GC/MSD, GC/MS/MS, Sample Preparation, GC/QQQ, Consumables
IndustriesFood & Agriculture
ManufacturerAgilent Technologies
Importance of the topic
This summary addresses the critical need for sensitive and reliable methods to monitor pesticide residues in mango. As a major global exporter, Brazil must ensure its mangoes comply with safety regulations and consumer health standards. Advanced analytical approaches help detect both regulated and non-permitted pesticides at trace levels, safeguarding trade and public health.
Objectives and overview of the study
The study developed two complementary GC/MS/MS workflows for mango analysis. The first is a quantitative method targeting 19 pesticides with Brazilian ANVISA maximum residue limits (MRLs) and nine additional compounds. The second is a qualitative multiresidue screening for 258 pesticides and metabolites, following SANCO/12571/2013 guidelines. Real-world samples were tested to evaluate compliance and detect illegal residues.
Methodology
Mango samples (10 g) underwent QuEChERS EN extraction and dispersive SPE cleanup to remove pigments. Chromatography used an Agilent 7890A GC with a DB-5ms column and constant pressure/postcolumn backflush, coupled to an Agilent 7000B triple quadrupole MS in MRM mode. Calibration curves (¼–5× MRL) were prepared in matrix. Validation metrics included linearity (R² > 0.99), recoveries (70–120%), precision (RSD < 20%), LODs (0.0006–0.0607 mg/kg) and LOQs (0.0025–0.5 mg/kg).
Applied instrumentation
- Agilent 7890A Gas Chromatograph with constant pressure/postcolumn backflush
- Agilent 7000B Triple Quadrupole GC/MS System in EI mode
- Agilent Bond Elut QuEChERS EN extraction kit (p/n 5982-5650CH)
- Agilent Bond Elut QuEChERS SPE Dispersive Kit for Pigmented Fruits and Vegetables (p/n 5982-5256CH)
- Agilent 7693A Automatic Liquid Sampler
- Agilent J&W DB-5ms column, 30 m × 0.25 mm, 0.25 µm (p/n 122-5532)
Main results and discussion
The quantitative method achieved strong linearity, accurate recoveries and low detection limits. Analysis of 20 commercial mango lots identified multiple regulated pesticides below MRLs and four non-permitted residues. Two samples exceeded the ANVISA MRL for prochloraz (0.85 and 0.92 mg/kg vs. 0.2 mg/kg). The qualitative screen detected over 250 compounds, enabling rapid identification prior to targeted quantification.
Benefits and practical applications
- Confirms compliance with national and international residue limits
- Detects unauthorized pesticide applications to enforce regulations
- Optimizes resource use by prioritizing quantitation based on screening
- Supports quality assurance in export supply chains
Future trends and possibilities of use
Expanding multiresidue libraries, automating sample preparation, and integrating high-resolution MS will enhance sensitivity and throughput. Advances in miniaturized extraction, AI-driven data analysis, and digital traceability systems promise to further streamline routine pesticide monitoring and strengthen food safety management.
Conclusion
The dual-method GC/MS/MS strategy offers precise quantitation of key regulated pesticides and broad-spectrum screening for additional compounds. This workflow improves analytical efficiency, ensures regulatory compliance, and detects illicit pesticide use in mango, contributing to safer produce and reliable export performance.
References
- European Commission SANCO. Guidance Document on Analytical Quality Control and Validation Procedures for Pesticide Residues Analysis in Food and Feed. SANCO/12571/2013.
- Anvisa. Brazilian Health Surveillance Agency Pesticide Residue Monitoring Program.
- Anastassiades M., Lehotay S. J. Fast and Easy Multiresidue Method Employing Acetonitrile Extraction and Dispersive Solid-Phase Extraction. J. AOAC Int. 2003.
- Ciscato C. H. P. et al. Pesticide Residue Monitoring of Brazilian Fruit for Export. Food Additives and Contaminants Part B 2009.
- Agilent Technologies. GC/MS/MS Pesticide Residue Analysis Reference Guide. Publication 5991-2389EN, 2013.
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