title: A simultaneous derivatization of 3-monochloropropanediol and 1,3-dichloropropane with hexamethyldisilazane-trimethylsilyl trifluoromethanesulfonate at room temperature for efficient analysis of food sample analysis.
abstract: This paper reports the application of hexamethyldisilazane-trimethylsilyl trifluoromethanesulfonate (HMDS-TMSOTf) for the simultaneous silylation of 3-monochloro-1,2-propanediol (3-MCPD) and 1,3-dicholoropropanol (1,3-DCP) in solid and liquid food samples. 3-MCPD and 1,3-DCP are chloropropanols that have been established as Group 2B carcinogens in clinical testing. They can be found in heat-processed food, especially when an extended high-temperature treatment is required. However, the current AOAC detection method is time-consuming and expensive. Thus, HMDS-TMSOTf was used in this study to provide a safer, and cost-effective alternative to the HFBI method. Three important steps are involved in the quantification of 3-MCPD and 1,3-DCP: extraction, derivatization and quantification. The optimization of the derivatization process, which involved focusing on the catalyst volume, derivatization temperature, and derivatization time was performed based on the findings obtained from both the Box-Behnken modeling and a real experimental set up. With the optimized conditions, the newly developed method was used for actual food sample quantification and the results were compared with those obtained via the standard AOAC method. The developed method required less samples and reagents but it could be used to achieve lower limits of quantification (0.0043mgL(-1) for 1,3-DCP and 0.0011mgL(-1) for 3-MCPD) and detection (0.0028mgL(-1) for 1,3-DCP and 0.0008mgL(-1) for 3-MCPD). All the detected concentrations are below the maximum tolerable limit of 0.02mgL(-1). The percentage of recovery obtained from food sample analysis was between 83% and 96%. The new procedure was validated with the AOAC method and showed a comparable performance. The HMDS-TMSOTf derivatization strategy is capable of simultaneously derivatizing 1,3-DCP and 3-MCPD at room temperature, and it also serves as a rapid, sensitive, and accurate analytical method for food samples analysis.
authors.affiliation: Department of Chemistry, Faculty of Science, University of Malaya, 50603 Kuala Lumpur, Malaysia.
authors.forename: Bai Qin
authors.initials: BQ
authors.lastname: Lee
authors.affiliation: Department of Science and Technology Studies, Faculty of Science, University of Malaya, 50603 Kuala Lumpur, Malaysia.
authors.forename: Che Wan Jasimah Bt
authors.initials: CW
authors.lastname: Wan Mohamed Radzi
authors.affiliation: Department of Chemistry, Faculty of Science, University of Malaya, 50603 Kuala Lumpur, Malaysia. Electronic address: naomikhor@um.edu.my.
authors.forename: Sook Mei
authors.initials: SM
authors.lastname: Khor
mesh_terms: D002273:Carcinogens / Q000032:analysis* / Q000737:chemistry; D005504:Food Analysis / Q000379:methods*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D006801:Humans; D008698:Mesylates / Q000737:chemistry*; D017646:Organosilicon Compounds / Q000737:chemistry*; D011407:Propane / Q000031:analogs & derivatives* / Q000032:analysis / Q000737:chemistry; D019946:Propylene Glycol; D013696:Temperature; D014297:Trimethylsilyl Compounds / Q000737:chemistry*; D000517:alpha-Chlorohydrin / Q000032:analysis* / Q000737:chemistry
chemical_list: D002273:Carcinogens; D008698:Mesylates; D017646:Organosilicon Compounds; D014297:Trimethylsilyl Compounds; C053353:trimethylsilyl trifluoromethanesulfonate; D019946:Propylene Glycol; D000517:alpha-Chlorohydrin; C067434:1,3-dichloropropane; C024548:hexamethylsilazane; D011407:Propane
keywords: 1,3-Dichloropropanol (1,3-DCP); 3-Monochloropropanediol (3-MCPD); Acid hydrolyzed vegetable protein (acid–HVP); Hexamethyldisilazane–trimethylsilyl trifluoromethanesulfonate (HMDS–TMSOTf); Room temperature derivatization; Silylation