Malaysian Journal of Analytical Sciences Vol 25 No 2 (2021): 352 - 362

 

 

 

DETERMINATION OF METSULFURON METHYL IN CRUDE PALM OIL USING LIQUID CHROMATOGRAPHY TRIPLE QUADRUPOLE MASS SPECTROMETER

 

(Penentuan Metsulfuron Metil dalam Minyak Sawit Mentah Menggunakan Kromatografi Cecair Spektrometri Jisim Caturkutub Ganda Tiga)

 

Nik Sasha Khatrina Khairuddin¹*, Chee Beng Yeoh¹, Najwa Sulaiman¹, Farah Khuwailah Ahmad Bustamam¹, Halimah Muhamad¹, Ismail Sahid²

 

¹Malaysian Palm Oil Board,

No. 6, Persiaran Institusi, Bandar Baru Bangi, 43000 Kajang, Selangor, Malaysia

²School of Environmental Science and Natural Resources, Faculty Science and Technology,

Universiti Kebangsaan Malaysia, 43600 Bangi, Selangor, Malaysia.

 

*Corresponding author:  sashakhatrina@mpob.gov.my

 

 

Received: 23 December 2020 ; Accepted: 16 February 2021; Published:  25 April 2021

 

 

Abstract

A simple and fast method for the determination of metsulfuron methyl (MSM) in crude palm oil (CPO) was developed and validated in-house. The analytical method developed involved a liquid-liquid extraction of MSM with the incorporation of a heating step that has been found to enhance the extraction efficiency and stability. This is followed by clean-up using solid phase extraction (SPE), concentration and reconstitution of the analyte prior to injection into the liquid chromatography triple quadrupole mass spectrometer (LC/MS/MS). Using this method, good linearity with good coefficient correlation (r²) of >0.999 was obtained for matrix-matched calibration. Results showed that the average recoveries obtained for MSM in CPO samples at different levels of concentration (ultra-low, low, and high) are in the range between 84-98% with a relative standard deviation (RSD) of less than 5% for all samples. The limit of detection (LOD) and limit of quantification (LOQ) for analysis of residual MSM in CPO was estimated to be 1.0 and 5.0 ng/g, respectively. An experiment determining the repeatability resulted in an RSD of less than 5% for all samples and intermediate precision at spiking level at 10 ng/g and 50 ng/g showed RSD of 6.93% and 4.07%, respectively. A very low % RSD indicates good precision and suitability of this method for use in the analysis of residual MSM in CPO. Quick monitoring of Malaysian CPO was also carried out by analyzing 10 samples obtained from various mills throughout Malaysia. Results from the CPO monitoring showed that all samples were free from residual MSM.

 

Keywords: method development, metsulfuron methyl, pesticides, crude palm oil, liquid chromatography triple quadrupole mass spectrometer

 

Abstrak

Satu kaedah yang mudah dan pantas bagi penentuan kandungan metsulfuron metil (MSM) dalam minyak sawit mentah telah dibangunkan dan telah ditentusahkan. Kaedah analitikal yang telah dibangunkan melibatkan kaedah pengekstrakan MSM jenis cecair-cecair, dengan penambahan langkah pemanasan yang didapati dapat meningkatkan kecekapan dan kestabilan pengekstrakan, diikuti dengan langkah pembersihan menggunakan pengekstrakan jenis fasa pepejal (SPE), serta pemekatan dan pelarutan semula analit sebelum disuntik ke dalam instrumen kromatografi cecair spektrometri jisim caturkutub ganda tiga (LC/MS/MS). Melalui kaedah ini, kelinearan dan korelasi pekali penentuan yang baik, dengan nilai (r²) >0.999 bagi kalibrasi padanan matriks telah diperolehi. Keputusan menunjukkan purata perolehan semula yang diperolehi bagi MSM dalam sampel minyak sawit mentah pada kepekatan yang berbeza (sangat rendah, rendah dan tinggi) adalah pada julat antara 84-98% dengan nilai sisihan piawai relatif (RSD) kurang daripada 5% bagi kesemua sampel. Had pengesanan (LOD) dan had pengkuantitian (LOQ) bagi analisis sisabaki MSM dalam minyak sawit mentah masing-masing adalah 1.0 dan 5.0 ng/g. Eksperimen bagi penentuan kebolehulangan menunjukkan nilai RSD yang kurang daripada 5% untuk kesemua sampel dan kejituan pertengahan pada kepekatan 10 ng/g dan 50 ng/g menunjukkan nilai RSD masing-masing 6.93% and 4.07%. Nilai RSD yang sangat rendah menunjukkan kejituan yang baik dan kesesuaian penggunaan kaedah ini untuk analisis sisabaki MSM dalam minyak sawit mentah. Satu kajian pemantauan kandungan MSM dalam minyak sawit mentah di Malaysia juga telah dijalankan terhadap 10 sampel minyak sawit mentah yang diperolehi daripada beberapa kilang pemprosesan minyak sawit di Malaysia. Hasil keputusan pemantauan ini menunjukkan bahawa semua sampel minyak sawit mentah yang dianalisa adalah bebas dari sisabaki MSM.

 

Kata kunci: pembangunan kaedah, metsulfuron metil, pestisid, minyak sawit mentah, kromatografi cecair spektrometri jisim caturkutub ganda tiga

 

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