RESUMEN
3-Monochloropropane-1,2-diol (3-MCPD), 2-monochloropropane-1,2-diol (2-MCPD) and 2,3-epoxy-1-propanol (glycidol), in their free form or esterified to fatty acids, are food contaminants formed during the refinement of oils and fats. We conducted a survey to quantify the levels of these compounds in 130 food items, in order to assess the exposure to them in food and the consequent health risk for consumers. Food samples, including infant formula, were analysed by gas-chromatography mass spectrometry with the indirect method, and we used the latest open access food consumption database for the Italian population for a probabilistic assessment of exposure. We adopted an in silico approach to fill the gap for the toxicity of 2-MCPD. The occurrence values for the three contaminants in food were in most cases lower than or comparable to those reported in previous surveys. Exposure assessment for the most exposed individuals (95thpercentiles of consumers only) of different age groups, gave values below the tolerable daily intake recommended by the European Food Safety Authority for 3-MCPD and below the simulated or predicted toxicity thresholds for 2-MCPD, indicating a negligible risk due to dietary exposure to these contaminants. For glycidol, however, estimated exposure indicated a non-negligible increase in cancer risk, and a margin of exposure <25,000 for younger population groups, indicating a potential health concern.
Asunto(s)
Exposición Dietética , Compuestos Epoxi , Contaminación de Alimentos , Propanoles , alfa-Clorhidrina , Compuestos Epoxi/toxicidad , Compuestos Epoxi/análisis , Exposición Dietética/análisis , Exposición Dietética/estadística & datos numéricos , Propanoles/análisis , Medición de Riesgo , Humanos , alfa-Clorhidrina/análisis , Italia , Contaminación de Alimentos/análisis , Adulto , Lactante , Adolescente , Adulto Joven , Preescolar , Niño , Persona de Mediana Edad , Glicoles de PropilenoRESUMEN
Chinese bacon is highly esteemed by consumers worldwide due to its unique aroma. The composition of volatile organic compounds (VOCs) varies significantly among different types of Chinese bacon. This study analyzed the VOCs of Chinese bacon from Sichuan, Hunan, Guangxi, and Shaanxi provinces using gas chromatography-mass spectrometry (GC-MS), an electronic nose (E-nose), and gas chromatography-ion mobility spectrometry (GC-IMS). The results demonstrate that the combination of GC-MS and GC-IMS effectively distinguishes Chinese bacon from different regions. Notably, Guangxi bacon lacks a smoky aroma, which sets it apart from the other types. However, it contains many esters that play a crucial role in its flavor profile. In contrast, phenols, including guaiacol, which is typical in smoked bacon, were present in the bacon from Sichuan, Hunan, and Shaanxi but were absent in Guangxi bacon. Furthermore, Hunan bacon exhibited a higher aldehyde content than Sichuan bacon. 2-methyl-propanol and 3-methyl-butanol were identified as characteristic flavor compounds of Zhenba bacon. This study provides a theoretical foundation for understanding and identifying the flavor profiles of Chinese bacon. Using various analytical techniques to investigate the flavor compounds is essential for effectively distinguishing bacon from different regions.
Asunto(s)
Nariz Electrónica , Cromatografía de Gases y Espectrometría de Masas , Compuestos Orgánicos Volátiles , Compuestos Orgánicos Volátiles/análisis , Cromatografía de Gases y Espectrometría de Masas/métodos , Espectrometría de Movilidad Iónica/métodos , Odorantes/análisis , Productos de la Carne/análisis , China , Aromatizantes/análisis , Aromatizantes/química , Propanoles/análisis , Aldehídos/análisis , PentanolesRESUMEN
This study presents a method based on acid transesterification and the purification by solid-phase extraction (SPE) coupled with gas chromatography-tandem mass spectrometry for quantifying 3- and 2-monochloropropanediol esters (3-MCPDE, 2-MCPDE) and glycidyl esters (GE) in nutritional foods. The fat was extracted by liquid-liquid extraction with petroleum ether and diethyl ether after the sample was hydrolysed with ammonia. Then the extract was purified by a SPE cartridge filled with the aminopropyl sorbents. It was demonstrated that the optimal elution volume for 3-MCPDE, 2-MCPDE and GE greatly depended on the sample matrix and varied from 6 to 12 mL for four different kinds of food matrices. All three analytes in the sample solution could be fully collected in the first 10-12 mL of eluate. By this way, monoacylglycerols commonly present in the samples were fully removed. Therefore, the overestimation of GE quantification was effectively eliminated. The modified analytical procedure was fully validated in a single laboratory and has been recommended as a Chinese Food Safety National Standard. In addition, two derivatisation agents, heptafluorobutyrylimidazole and phenylboronic acid, were proved to be equivalent in method accuracy and precision for the quantification of three analytes.
