Method for the determination of 243 Residual Pesticides in Red Chili Powder using LCMS-8050 and GCMS-TQ8040 NX

Importance of the Topic

Red chili powder is widely used as a spice around the world. Intensive agricultural practices raise concerns about residual pesticide levels in chili powder and associated health risks. Regulatory limits such as MRLs must be met to ensure consumer safety. A robust analytical workflow capable of detecting multiple pesticide residues at trace levels in complex matrices is therefore essential for quality control and regulatory compliance.

Study Objectives and Overview

This study aimed to develop and validate a fast, sensitive, multi residue method for the determination of 243 pesticides in red chili powder. The approach combined liquid chromatography tandem mass spectrometry LC MS MS and gas chromatography tandem mass spectrometry GC MS MS to cover a broad range of compounds. Validation followed international guidelines to assess specificity, linearity, precision and recovery.

Methodology and Instrumentation

A modified QuEChERS extraction protocol was applied to a single sample aliquot. After extraction with acetonitrile and salts including sodium chloride and anhydrous magnesium sulfate, dispersive solid phase cleanup used C18 graphitized carbon black and primary secondary amine sorbents to reduce matrix interference. The final extracts were split for analysis:

• LC MS MS analysis on Shimadzu LCMS 8050 with Nexera X2, using biphenyl column and ammonium formate mobile phases under gradient conditions
• GC MS MS analysis on Shimadzu GCMS TQ 8040 NX with a 5Sil MS capillary column and splitless injection

Calibration employed matrix matched standards across relevant concentration ranges and weighted regression. Tandem MS utilized one target and two reference MRM transitions per analyte.

Main Results and Discussion

Specificity was confirmed by absence of significant blank interference. Linearity was achieved over 0.1 to 10 microgram per liter in LC MS MS and 1 to 50 microgram per liter in GC MS MS with correlation coefficients above 0.98. The method LOQ was 5 microgram per kilogram for 97 compounds by LC MS MS and for 41 compounds by GC MS MS. At the LOQ level, mean recoveries for the majority of analytes fell within 70 to 120 percent and both repeatability and reproducibility were under 20 percent RSD in accordance with SANTE guidelines.

Benefits and Practical Applications

The combined LC MS MS and GC MS MS workflow offers rapid multi residue coverage, high sensitivity and reliable quantitative performance in a challenging matrix. Laboratories engaged in food safety testing can adopt this method to monitor compliance with international pesticide regulations and support quality assurance in spice production.

Future Trends and Applications

Advances in ultra fast chromatography and high resolution mass spectrometry could expand screening capabilities and reduce analysis time further. Integration of automated sample preparation and AI driven data processing may improve throughput and lower detection limits. Growing pesticide databases and spectral libraries will enhance compound identification in complex food matrices.

Conclusion

A validated, high throughput method for simultaneous analysis of 243 pesticides in red chili powder has been established using Shimadzu LC MS MS and GC MS MS instruments. The approach meets stringent validation criteria and is suited for routine monitoring of pesticide residues to ensure consumer safety and regulatory compliance.

Reference

1. M. Anastassiades S J Lehotay D Stajnbäher F J Schenck Fast and Easy Multiresidue Method Employing Acetonitrile Extraction Partitioning and Dispersive Solid Phase Extraction for the Determination of Pesticide Residues in Produce J AOAC Int 86 412 431 2003
2. Guidance document on analytical quality control and method validation procedures for pesticide residues and analysis in food and feed SANTE 12682 2019