Malaysian Journal of Analytical Sciences, Vol 27 No 2 (2023): 271 - 279

 

DETERMINING NEREISTOXIN RESIDUE IN PALM OIL MATRIX – AN EXTENSION TO THE METHOD FOR THIOSULTAP DISODIUM RESIDUE DETERMINATION

(Penentuan Sisabaki Nereistoxin Dalam Matriks Minyak Sawit – Penambahan Kepada Kaedah Penentuan Sisabaki Thiosultap Disodium)

 

Chee Beng Yeoh*, Farah Khuwailah Ahmad Bustamam, Najwa Sulaiman, Mei Huey Saw,

and Nik Sasha Khatrina Khairuddin

Malaysian Palm Oil Board,

6 Persiaran Institusi, Bandar Baru Bangi, 43000 Kajang, Selangor, Malaysia


*Corresponding author: cbyeoh@mpob.gov.my

 

 

Received: 27 July 2022; Accepted: 17 January 2023; Published:  19 April 2023

 

 

Abstract

This study aimed to incorporate the nereistoxin, a compound that is the major metabolite of all nereistoxin analogue pesticides, including thiosultap-disodium into the previously reported analytical method developed for thiosultap-disodium residue analysis in the palm oil matrix. All steps that have been developed previously for the determination of thiosultap-disodium involving liquid-liquid extraction and subsequently determination using liquid chromatograph triple quadrupole mass spectrometer (LC-MS/MS) were followed, except the omission of matrix-matched calibration curve preparation and this was substituted with the use of spiked calibration curve technique due to its better performance in overcoming the matrix effect. The performance of the analytical method was evaluated in-house and found to be satisfactory. Recoveries of the nereistoxin residue spiked at 12, 30, and 50 ng g-1 were at 85-95% with a relative standard deviation of below 9%. Three months of monitoring of method intermediate precision by two analysts gave a relative standard deviation value of 3.6% to 8.3% for the same spiking levels. The limit of detection (LOD) and limit of quantification (LOQ) were first estimated using the standard deviation of the calibration curve at a 95% confidence level and subsequently evaluated by actual experimental work. The values found were 5.0 ng g-1 and 12.0 ng g-1. 

 

Keywords: nereistoxin, palm oil, method development, dimehypo, spiked calibration

 

Abstrak

Kajian ini bertujuan untuk menambahkan sebatian nereistoxin, iaitu sebatian metabolit utama bagi kesemua racun perosak dari kelas analog nereistoxin termasuk thiosultap-disodium ke dalam kaedah analisa sisabaki thiosultap-disodium dalam matriks minyak sawit yang dibangunkan sebelum ini. Kesemua langkah pengolahan sampel yang telah dibangunkan sebelum ini bagi penentuan thiosultap-disodium melibatkan pengekstrakan fasa cecair-cecair lalu penentuan menggunakan kromatografi cecair spektrometri jisim caturkutub ganda tiga masih diikut, kecuali langkah persediaan keluk kalibrasi padanan-matriks telah digantikan dengan penggunaan teknik keluk kalibrasi pemakuan memandangkan prestasinya yang lebih bagus dalam mengatasi kesan dari matriks. Prestasi kaedah analitikal ini telah dinilai secara dalaman di makmal sendiri dan didapati ianya memuaskan. Nilai perolehan semula sisabaki nereistoxin yang telah dipakukan pada 12, 30 and 50 ng g-1, masing-masing adalah dalam lingkungan 85-95 % dengan nilai piawai relatif di bawah 9%. Pemantauan selama tiga bulan bagi menentukan kepersisan perantaraan kaedah oleh dua orang penganalisa berbeza memberikan nilai piawai relatif 3.6% ke 8.3% untuk kepekatan pemakuan yang sama. Had pengesanan dan had kuantitatif telah dianggarkan pada permulaan menggunakan sisihan piawai yang diperolehi daripada keluk kalibrasi pada tahap keyakinan 95% lalu pengesahan dilakukan melalui kajian secara eksperimen. Nilai yang diperolehi adalah 5.0 ng g-1 dan 12.0 ng g-1, masing-masing.

 

Kata kunci: nereistoxin, minyak sawit, pembangunan kaedah, dimehypo, kalibrasi pemakuan

 

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