Asunto(s)
Ésteres , Análisis de los Alimentos , Contaminación de Alimentos , Cromatografía de Gases y Espectrometría de Masas , Propanoles , Extracción en Fase Sólida , Espectrometría de Masas en Tándem , Ésteres/análisis , Hidrólisis , Contaminación de Alimentos/análisis , Propanoles/análisis , Propanoles/química , Compuestos Epoxi/análisis , Compuestos Epoxi/química , alfa-Clorhidrina/análisis , Ácidos/análisis , Ácidos/químicaRESUMEN
We investigated the applicability of proton transfer reaction-time-of-flight mass spectrometry (PTR-TOF-MS) for quantitative analysis of mixtures comprising glycerin, acetol, glycidol, acetaldehyde, acetone, and propylene glycol. While PTR-TOF-MS offers real-time simultaneous determination, the method selectivity is limited when analyzing compounds with identical elemental compositions or when labile compounds present in the mixture produce fragments that generate overlapping ions with other matrix components. In this study, we observed significant fragmentation of glycerin, acetol, glycidol, and propylene glycol during protonation via hydronium ions (H3O+). Nevertheless, specific ions generated by glycerin (m/z 93.055) and propylene glycol (m/z 77.060) enabled their selective detection. To thoroughly investigate the selectivity of the method, various mixtures containing both isotope-labeled and unlabeled compounds were utilized. The experimental findings demonstrated that when samples contained high levels of glycerin, it was not feasible to perform time-resolved analysis in H3O+ mode for acetaldehyde, acetol, and glycidol. To overcome the observed selectivity limitations associated with the H3O+ reagent ions, alternative ionization modes were investigated. The ammonium ion mode proved appropriate for analyzing propylene glycol (m/z 94.086) and acetone (m/z 76.076) mixtures. Concerning the nitric oxide mode, specific m/z were identified for acetaldehyde (m/z 43.018), acetone (m/z 88.039), glycidol (m/z 73.028), and propylene glycol (m/z 75.044). It was concluded that considering the presence of multiple product ions and the potential influence of other compounds, it is crucial to conduct a thorough selectivity assessment when employing PTR-TOF-MS as the sole method for analyzing compounds in complex matrices of unknown composition.
Asunto(s)
Sistemas Electrónicos de Liberación de Nicotina , Espectrometría de Masas , Nicotiana , Compuestos Orgánicos Volátiles , Espectrometría de Masas/métodos , Compuestos Orgánicos Volátiles/análisis , Compuestos Orgánicos Volátiles/química , Nicotiana/química , Propilenglicol/análisis , Propilenglicol/química , Acetaldehído/análisis , Acetaldehído/química , Acetona/análisis , Acetona/química , Acetona/análogos & derivados , Glicerol/análisis , Glicerol/química , Calor , Compuestos Epoxi/química , Compuestos Epoxi/análisis , Propanoles/química , Propanoles/análisisRESUMEN
Pinacolyl alcohol (PA), a key forensic marker for the nerve agent Soman (GD), is a particularly difficult analyte to detect by various analytical methods. In this work, we have explored the reaction between PA and 1,1'-carbonyldiimidazole (CDI) to yield pinacolyl 1H-imidazole-1-carboxylate (PIC), a product that can be conveniently detected by gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-high-resolution mass spectrometry (LC-HRMS). Regarding its GC-MS profile, this new carbamate derivative of PA possesses favorable chromatographic features such as a sharp peak and a longer retention time (RT = 16.62 min) relative to PA (broad peak and short retention time, RT = 4.1 min). The derivative can also be detected by LC-HRMS, providing an avenue for the analysis of this chemical using this technique where PA is virtually undetectable unless present in large concentrations. From a forensic science standpoint, detection of this low molecular weight alcohol signals the past or latent presence of the nerve agent Soman (GD) in a given matrix (i.e., environmental or biological). The efficiency of the protocol was tested separately in the analysis and detection of PA by EI-GC-MS and LC-HRMS when present at a 10 µg/mL in a soil matrix featured in the 44th PT and in a glycerol-rich liquid matrix featured in the 48th Official Organization for the Prohibition of Chemical Weapons (OPCW) Proficiency Test when present at a 5 µg/mL concentration. In both scenarios, PA was successfully transformed into PIC, establishing the protocol as an additional tool for the analysis of this unnatural and unique nerve agent marker by GC-MS and LC-HRMS.
