Method Validation for the Determination of D-psicose in Raisins Using Ultrasound-assisted Extraction Coupled with Ionic Chromatography

Fahmi Maulana Zulkarnaen, Dr. Widiastuti Setyaningsih, S.T.P., M.Sc. ; Prof. Miguel Palma Lovillo

2022 | Tesis | MAGISTER ILMU DAN TEKNOLOGI PANGAN

D-psicose adalah gula rendah kalori yang dapat digunakan sebagai alternatif sukrosa karena memiliki 70% rasa manis sukrosa tetapi penyerapan kalori rendah dalam tubuh manusia. Mempertimbangkan efek menguntungkan dari D-psicose dan ketersediaannya yang tinggi dalam matriks kismis sebagai buah kering yang paling banyak dikonsumsi di dunia, menarik untuk membawa metode analisis yang andal untuk menentukan kandungan D-psicose dalam kismis, terutama ketika sejumlah besar sampel harus ditentukan per hari. Di sini metode baru untuk menentukan D-psicose dalam kismis komersial menggunakan ekstraksi berbantuan ultrasound (UEA) dalam hubungannya dengan kromatografi pertukaran anion telah dikembangkan dan divalidasi. Stabilitas D-psicose dan pendahulunya sebelumnya dinilai dengan menentukan efek daya UEA tertentu (100 W) dan siklus tugas pulsa (0,5/s) dengan suhu ekstraksi yang bervariasi (10, 25, 40, 55, 70, dan 85 C) dan kali (5, 10, 15, 20, dan 25 menit). D-psicose ditentukan dalam ekstrak menggunakan kromatografi pertukaran anion berkinerja tinggi yang dipasangkan dengan sistem deteksi amperometrik berdenyut (HPAEC-PAD). Metode ini divalidasi dengan linearitas tinggi (R2>0,999), akurasi (89,78-101,06%), dan presisi (4,8% intra-hari dan 4,34% antar-hari). Sejumlah produk kismis diperiksa selama penilaian penerapan metode. Konsentrasi setinggi 520 mg/kg ditemukan dalam sampel kismis komersial.

D-psicose is a low-calorie sugar that can be used as an alternative to sucrose because it has 70% sweetness of sucrose but low absorption of calories in the human body. Considering the beneficial effects of D-psicose and its high availability in the raisin matrix as the most widely consumed dried fruit in the world, it is interesting to bring a reliable analytical method to determine the D-psicose content in raisins, especially when a large number of samples has to be determined per day. Here a new method for determining D-psicose in commercial raisins using ultrasound-assisted extraction (UAE) in conjunction with anion exchange chromatography has been developed and validated. The stability of D-psicose and its prior predecessors was assessed by determining the specific UAE power effect (100 W) and pulse duty cycle (0.5/s) with varying extraction temperatures (10, 25, 40, 55, 70, and 85 C) and times (5, 10, 15, 20, and 25 minutes). D-psicose was determined in extracts using high-performance anion-exchange chromatography coupled to a pulsed amperometric detection system (HPAEC-PAD). This method was validated with high linearity (R2>0.999), accuracy (89.78-101.06%), and precision (4.8% intra-day and 4.34% between-day). A number of raisin products were examined during the method applicability assessment. Concentrations as high as 520 mg/kg were found in commercial raisin samples.

Kata Kunci : D-psicose; fructose; high-performance anion exchange chromatography; pulsed amperometric detection; rare sugar.