title: Development, validation and determination of multiclass pesticide residues in cocoa beans using gas chromatography and liquid chromatography tandem mass spectrometry.
abstract: An efficient and rapid method for the analysis of pesticide residues in cocoa beans using gas and liquid chromatography-tandem mass spectrometry was developed, validated and applied to imported and domestic cocoa beans samples collected over 2 years from smallholders and Malaysian ports. The method was based on solvent extraction method and covers 26 pesticides (insecticides, fungicides, and herbicides) of different chemical classes. The recoveries for all pesticides at 10 and 50 μg/kg were in the range of 70-120% with relative standard deviations of less than 20%. Good selectivity and sensitivity were obtained with method limit of quantification of 10 μg/kg. The expanded uncertainty measurements were in the range of 4-25%. Finally, the proposed method was successfully applied for the routine analysis of pesticide residues in cocoa beans via a monitoring study where 10% of them was found positive for chlorpyrifos, ametryn and metalaxyl.
authors.affiliation: Analytical Services Laboratory, Chemistry and Technology Division, Malaysian Cocoa Board, Cocoa Innovative and Technology Centre, Lot 12621 Kawasan Perindustrian Nilai, 71800 Nilai, Negeri Sembilan, Malaysia. Electronic address: badrul@koko.gov.my.
authors.forename: Badrul Hisyam
authors.initials: BH
authors.lastname: Zainudin
authors.affiliation: Analytical Services Laboratory, Chemistry and Technology Division, Malaysian Cocoa Board, Cocoa Innovative and Technology Centre, Lot 12621 Kawasan Perindustrian Nilai, 71800 Nilai, Negeri Sembilan, Malaysia. Electronic address: salsazali@koko.gov.my.
authors.forename: Salsazali
authors.initials: S
authors.lastname: Salleh
authors.affiliation: Analytical Services Laboratory, Chemistry and Technology Division, Malaysian Cocoa Board, Cocoa Innovative and Technology Centre, Lot 12621 Kawasan Perindustrian Nilai, 71800 Nilai, Negeri Sembilan, Malaysia. Electronic address: rahmat@koko.gov.my.
authors.forename: Rahmat
authors.initials: R
authors.lastname: Mohamed
authors.affiliation: Advanced Chemistry Solutions, 43 Jalan Wangsa 1/2, Taman Wangsa Permai, 52200 Kuala Lumpur, Malaysia. Electronic address: haruyapkc@gmail.com.
authors.forename: Ken Choy
authors.initials: KC
authors.lastname: Yap
authors.affiliation: Product Development and Advisory Services, Analytical and Quality Development Unit, Malaysian Palm Oil Board, No. 6 Persiaran Institusi, Bandar Baru Bangi, 43000 Kajang, Selangor, Malaysia. Electronic address: halimah@mpob.gov.my.
authors.forename: Halimah
authors.initials: H
authors.lastname: Muhamad
mesh_terms: D000409:Alanine / Q000031:analogs & derivatives / Q000032:analysis / Q000302:isolation & purification; D002099:Cacao / Q000737:chemistry*; D004390:Chlorpyrifos / Q000032:analysis / Q000302:isolation & purification; D002851:Chromatography, High Pressure Liquid; D005504:Food Analysis / Q000379:methods*; D008401:Gas Chromatography-Mass Spectrometry; D010573:Pesticide Residues / Q000032:analysis* / Q000302:isolation & purification; D052616:Solid Phase Extraction; D053719:Tandem Mass Spectrometry; D014227:Triazines / Q000032:analysis / Q000302:isolation & purification
chemical_list: D010573:Pesticide Residues; D014227:Triazines; C028175:metalaxyl; C100057:ametryne; D004390:Chlorpyrifos; D000409:Alanine
keywords: Cocoa beans; GC–MS/MS; LC–MS/MS; Method validation; Pesticide residues