Asunto(s)
Cromatografía de Gases y Espectrometría de Masas , Soman , Soman/análisis , Soman/análogos & derivados , Humanos , Cromatografía Liquida , Imidazoles/química , Agentes Nerviosos/análisis , Agentes Nerviosos/química , Toxicología Forense/métodos , Sustancias para la Guerra Química/análisis , Espectrometría de Masas/métodos , Propanoles/química , Propanoles/análisisRESUMEN
Here, we investigated the use of breath-borne volatile organic compounds (VOCs) for rapid monitoring of air pollution health effects on humans. Forty-seven healthy college students were recruited, and their exhaled breath samples (n = 235) were collected and analyzed for VOCs before, on, and after two separate haze pollution episodes using gas chromatography-ion mobility spectrometry (GC-IMS). Using a paired t-test and machine learning model (Gradient Boosting Machine, GBM), six exhaled VOC species including propanol and isoprene were revealed to differ significantly among pre-, on-, and post-exposure in both haze episodes, while none was found between clean control days. The GBM model was shown capable of differentiating between pre- and on-exposure to haze pollution with a precision of 90-100% for both haze episodes. However, poor performance was detected for the same model between two different clean days. In addition to gender and particular haze occurrence influences, correlation analysis revealed that NH4+, NO3-, acetic acid, mesylate, CO, NO2, PM2.5, and O3 played important roles in the changes in breath-borne VOC fingerprints following haze air pollution exposure. This work has demonstrated direct evidence of human health impacts of haze pollution while identifying potential breath-borne VOC biomarkers such as propanol and isoprene for haze air pollution exposure.
Asunto(s)
Contaminantes Atmosféricos , Contaminación del Aire , Compuestos Orgánicos Volátiles , Contaminantes Atmosféricos/análisis , Contaminación del Aire/análisis , Pruebas Respiratorias , Cromatografía de Gases y Espectrometría de Masas , Humanos , Propanoles/análisisRESUMEN
The p-methoxycinnamic acid (p-MCA) is one of the most studied phenylpropanoids with high importance not only in the wide spectrum of therapeutic activities but also its potential application for the food industry. This natural compound derived from plants exhibits a wide range of biologically useful properties; therefore, during the last two decades it has been extensively tested for therapeutic and nutraceutical applications. This article presents the natural sources of p-MCA, its metabolism, pharmacokinetic properties, and safety of its application. The possibilities of using this dietary bioactive compound as a nutraceutical agent that may be used as functional food ingredient playing a vital role in the prevention and treatment of many chronic diseases is also discussed. We present the antidiabetic, anticancer, antimicrobial, hepato-, and neuroprotective activities of p-MCA and methods of its lipophilization that have been developed so far to increase its industrial application and bioavailability in the biological systems.
Asunto(s)
Cinamatos/química , Cinamatos/farmacología , Antiinfecciosos/farmacología , Antiinfecciosos/uso terapéutico , Antineoplásicos/farmacología , Antineoplásicos/uso terapéutico , Cinamatos/metabolismo , Cinamatos/uso terapéutico , Suplementos Dietéticos , Hipoglucemiantes/farmacología , Hipoglucemiantes/uso terapéutico , Hígado/efectos de los fármacos , Hígado/fisiología , Fármacos Neuroprotectores/farmacología , Fármacos Neuroprotectores/uso terapéutico , Polifenoles/análisis , Polifenoles/farmacología , Propanoles/análisis , Propanoles/farmacologíaRESUMEN
A fast and simple ultra-high performance supercritical fluid chromatography method has been developed for the determination of six analytes, namely (paeonol, coumarin, cinnamic alcohol, cinnamic acid, paeoniflorin, and amygdalin) in Guizhi Fuling capsule and tablet samples. The influence of the key chromatographic parameters for the separation purposes was evaluated. The optimal column was Trefoil CEL1 column. The optimal mobile phase was a gradient mixture of carbon dioxide and methanol at flow rate of 1.0 mL/min. The back pressure of the system was set to 1.38 × 107 Pa and the temperature to 45°C. The six compounds were separated within 11 min by the proposed ultra-high performance supercritical fluid chromatography method with satisfactory resolution. Method validation confirmed that the procedure is accurate with the recovery rates from 87.04 to 104.30%, intraday precision values less than 4.81% and interday precision less than 5.22%, and linear with R2 higher than 0.9967. Therefore, this work provides a simple and novel method for the simultaneous analysis of six compounds in Guizhi Fuling capsule and tablet samples.
