Application of static headspace GC–MS for detection of residual trichloroethylene and toluene solvents in β-cyclodextrin

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The β-CD has been used for foods, directly, or as food additives and recognized as “Generally recognized as safe (GRAS)”. The recommendation of the Joint FAO/WHO Expert Committee on Food Additives (JECFA) established the maximum advisable level of β-CD in foods at 5 mg/kg/day and remained as it is after re-evaluation by European Food Safety Authority (EFSA) in 2016 concerning the presence of trichloroethylene, classified as carcinogenic to humans (Group 1), as residual solvent in β-cyclodextrin (E 459). The Panel also noted that based on the maximum permitted residual level of trichloroethylene in the EU specifications of β-cyclodextrin (E 459) (1 mg/kg), the exposure to trichloroethylene associated to theuse of β-cyclodextrin as a food additive at the ADI of 5 mg/kg bw per day would be 5 ng/kg bw per day. [1]

Trichloroethylene (TCE) and toluene (TOL), which have been used for β-cyclodextrin (β-CD) synthesis, need to be properly inspected for quality assurance and safety of food additives. In this study, a combination of static headspace separation and gas chromatography-mass spectrometry (SH–GC–MS) was optimized for detecting those residual solvents in β-CD in the compatible safe and green chemistry. [2] Sample injection amount for SH was determined to 100 μL with the minimum volume that provides the suitable accuracy. For the safety and accuracy of analysis, equilibrium conditions of solvents were considered and selected to 60°C for 45 min. It was also found that the addition of salt, like CaCl2, adversely affected recovery efficiency. Under the proposed condition, coefficients of determination (R2) of both TCE and TOL were more than 0.99 between 0.05–10 mg/L concentrations. Recovery rates and relative standard deviation (RSD) of tested solvents were between 91.7–106.0% and 1.0–8.9%, respectively. From validation with two commercial β-CDs, both TCE and TOL presented lower than regulatory limits for food additives (1 ppm) with satisfactory RSDs (<20%). Collectively, the proposed analytical methods can contribute to safer, simpler, and greener inspection of residual chemicals present in foods for public health.

References:

[1] Re-evaluation of β-cyclodextrin (E 459) as a food additive. EFSA Journal 2016,
https://doi.org/10.2903/j.efsa.2016.4628

[2] Yu-Kyeong Kim, Seo-Yeon Kwon, Yong-Soo Seo, Yang-Bong Lee, Jin Hong Mok (2024) Application of static headspace GC–MS for detection of residual trichloroethylene and toluene solvents in β-cyclodextrin. Food Research International 197, 115292. https://doi.org/10.1016/j.foodres.2024.115292

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