Comprehensive strategy for pesticide residue analysis in cocoa beans through qualitative and quantitative approach.

Multiresidue quantitative and qualitative screening method for the analysis of pesticide residues in dried cocoa beans was validated and applied to imported and domestic cocoa beans samples. The quantitative method comprises of 15 pesticides while the screening method covers 110 pesticides of different chemical classes. The method was based on modified QuEChERS (Quick Easy Cheap Efficient Rugged Safe) extraction and detection using triple quadrupole (QQQ-MS) and ion mobility quadrupole time of flight mass spectrometry (IMS-QTOF). The method was quantitatively validated in terms of linearity, limit of quantification (LOQ), specificity, selectivity, accuracy, and precision. On the other hand, screening detection limits were established for 110 pesticides. Finally, the optimized strategy was successfully applied for the routine analysis of pesticide residues in 137 cocoa bean samples and 32% of the total samples were found positive for ametryn, chlorpyrifos, isoprocarb, and metalaxyl.

Method validation and determination of heavy metals in cocoa beans and cocoa products by microwave assisted digestion technique with inductively coupled plasma mass spectrometry.

In this article, an easy and quick method based on microwave assisted acid digestion technique prior to quantification using inductively coupled plasma mass spectrometry for the analysis of heavy metals in cocoa beans, cocoa powder and chocolate was established and validated for arsenic (As), cadmium (Cd), lead (Pb), and antimony (Sb). Limit of quantification for all elements were product dependent and varies from 7.84 to 194.52 µg/kg. The recoveries of the heavy metals at 250 and 1000 µg/kg spiking levels were ranged between 96.27-108.75%, 90.43-101.97% and 89.72-106.26% for cocoa beans, cocoa powder, and chocolate, respectively. Relative standard deviation values obtained were all below 20% and the expanded uncertainty measurements for the elements were less than 25%. The analysis of real samples found that the concentration level is far from the national alarming level except for cadmium in cocoa beans.

Development, validation and determination of multiclass pesticide residues in cocoa beans using gas chromatography and liquid chromatography tandem mass spectrometry.

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.