Asunto(s)
Medicamentos Herbarios Chinos/química , Acetofenonas/análisis , Amigdalina/análisis , Cápsulas/análisis , Cromatografía con Fluido Supercrítico , Cinamatos/análisis , Cumarinas/análisis , Glucósidos/análisis , Monoterpenos/análisis , Propanoles/análisis , ComprimidosRESUMEN
The development and validation of a method for the analysis of traces of 3-monochloropropanediol (3-MCPD) esters (19) and glycidyl esters (7) of fatty acids in vegetable oils, margarine, biscuits and croissants was performed. An extraction method based on the use of solvents (tertbutyl methyl ether (20% ethyl acetate, v/v)) was carried out and cleaning of the extract with a mixture of sorbents (Si-SAX, PSA and Z-sep+) was optimized for the elimination of fatty interferents. The analysis of the targeted compounds was carried out by ultra-high-performance liquid chromatography coupled to tandem mass spectrometry, using a triple quadrupole analyzer (UHPLC-MS/MS-QqQ). The validation of the method provided trueness values between 72 and 118% and precision lower than 20%. The limits of quantification ranged from 0.01 to 0.1 mg kg-1, which were below the current legal limits. Twenty samples of vegetable oils as well of 4 samples of margarine, biscuits and croissants were analyzed. Six out of the 24 samples (25%) exceeded the limits set by European legislation, and a maximum contamination of 3-MCPD esters at 2.52 mg kg-1 was obtained in a sample of corn oil (being 1-myristoyl-3-MCPD the compound detected at the highest concentration). A maximum concentration of glycidyl esters at 7.84 mg kg-1 was determined in a soybean oil sample (glycidyl linoleate as the main compound). Only one sample of olive oil exceeded the maximum allowable limit for 3-MCPD esters with a value of 1.72 mg kg-1, expressed as 3-MCPD.
Asunto(s)
Cromatografía Líquida de Alta Presión/métodos , Ésteres/análisis , Espectrometría de Masas en Tándem/métodos , alfa-Clorhidrina/análisis , Compuestos Epoxi/análisis , Ácidos Grasos/análisis , Contaminación de Alimentos/análisis , Límite de Detección , Margarina/análisis , Aceite de Oliva/análisis , Propanoles/análisis , Estándares de Referencia , Reproducibilidad de los Resultados , Aceite de Soja/análisisRESUMEN
The study aimed to establish the detection method for bound 3-, 2-MCPD, and glycidol using accelerated solvent extraction (ASE) and gas chromatography mass spectrometry (GC-MS). The ASE was modified for reduced solvent volume and process time to extract lipid from the chocolate spread, infant formula, potato chips, and sweetened creamer. The solvent selected for ASE was a mixture of iso-hexane and acetone at 100°C with the lipid and analyte recovery ranging from 96.9% to 98.6% and 84.1% to 107.5%, respectively. The derivatisation of analytes was adopted from the AOCS method Cd29a-13 for GC-MS analysis. The results showed that the coefficient of determination (R2) of all analytes was >0.99. The limit of detection (LOD) was 0.1 mg kg-1 expressed in lipid basis for both bound 3- and 2-MCPD and 0.2 mg kg-1 expressed in lipid basis for bound glycidol. The limit of quantitation (LOQ) was 0.3 mg kg-1 expressed in lipid basis for both bound 3- and 2-MCPD and 0.6 mg kg-1 expressed in lipid basis for bound glycidol. A blank spiked with 3-monochloropropanediols fatty acid esters (MCPDE) and 2-MCPDE (0.3, 2.1, and 7.2 mg kg-1) and glycidol esters (0.6, 4.7, and 16.6 mg kg-1) were chosen for accuracy and precision tests. The recoveries were 91.7% to 105.9%. Both repeatability and within-laboratory reproducibility of the analysis were within the acceptable level of precision ranging from 1.7% to 16%. This is the first time that a full validation procedure extending to both accuracy and precision tests has been carried out for sweetened creamer and chocolate spread. Overall, the combined protocol of ASE and AOCS Cd29a-13 was successfully validated for both solid and liquid food samples with lipid content from 10% to 30%.
