Malaysian Journal of Analytical Sciences, Vol 27 No 5 (2023): 1062 - 1078

 

OPTIMIZATION OF SUNFLOWER OIL HYDROLYSIS USING THE D-OPTIMAL DESIGN

 

(Pengoptimuman Hidrolisis Minyak Bunga Matahari Menggunakan Reka Bentuk D-Optimal)

 

Muhammad Muizzuddin Khairuddin1, Asiah Abdullah1,2, Nur Nadia Dzulkifli1,2, and Nurazira Mohd Nor1,2*

 

1School of Chemistry and Environment,

Faculty of Applied Sciences,

Universiti Teknologi MARA, Cawangan Negeri Sembilan, Kampus Kuala Pilah,

72000 Kuala Pilah, Negeri Sembilan, Malaysia

2Material, Inorganic and Oleochemistry (MaterOleo) Research Group,

Faculty of Applied Sciences,

Universiti Teknologi MARA, Cawangan Negeri Sembilan Kampus Kuala Pilah,

72000 Kuala Pilah, Negeri Sembilan, Malaysia

 

*Corresponding author: nurazira@uitm.edu.my

 

 

Received: 24 May 2023; Accepted: 7 September 2023; Published:  xx October 2023

 

 

Abstract

The hydrolysis process of sunflower oil (SFO) was carried out to produce sunflower oil fatty acids (SFOFAs). The optimization of reaction parameters was performed using response surface methodology (RSM) via D-optimal design. The optimization parameters were varied from 1.0 to 2.5 M molarity of ethanolic KOH, 50 to 70°C of reaction temperature and 0.5 to 2.5 hours of reaction time. The highest percentage of SFOFAs yield was 96.68% with a free fatty acid (FFA) of 103.23%, which was achieved at optimal conditions: 2.3 M ethanolic KOH concentration, reaction temperature of 50.14°C and 0.97 hours of reaction time. The structure of SFO and SFOFAs were confirmed using Fourier Transform Infrared Spectroscopy (FTIR) and Nuclear Magnetic Resonance (NMR). SFOFAs was monitored by the absence of C=O (ester) at 1746.33 cm-1 and the existence of C=O (carboxylic acid) at 1710.23 cm-1 with OH stretching at 2400-3400 cm-1 in SFOFAs FTIR spectrum. Under the NMR spectrum of SFOFAs, the absence peak of ester (C=O) at 172.79 to 173.21 ppm (13C NMR), the emergence peak of OH at 10.61 ppm (1H NMR) and the peak of carbon for carboxylic acid (C=O) (13C NMR) at 180.45 ppm showed that the fatty acid was successfully obtained.

 

Keywords: D-optimal design, hydrolysis, response surface methodology, saponification, sunflower oil

 

Abstrak

Proses hidrolisis minyak bunga matahari (SFO) telah dijalankan untuk menghasilkan asid lemak minyak bunga matahari (SFOFA). Pengoptimuman parameter tindak balas dilakukan menggunakan kaedah permukaan tindak balas (RSM) melalui reka bentuk D-optimal. Parameter pengoptimuman telah diubah daripada 1.0 hingga 2.5 M kemolaran etanol KOH, 50 hingga 70 °C suhu tindak balas dan 0.5 hingga 2.5 jam masa tindak balas. Peratusan tertinggi hasil SFOFAs ialah 96.68% dengan asid lemak bebas (FFA) sebanyak 103.23%, yang dicapai pada keadaan optimum: kepekatan KOH etanol 2.3 M, suhu tindak balas 50.14 °C dan 0.97 jam masa tindak balas. Struktur SFO dan SFOFAs telah disahkan menggunakan spektroskopi infra-merah transformasi Fourier (FTIR) dan resonans magnetik nuklear (NMR). SFOFAs dilihat dengan ketiadaan C=O (ester) pada 1746.33 cm-1 dan kewujudan C=O (asid karboksilik) pada 1710.23 cm-1 dengan regangan OH pada 2400-3400 cm-1 dalam spektrum FTIR SFOFAs. Di bawah spektrum NMR SFOFAs, kehilangan puncak ester (C=O) pada 172.79 hingga 173.21 ppm (13C NMR), kemunculan puncak OH pada 10.61 ppm (1H NMR) dan puncak karbon untuk asid karboksilik (C=O) (13C NMR) pada 180.45 ppm menunjukkan bahawa asid lemak berjaya diperolehi.

 

Kata kunci: reka bentuk D-optimal, hidrolisis, kaedah permukaan tindak balas, penyabunan, minyak bunga matahari

 

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