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ARS Home » Pacific West Area » Parlier, California » San Joaquin Valley Agricultural Sciences Center » Commodity Protection and Quality Research » Research » Publications at this Location » Publication #429794
Research Project: Improved Systems-based Approaches that Maintain Commodity Quality and Control of Arthropod Pests Important to U.S. Agricultural Production, Trade and Quarantine

Location: Commodity Protection and Quality Research

Title: Validation of an HS-SPME-GC-MS method for the analysis of multiple fumigants in low moisture agricultural commodities

Author
item Hall Iv, Wiley
item STIGLMEIER, KYLIE - Oak Ridge Institute For Science And Education (ORISE)
item JONES, THOMAS - Dfa Of California

Submitted to: Analytical Methods
Publication Type: Peer Reviewed Journal
Publication Acceptance Date: 3/20/2026
Publication Date: N/A
Citation: N/A

Interpretive Summary: Postharvest fumigation is a critical component in world-wide trade of durable agricultural commodities, used to prevent both the spread of invasive insects and the loss of stored products. The main tool to enforce the responsible use of fumigants is by measuring the amount of fumigant (or the chemical the fumigant transforms into) leftover on the treated commodity. Therefore, efficient and accurate methods to detect and quantify fumigant residues are of great importance. Unfortunately, fumigants can be difficult to measure accurately, and the current existing methods for their analysis do not fit well within routine laboratory residue tests. Fumigants need to be analyzed separately from most other pesticide residues. Two important fumigants: ethylene oxide (EtO), used to prevent the spread of human pathogens on spices, and propylene oxide (PPO), used to treat tree nuts and other commodities for both insects and pathogens, require especial care to prevent the compounds from degrading into other regulated chemicals during treatment. This paper presents a quick, inexpensive, and sensitive method to simultaneously detect several fumigants in a single test without causing the degradation of PPO and EtO.

Technical Abstract: A single method for the analysis of multiple fuimgant residues in low moisture commodity is presented. HS-SPME-GC-MS is used to detect the preplant and postharvest fumigants SF, EF, MB, EtO, PPO, EF, MITC and 1,3-D, and the degradants PCH, PBH, ECH, EBH, and EtOH are detected with detection limits below 0.010 mg kg-1 with 0.02 mg kg-1 limits of quantitation. Recoveries of the analytes from fortified walnut and rice samples were all between 70 and 120% accuracy with RSDs below 20%. Good Linearities were obtained over the concentration range of 7 – 235 ng g-1 with correlation coefficients over 0.990. Derivatization of PPO and EtO with iodide salt, prevented their degradation during the analysis. The method is quick, produces little waste and is shown to be sensitive and accurate.