Asunto(s)
Compuestos Epoxi/análisis , Análisis de los Alimentos , Contaminación de Alimentos/análisis , Glicerol/análogos & derivados , Propanoles/análisis , alfa-Clorhidrina/análisis , Cromatografía de Gases y Espectrometría de Masas , Glicerol/análisis , Solventes/químicaRESUMEN
The dietary exposures to fatty esters of 3- and 2-monochloropropanediol (MCPD) and glycidol were estimated for children aged 2- to 3-year-old from two areas of China using duplicate diet collection method. The 24-h daily duplicate diet samples over three consecutive days were collected from 40 healthy children aged between 26 and 36 months. The analysis of these contaminates in food samples was measured by an indirect method that entails MCPD/glycidol cleavage from their esterified forms for GC-MS analysis. Over 71% of the mixed diet and dairy products samples were found to be contaminated with 3-MCPD and glycidyl esters. The estimated daily exposure to bound 3-MCPD (mean: 0.48-0.49 µg kg-1 bw day-1; P95: 1.00-1.11 µg kg-1 bw day-1) were well below the health guidance values and were considered of low safety concern. The daily exposure to bound 2-MCPD was estimated to be 0.031-0.038 µg kg-1 bw day-1 on average and 0.12-0.14 µg kg-1 bw day-1 for the P95 exposure. However, it was not possible to assess its risk due to the lack of health guidance value of 2-MCPD. The margin of exposure (MOE) estimates for the mean exposure to bound glycidol (0.10-0.12 µg kg-1 bw day-1) were far above 10000 and were considered of low safety concern. However, the margin of exposure estimates for the P95 bound glycidol exposure (0.41-0.45 µg kg-1 bw day-1) were below 10000 and indicated a health concern. Our data indicated that the mixed diet accounted for nearly 76% to 91% of bound MCPD and glycidol exposure. In addition, the follow-on formula was also an important source for the children aged 2-3 years.
Asunto(s)
Exposición Dietética/análisis , Compuestos Epoxi/análisis , Contaminación de Alimentos/análisis , Glicerol/análogos & derivados , Propanoles/análisis , Escuelas de Párvulos , alfa-Clorhidrina/análisis , Preescolar , China , Ésteres/análisis , Ácidos Grasos/análisis , Femenino , Análisis de los Alimentos , Glicerol/análisis , Humanos , MasculinoRESUMEN
Enzyme immobilization using inorganic membranes has enticed increased attention as they not only improve enzyme stability, but also furnish user-friendly biodevices that can be tailored to different applications. Herein, we explored the suitability of the glass fiber membrane for enzyme immobilization and its application for halocarbon detection. For this, halohydrin dehalogenase (HheC) and bovine serum albumin were crosslinked and immobilized on a glass fiber membrane without membrane functionalization. Immobilized HheC exhibited higher storage stability than its free counterpart over 60 days at 4 °C (67% immobilized vs. 8.1% free) and 30 °C (77% immobilized vs. 57% free). Similarly, the thermal endurance of the immobilized HheC was significantly improved. The practical utility of the membrane-immobilized enzyme was demonstrated by colorimetric detection of 1,3-dichloro-2-propanol (1,3-DCP) and 2,3-dibromo-1-propanol (2,3-DBP) as model analytes. Under optimized conditions, the detection limits of 0.06 mM and 0.09 mM were achieved for 1,3-DCP and 2,3-DBP, respectively. The satisfactory recoveries were observed with spiked river and lake water samples, which demonstrate the application potential of immobilized HheC for screening contaminants in water samples. Our results revealed that the proposed frugal and facile approach could be useful for enzyme stabilization, and mitigation of halocarbon pollution.
