Multiresidue pesticides analysis in Curcumin color additive powder using GCMS-TQ8040 NX and LCMS-8050

Importance of the topic

Curcumin is a widely used natural color additive derived from turmeric with applications in food, cosmetics and pharmaceuticals. Due to intensive pesticide use in turmeric cultivation, monitoring trace levels of multiple pesticide residues in curcumin powder is critical for consumer safety and regulatory compliance. Ensuring reliable detection at low limits of quantitation supports quality assurance in complex botanical matrices.

Objectives and overview

This study aims to develop and validate a single extraction, multiresidue analytical method for quantifying 72 pesticides in curcumin powder. By combining a modified QuEChERS procedure with both gas chromatography tandem mass spectrometry and liquid chromatography tandem mass spectrometry, the work evaluates linearity, recovery, repeatability and reproducibility to meet standard method performance requirements.

Methodology and instrumentation

The extraction uses optimized QuEChERS salts and acetonitrile, followed by cleanup with C-18, graphitized carbon black, primary secondary amine, zirconium and magnesium sulfate to reduce matrix effects. After partitioning, one aliquot is reconstituted in ethyl acetate for GC-MS/MS and the other diluted with methanol for LC-MS/MS. Matrix matched calibration ranges cover 0.5 to 200 μg/L for GC and 0.1 to 20 μg/L for LC. Fortified samples at 5, 10 and 20 μg/kg are analyzed in six replicates. Instrumental conditions are optimized using vendor method packages and pesticide databases. Data processing is performed with dedicated software to evaluate validation criteria.

Used instrumentation

• GC-MS/MS system with GCMS TQ8040 NX and AOC-20i auto injector, SH-Rxi-5Sil MS column
• LC-MS/MS system with LCMS 8050 coupled to Nexera X2, Shim-pack Scepter column
• Software for method optimization and data processing supporting high throughput analysis

Main results and discussion

• Limit of quantitation of 5 μg/kg was achieved for 61 out of 72 pesticides; six compounds required higher LOQs
• Linearity coefficients (R2) exceeded 0.98 for most analytes across calibration ranges
• Recoveries at LOQ levels fell within 60 to 120 percent, meeting Standard Method Performance Requirements
• Repeatability RSD_r was below 20 percent and reproducibility RSD_R was below 30 percent for the majority of compounds
• The modified QuEChERS cleanup effectively suppressed matrix interference in curcumin powder

Benefits and practical applications

The validated approach enables simultaneous monitoring of a broad range of pesticides in complex botanical additives, supporting regulatory control and quality assurance in the spice and food industries. The dual platform use allows selection of the most suitable technique based on required sensitivity and compound properties, enhancing laboratory efficiency and throughput.

Future trends and potential applications

Advances in high resolution mass spectrometry and automated sample preparation promise further improvements in residue analysis. Expanding the method to other plant derived ingredients, integrating novel sorbents for matrix cleanup and applying machine learning for data evaluation could enhance selectivity and reduce analysis time. Real time monitoring and portable mass spectrometric systems may enable on site testing in supply chains.

Conclusion

The combined modified QuEChERS extraction with GC-MS/MS and LC-MS/MS provides a robust, high throughput solution for multiresidue pesticide analysis in curcumin powder. The method meets stringent validation criteria for sensitivity, accuracy and precision in a challenging matrix, offering a practical tool for routine monitoring.

References

1. Anastassiades M, Lehotay SJ, Štajnbaher D, Schenck FJ. Fast and easy multiresidue method employing acetonitrile extraction partitioning and dispersive solid phase extraction for the determination of pesticide residues in produce. Journal of AOAC International. 2003;86:412–431
2. European Commission. Guidance document on analytical quality control and method validation procedures for pesticide residues and analysis in food and feed. SANTE 12682/2019