Extraction and measurement of 1,4 dioxane in detergents using head space microextraction followed by gas chromatography.

Abstract

Background: 1,4-dioxane is a hazardous by-product commonly found in sanitary detergents due to certain manufacturing processes. Accurate detection and quantification of this compound are essential for consumer safety.

Objective: This study aims to develop and optimize a method for detecting and quantifying 1,4-dioxane in sanitary detergents. The approach involves electropolymerization of graphene oxide nanocomposites on stainless steel mesh, followed by headspace microextraction (HS-ME) and analysis using gas chromatography with a flame ionization detector (GC-FID).

Methods: Graphene oxide nanocomposites were electropolymerized on stainless steel mesh to create the absorbent material. This absorbent was utilized in HS-ME for extracting 1,4-dioxane from sanitary detergent samples. A Plackett-Burman design (PBD) screened Seven factors, including extraction time, extraction temperature, salt addition effect, stirring speed, desorption time, type of extraction solvent, and volume of extraction solvent. Based on the screening results a central composite design (CCD) optimized the four critical factors: extraction time, extraction temperature, stirring speed, and type of extraction solvent. Quantification of 1,4-dioxane was performed using GC-FID.

Results: The optimized method demonstrated a linear range of 0.5 to 200 μg/mL with a correlation coefficient (R2) of 0.9989. The limits of detection and quantification were determined as 0.15 and 0.5 μg/mL, respectively. Method accuracy, assessed through the relative recovery percentage of 1,4-dioxane, yielded values between 91.6 and 104%. Intra-laboratory reproducibility percentages ranged from 3.2 to 6.8%.

Conclusion: The developed method, utilizing electropolymerized graphene oxide nanocomposites on stainless steel mesh for HS-ME coupled with GC-FID, provides a sensitive and accurate approach for detecting and quantifying 1,4-dioxane in sanitary detergents.

Highlights: Electropolymerization of graphene oxide nanocomposites on stainless steel mesh was successfully implemented to create an effective absorbent for HS-ME of dioxane. A systematic optimization approach, combining PBD and CCD, identified and fine-tuned critical factors influencing extraction efficiency.