Asunto(s)
Colorimetría/métodos , Vidrio/química , Hidrolasas/metabolismo , Propanoles/análisis , alfa-Clorhidrina/análogos & derivados , Agrobacterium tumefaciens/enzimología , Estabilidad de Enzimas , Enzimas Inmovilizadas/química , Enzimas Inmovilizadas/metabolismo , Agua Dulce/análisis , Concentración de Iones de Hidrógeno , Hidrolasas/química , Hidrolasas/genética , Límite de Detección , Proteínas Recombinantes/biosíntesis , Proteínas Recombinantes/química , Proteínas Recombinantes/aislamiento & purificación , Temperatura , Contaminantes Químicos del Agua/análisis , alfa-Clorhidrina/análisisRESUMEN
Dietary supplements based on fish oils might be contaminated with thermal processing contaminants, which are generated during the fish oil deodorisation. In the study, 30 samples of dietary supplements were analysed in terms of the occurrence of 3-monochloropropane-1,2-diol esters (3-MCPDE), 2-monochloropropane-1,3-diol esters (2-MCPDE) and glycidyl esters (GE). The results showed that the highest levels of 3-MCPDE (mean: 1461 µg kg-1) as well as 2-MCPDE (mean: 357 µg kg-1) were observed in the products containing shark liver oil. In the case of GE, they were mainly detected in the supplements including shark liver and cod liver oils. Although the results indicated that the consumption of the investigated supplements constituted no more than 1% of tolerable daily intake (TDI), the occurrence of MCPDE and GE in fish oil dietary supplements with a special attention to the origin of ester precursors should be thoroughly investigated in further studies.
Asunto(s)
Suplementos Dietéticos/análisis , Aceites de Pescado/análisis , Contaminación de Alimentos/análisis , Glicerol/análogos & derivados , alfa-Clorhidrina/análisis , Animales , Aceite de Hígado de Bacalao/química , Diglicéridos/análisis , Compuestos Epoxi/análisis , Ésteres/análisis , Glicerol/análisis , Humanos , Hígado/química , Concentración Máxima Admisible , Propanoles/análisis , TiburonesRESUMEN
Cinnamic acid was chosen as an exemplar molecule to study the effect of potential contaminants on the kinetics and mechanism of the photocatalytic destruction of hydrocarbons in aqueous solutions. We identify the principal intermediates in the photocatalytic reaction of the acid and corresponding alcohol, and propose a mechanism that explains the presence of these species. The impact of two likely contaminants of aqueous systems, sulfate and chloride ions were also studied. Whereas sulfate ions inhibit the degradation reaction at all concentrations, chloride ions, up to a concentration of 0.5 M, accelerate the removal of cinnamic acid from solution by a factor of 1.6. However, although cinnamic acid is removed, the pathway to complete oxidation is blocked by the chloride, with the acid being converted (in the presence of oxygen) into new products including acetophenone, 2-chloroacetophenone, 1-(2-chlorophenyl)ethenone and 1,2-dibenzoylethane. We speculate that the formation of these products involves chlorine radicals formed from the reaction of chloride ions with the photoinduced holes at the catalyst surface. Interestingly, we have shown that the 1-(2-chlorophenyl)ethenone and 1,2-dibenzoylethane products form from 2-chloroacetophenone when irradiated with 365 nm light in the absence of the catalyst. The formation of potentially dangerous side products in this reaction suggest that the practical implementation of the photocatalytic purification of contaminated water needs to considered very carefully if chlorides are likely to be present.
Asunto(s)
Cinamatos/análisis , Luz , Propanoles/análisis , Contaminantes Químicos del Agua/análisis , Purificación del Agua/métodos , Catálisis , Cloro/química , Cinamatos/efectos de la radiación , Oxidación-Reducción , Propanoles/efectos de la radiación , Sulfatos/química , Titanio/química , Contaminantes Químicos del Agua/efectos de la radiaciónRESUMEN
Fatty acid esters of 3-monochloropropanediol (3-MCPD), 2-MCPD and glycidol (Gly) are food-processing contaminants that cause concerns about possible adverse health effects. The present study evaluates the contamination levels of the three ester classes in 130 samples of foodstuffs marketed in Italy covering 10 food categories, namely margarines, oils, roasted coffee, breakfast cereals, salted crackers, cookies, infant biscuits, rusks, breads and potato crisps. The analytical method employed is a so-called indirect method that entails MCPD/glycidol cleavage from their esterified forms, cleanup, derivatisation and GC-MS analysis. The MCPDs and glycidol concentrations (from esters) were found to be equal or a little higher than the levels reported in previous studies conducted in other European countries and described in the literature. 3-MCPD was the predominant compound in all foodstuffs analysed with the exception for rusks where Gly levels were slightly higher. Considering the sum of MCPD and Gly esters, the most contaminated foodstuffs were seed oils, followed by margarines and cookies, whereas roasted coffee, bread, rusks, cornflakes and infant biscuits were less contaminated with MCPDs and Gly concentrations often below LOQ or LOD values. Refined olive oil, potato chips and salted crackers showed contamination levels intermediate between the two above groups. The results of this study also confirm that the use of palm oil as an ingredient or frying medium is an important cause of increase of the levels of MCPD and Gly esters, especially in salted crackers, rusks and potato crisps. Finally, the Italian intake of 3-MCPD due to the various foods analysed has been calculated and related to TDI. The MoE for Gly was also estimated.
