) and Taguchi experimental design to determine the optimised condition for ARAC extraction. The OVAT analysis identified that using methanol: acetonitrile (1:1) as the desorption solvent, incorporating Na2SO4 to boost extraction efficiency, employing salt volume of 200 μL, and utilising a sample volume of 20 mL produced the most favourable outcomes. Meanwhile, the Taguchi experiments pinpointed the optimum conditions as pH 2, an adsorbent dosage of 25 mg, an extraction duration of 2 minutes, a desorption period of 3 minutes, and a desorption solvent volume of 400 μL. Under the optimised conditions, the R2 value obtained was 0.999 while the limit of detection (LOD) and limit of quantification (LOQ) values were 0.1 mgL-1 and 0.4 mgL-1, respectively. The studied ARAC also obtained relative recovery values between 80% to 111%. Therefore, it is safe to conclude that the newly proposed SS: DoAc@Fe3O4-based MSPE is an environmentally friendly, simple, affordable, and effective technique for the extraction of ARAC in drink samples.

 

Keywords: Allura red AC, deep eutectic solvents, dodecanoic acid, magnetic solid phase extraction, silicone surfactant

 

Abstrak

Kebelakangan ini, pewarna makanan sintetik semakin popular dan kerap digunakan sebagai bahan tambahan menggantikan pewarna semula jadi, dengan pewarna azo merangkumi kira-kira 65% daripada pasaran pewarna komersial. Walau bagaimanapun, kebimbangan mengenai kesan toksik pewarna azo yang digunakan dalam pewarna makanan telah mendorong pembangunan kaedah analisis lanjutan untuk mengesannya dalam pelbagai matriks makanan. Kaedah tersebut biasanya melibatkan proses pra-kepekatan yang rumit, prosedur yang memakan masa, dan penggunaan instrumen yang mahal, sekaligus menekankan keperluan untuk pendekatan yang sensitif dan terpilih. Oleh itu, kajian ini bertujuan untuk meneroka aplikasi pelarut eutektik mendalam (DES) untuk mengekstrak pewarna merah allura AC (ARAC). Pertama, penjerap zarah nano magnetik difungsikan dengan DES (surfaktan silikon:asid dodekanoik) (SS:DoAc@Fe3O4) telah berjaya disintesis dan dianalisis menggunakan spektroskopi transformasian Fourier inframerah dengan pantulan keseluruhan dikecilkan (ATR-FTIR) untuk mengenal pasti ikatan berfungsi. Bahan penjerap ini kemudiannya digunakan dalam teknik pengekstrakan fasa pepejal magnetik (MSPE) untuk mengekstrak ARAC dalam sampel minuman ringan. Berbeza dengan zarah Fe3O4 tulen, ARAC lebih mudah diserap ke permukaan SS:DoAc@Fe3O4 disebabkan oleh pembentukan interaksi hidrofobik yang kuat antara ARAC dan penjerap, sekaligus menguatkan kecekapan pengekstrakan. Pengoptimuman lanjut kemudiannya dilakukan melalui satu-pembolehubah-pada-satu-masa (OVAT) dan reka bentuk eksperimen Taguchi bagi menentukan keadaan optimum untuk pengekstrakan ARAC. Analisis OVAT mendapati bahawa penggunaan metanol:acetonitrile (1:1) sebagai pelarut penyahjerapan, penambahan garam untuk meningkatkan kecekapan pengekstrakan, penggunaan isipadu garam sebanyak 200 μL, dan penggunaan isipadu sampel 20 mL memberikan hasil yang paling baik. Sementara itu, eksperimen Taguchi menunjukkan keadaan optimum sebagai pH 2, dos penjerap sebanyak 25 mg, tempoh pengekstrakan selama 2 minit, tempoh penyahjerapan selama 3 minit, dan isipadu pelarut penyahjerapan sebanyak 400 μL. Dibawah keadaan yang dioptimumkan, nilai R2 yang diperolehi adalah 0.999 manakala nilai had pengesanan (LOD) dan had kuantifikasi (LOQ) masing-masing adalah 0.1 mgL-1 dan 0.4 mgL-1. ARAC yang dikaji juga memperoleh nilai pemulihan relatif antara 80% hingga 111%. Oleh itu, dapat disimpulkan bahawa MSPE berasaskan SS:DoAc@Fe3O4 yang dicadangkan adalah satu teknik mesra alam, mudah, berpatutan, dan berkesan untuk pengekstrakan ARAC dalam sampel minuman.

 

Kata kunci: Pewarna merah allura AC, pelarut eutektik mendalam, asid dodekanoik, pengekstrakan fasa pepejal magnetik, surfaktan silikon

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