Simultaneous Analysis of 3-MCPD and 1,3-DCP in Asian Style Sauces Using QuEChERS Extraction and Gas Chromatography–Triple Quadrupole Mass Spectrometry

Abstract

Acid hydrolyzed vegetable protein (aHVP) is used for flavoring a wide variety of foods and also in the production of nonfermented soy sauce. During the production of aHVP, chloropropanols including 3-monochloropropane-1,2-diol (3-MCPD) and 1,3 dichloropropane-2-ol (1,3-DCP) can be formed through the reaction of the hydrochloric acid catalyst and residual fat and the reaction of 3-MCPD with acetic acid, respectively. 3-MCPD is a carcinogen, and 1,3-DCP has been classified as a genotoxic carcinogen. The European Union (EU) has set a maximum concentration of 0.02 mg/kg of 3-MCPD in aHVP, and the Food and Drug Administration (FDA) set a guidance limit of 1 mg/kg of 3-MCPD in aHVP. 1,3-DCP is not an approved food additive, and the Joint FAO/WHO Expert Committee on Food Additives (JEFCA) has set a limit at 0.005 mg/kg, which is close to the estimated method detection limit. Currently there are few analytical methods for the simultaneous determination of 3-MCPD and 1,3-DCP without derivatization due to differences in their physical chemical properties and reactivity. A new method was developed using QuEChERS (quick, easy, cheap, effective, rugged, and safe) with direct analysis of the extract without derivatization using gas chromatography–triple quadrupole mass spectrometry (GC-QQQ). Additionally, a market sampling of 60 soy sauce samples was performed in 2015 to determine if concentrations have changed since the FDA limit was set in 2008. The sampling results were compared between the new QuEChERS method and a method using phenylboronic acid (PBA) as a derivatizing agent for 3-MCPD analysis. The concentrations of 3-MCPD detected in soy sauce samples collected in 2015 (<MDL to 0.53 mg/kg) compared to 2003 (<MDL to 876 mg/kg) indicate that manufacturing controls currently in use during aHVP production have been effective at reducing 3-MCPD below current regulatory limits

Assessment of estimated daily intake of 3-monochloropropane-1,2-diol from soy sauce in Korea

“…In comparison, among 164 Chinese soy sauce samples reported in 2013, eleven samples exceeded 20 lg/kg (Xu et al, 2013). Genualdi and Nyman (2017) also found a substantial reduction of 3-MCPD level in 60 Asian soy sauces analysed in 2015 in comparison with those in 2003. These indicate that 3-MCPD concentration in soy sauce has been significantly decreased.…”

“…3-MCPD is generally derivatized prior to gas chromatographic analysis due to its low volatility and high polarity (Hamlet et al, 2002). Phenylboric acid (PBA), heptafluorobutyric acid (HFBA), and HFBI has been commonly used as a derivatizing reagent of 3-MCPD (Genualdi and Nyman 2017;Kim et al, 2006a;Christova-Bagdassarian et al, 2013;Xu et al, 2013;Wong et al, 2006). 3-MCPD derivatized with HFBI had more fragments than other derivatives in mass spectrometry, which made it easier to confirm 3-MCPD from foods that contains various components (Lee and Khor, 2015).…”

OIL PALM ECONOMIC PERFORMANCE IN MALAYSIA AND R&D PROGRESS IN 2017 – Review Article

“…Mitigation approaches were proposed through the choice of fertilisers, implementation of timely harvesting and fruit milling as well as employing milder processing conditions and utilisation of additional processing technologies such as short path distillation for their efficient removal (Clemens et al, 2017). Intensive R&D of robust analytical methods for the determination of 3-MCPD esters and GE in recent years has led to novel, fast and reliable techniques for the identification and quantification of these compounds in different food matrices using state-of-the-art high resolution instrumentation such as gas chromatographymass spectrometry, gas chromatography-triple quadrupole mass spectrometry and liquid chromatography-high resolution mass spectrometry (Cheng et al, 2017;Genualdi et al, 2017;Jedrkiewicz et al, 2017). The urgency in addressing concerns pertaining to 3-MCPD esters and GE has resulted in a concentrated holistic approach within the palm oil industry in the past year to develop mitigation strategies throughout the supply chain, in addition to the food safety analysis of these compounds.…”

Non-Target Detection of Diversity of Volatile Chlorine Compounds in Frying Oil and Study on the Influencing Factors of Their Formation

“…The free 3-MCPD also directly exists in edible oil in a small amount (Svejkovská et al, 2018). The determination method of such trace small molecular chlorinated compounds mainly based on gas chromatography-mass spectrometry (GC-MS) and gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) (Genualdi et al, 2017;Kim et al, 2015;Küsters et al, 2010;Yang et al, 2018). However, these MS methods pose technical problems, including low m/z fragmentation patterns, expensive instrumentation, and high running costs.…”