Asunto(s)
Compuestos Epoxi/análisis , Ésteres/análisis , Ácidos Grasos/análisis , Análisis de los Alimentos , Contaminación de Alimentos/análisis , Glicerol/análogos & derivados , Propanoles/análisis , Manipulación de Alimentos , Glicerol/análisis , Humanos , ItaliaRESUMEN
Fatty acid esters of 3-monochloropropane-1,2-diol (3-MCPD) and glycidol are potentially carcinogenic and/or genotoxic processing contaminants that are formed during the process of edible oil refining. Because of their toxicological properties, the presence of these compounds in refined oils and foods containing these oils, particularly infant formula, poses a potential food safety concern. For this reason, recent research efforts have focussed on the development of methods for the analysis of MCPD and glycidyl esters in infant formula in order to estimate levels of exposure. This work presents occurrence data for 3-MCPD and glycidyl esters in 222 infant formulas purchased in the United States between December 2017 and January 2019. The results of this study show a wide range of contaminant concentrations across four different manufacturers, with average bound 3-MCPD concentrations ranging from 0.035 µg g-1 to 0.63 µg g-1 and average bound glycidol concentrations ranging from 0.019 µg g-1 to 0.22 µg g-1. The data suggest that manufacturers B and C source palm oil produced with mitigation measures, leading to reduced amounts of 3-MCPD and glycidyl esters in their infant formulas. Additionally, comparison with a previously published study in our laboratory of the occurrence of 3-MCPD and glycidyl esters in infant formula purchased in the U.S. between 2013 and 2016 revealed that, since 2016, contaminant concentrations have decreased in products produced by manufacturers A, B, and C, while contaminant amounts in formulas from manufacturer D have slightly increased.
Asunto(s)
Compuestos Epoxi/análisis , Ésteres/análisis , Ácidos Grasos/análisis , Fórmulas Infantiles/análisis , Propanoles/análisis , alfa-Clorhidrina/análisis , Estados UnidosRESUMEN
The present study aims at synthesizing and in vitro antibacterial activity evaluation of chitosan oligosaccharide (COS) modified by Cinnamyl alcohol (Cin) onto the OH position of COS. Three different degrees of substitution (DS) COS-O-Cin1-3 were synthesized by changing different molar ratios of COS to Cin. UV-visible spectroscopy (UV-vis), Fourier transform infrared (FT-IR), 1H nuclear magnetic resonance (1H NMR), thermogravimetric analysis (TGA), X-ray diffraction (XRD) and elemental analysis were conducted to characterize the successful synthesis of COS-O-Cin1-3. The results showed that they exhibited higher thermal stability, weaker crystallinity and better antibacterial properties than that of COS. These results aided in obtaining the important supports for exploring new functional antibacterial agents, which expand the scope of COS's application in the food industry.
Asunto(s)
Quitosano/química , Quitosano/farmacología , Propanoles/química , Propanoles/farmacología , Antibacterianos/análisis , Antibacterianos/síntesis química , Antibacterianos/química , Antibacterianos/farmacología , Quitosano/análisis , Quitosano/síntesis química , Escherichia coli/efectos de los fármacos , Espectroscopía de Resonancia Magnética , Propanoles/análisis , Espectroscopía Infrarroja por Transformada de Fourier , Staphylococcus aureus/efectos de los fármacos , Difracción de Rayos XRESUMEN
Monochlorpropanediol fatty acid esters (MCPDE) and glycidyl fatty acid esters (GE) are mainly considered to be processing contaminants and their concentration can rise during high temperature refining and deodorization of edible oils. Free forms formed during digestive hydrolysis of esters such as 3-monochloropropane-1,2-diol (3-MCPD), 2-MCPD and glycidol can provoke a negative effect on human health. Therefore the quantitative determination of MCPDE and GE in edible oils, fats and fat blends is needed. The aim - this manuscript deals with MCPDE and GE concentration measured as free 3-MCPD, 2-MCPD and glycidol in different edible oils, fats and fat blends of Russian market. Material and methods. 55 edible oil and fat samples sold on Russian market including refined and non-refined oils and fat blends such as spreads, dairy fat replacers, and margarines have been analyzed. Slow alkaline transesterification method with GC-MS/MS was used. Results. According to the data obtained, the highest concentrations of the contaminants were detected in fat blends: <0.10-5.03 mg/kg for 3-MCPD, <0.10-2.50 mg/kg for 2-MCPD and 0.1 5-11.17 mg/kg for glycidol. In palm oils and its fractions concentration of 3-MCPD was <0.10-6.61 mg/kg, 2-MCPD - <0.10-2.69 mg/kg and glycidol - <0.10-6.29 mg/kg. The content of glycidol in sunflower oils fluctuated in the range <0.10-1.19 mg/kg, 3-MCPD was <0.10-2.47 mg/kg, and 2-MCPD <0.10-0.67 mg/kg. Non-refined edible oils and olive oils had no or little MCPDE or GE. Conclusion. In this work we indicate high importance of monitoring MCPDE and GE in edible oils and fats both as ready-to-eat products and as ingredients prior to the Russian market release. There is strong need in mitigation of these process contaminants during fat blends manufacturing.
Asunto(s)
Grasas de la Dieta/análisis , Compuestos Epoxi/análisis , Contaminación de Alimentos/análisis , Glicerol/análogos & derivados , Aceites de Plantas/análisis , Propanoles/análisis , Espectrometría de Masas en Tándem , alfa-Clorhidrina/análisis , Esterificación , Glicerol/análisis , Humanos , Federación de RusiaRESUMEN
A method for the rapid screening of 1,3-dichloro-2-propanol, 2,3-dichloro-1-propanol,3-monochloropropane-1,2-diol, and 2-monochloropropane-1,3-diol in soy sauce was developed based on dispersive solid phase extraction-gas chromatography-high resolution mass spectrometry (GC-HRMS). The samples were extracted by ethyl acetate, cleaned up using N-propylethylenediamine and detected by GC-HRMS. The chloropropanols were quantified by the internal standard method. The results demonstrated that the limits of quantitation of the four chloropropanols were in the range of 0.5-10 µg/kg. The recoveries of the four chloropropanols in soy sauce spiked with three levels varied from 78% to 103%, and the relative standard deviations were no more than 8.8%. The proposed method is simple, accurate, sensitive and suitable for the rapid screening of the four chloropropanols in soy sauce.
Asunto(s)
Propanoles/análisis , Alimentos de Soja/análisis , Cromatografía de Gases y Espectrometría de Masas , Extracción en Fase SólidaRESUMEN
This study was conducted to investigate on the effect of different sampling regions of palm-refined oils and fats on the 2- and 3-monochloropropanediol fatty acid esters (MCPDE) and glycidol fatty acid esters (GE) levels. The American Oil Chemists' Society (AOCS) Official Method Cd 29a-13 on the determination of MCPDE and GE in edible oils and fats by acid transesterification was successfully verified and optimised, with slight modification using 7890A Agilent GC system equipped with 5975C quadrupole detector. The determined limits of detection (LOD) for MCPDE were 0.02 mg kg-1 and 0.05 mg kg-1 for GE. The method performance has showed good recovery between 80% and 120% for all pertinent compounds with seven replicates assayed in three separate days. Round robin test with two European laboratories, i.e. Eurofins and SGS, has shown compliance results with those of the present study. Among the sampling regions, only one refinery located in the central region of Malaysia showed a significant increment of the MCPDE and GE levels after refining process. The GE level averaging at 2.5 mg kg-1 was slightly higher than that of 3-MCPDE averaging at 1.3 mg kg-1. Both esters were preferentially partitioned into the liquid phase rather than the solid phase after fractionation. However, the overall results exhibited no direct correlation between the esters content and the different sampling locations of the palm oil products in Malaysia. Analysis of total chlorine content also displayed significant variations between sampling locations which clearly show its effect on the chlorine content in the CPO samples.