Determination Of 5-hydroxymethylfurfural Research Articles

A Novel HPLC Method for Rapid Determination of HMF in Dulce de Leche: A Potential Tool for Quality Control

A validated isocratic method utilizing reverse-phase high-performance liquid chromatography (RP-HPLC) was developed for the quantification of hydroxymethylfurfural (HMF) in five distinct commercially available Dulce de Leche samples that are sold in Turkish markets. The X-Terra RP-18 column, which has dimensions of 150 × 4.60 mm i.d. and a particle size of 5 μm, was selected for the stationary phase. The separation process was conducted isocratically by utilizing a methanol-water mixture (10:90, v/v) containing 1% TCA as the mobile phase. The separation was carried out at a temperature of 25 oC and a flow rate of 0.5 mL/min. The detection was performed at a wavelength of 284 nm. The methodology exhibited favorable selectivity and linearity, as evidenced by a correlation coefficient (r) exceeding 0.999. The obtained values for the limit of detection (LOD) and limit of quantification (LOQ) were 0.0019 μg/mL and 0.0059 μg/mL, respectively. Additionally, the recovery rate was determined to be 95.45%. Furthermore, it has been reported that the levels of HMF in commercially available Dulce de Leche originating from Turkey vary between 50.55 and 90.18 mg/kg for the total HMF content.

ANÁLISE FÍSICO-QUÍMICA E DE ROTULAGEM DE MÉIS CONSUMIDOS NA CIDADE DE CAXIAS DO SUL – RS

Honey is one of the purest of nature products, derived from nectar and other natural plant secretions, which are collected and processed by bees. Frauds in this food, as well as problems related to its processing, raise concerns for health authorities and, in this context, studies analyzing its quality are extremely important. The objective of this work was to analyze the physical and chemical quality and labeling of ten samples of honeys marketed in the city of Caxias do Sul, Rio Grande do Sul. Moisture determination, refractive index determination, pH determination, acidity determination, Lund test, Lugol test and hydroxymethylfurfural determination were performed. The physico-chemical tests were performed at the Science Laboratory of the Federal Institute of Education of Rio Grande do Sul - Campus Bento Goncalves, at the Science Laboratory of the State University of Rio Grande do Sul - Campus Caxias do Sul and at the Science Laboratory of the Fatima Faculty. In addition, product labeling analysis and comparison of compliance with current legislation were performed. The results were analyzed descriptively. Two (20%) of the ten samples analyzed presented nonconformity in the hydroxymethylfurfural test and two (20%) presented nonconformity in the moisture test. The other results found in the physico-chemical tests were in accordance with current legislation. In addition, 100% of the honeys sold in Caxias do Sul were within the standard established by the labeling legislation.

Hydroxymethylfurfural determination in cereal and insect bars by high-performance liquid chromatography-mass spectrometry employing a functionalized mesostructured silica as sorbent in solid-phase extraction

In this work a new method for the determination of 5-hydroxymethylfurfural (HMF) in cereal and insect bars has been developed and validated. The method consisted of a solid-liquid extraction (SLE) followed by a solid phase extraction (SPE), employing functionalized mesostructured silica as sorbent, and prior to high-performance liquid chromatography coupled to mass spectrometry analysis (HPLC-MS/MS). Mesostructured silica with a large pore (SBA-15-LP) functionalized with aminopropyl- groups (SBA-15-LP-NH2), octyl- groups (SBA-15-LP-C8) and bifunctionalized with both organic ligands (SBA-15-LP-C8-NH2) were prepared, characterized and tested for this purpose. The optimal conditions showed that the best extraction solvent was water acidified with HCl (pH 1.0) and the best material for SPE was SBA-15-LP-NH2 (recoveries near 100%). Results were compared with other analogous commercial sorbent (Discovery® DSC-NH2), evaluated under similar conditions, and SBA-15-LP-NH2 sorbent showed better recoveries than the commercial one (62 ± 1%). The developed method was validated and good detection and quantification limits (MDL: 11 µg kg−1and MQL: 38 µg kg−1), good precision in terms of repeatability and within-laboratory reproducibility (RSD < 8%) and good accuracy (recoveries between 99-102%) were obtained. The method was successfully applied to the determination of HMF in different samples of cereals and insect bars. In all the samples analysed, high concentrations of HMF (ranging from 336 to 962 mg kg−1) have been found.

Method validation and determination of hydroxymethyl furfural (HMF) and furosine as indicators to recognize adulterated cow’s pasteurized and sterilized milks made by partial reconstitution of skim milk powder

In this research, Hydroxymethylfurfural (HMF) and Furosine, the two important markers of Maillard reaction, were determined as potential indicators in order to identify the adulteration of skim milk powder (SMP) addition (instead of milk solid non-fat) for the formation of cow’s milk (Pasteurized and sterilized). Method validation was performed by HPLC. Pasteurized and sterilized milks (2.5% fat) with 25, 50 or 75% reconstitution of milk powder were produced. By using HPLC method, there was a significant relation between HMF and furosine contents and an increase of SMP content. The correlation between the amount of added powder and HMF or furosine concentration was almost linear. Thus, the amount of SMP addition could be determined by quantification of HMF and furosine. Sensory evaluation and optical properties of treatments were also assessed. The sensory acceptance was significantly decreased by increasing SMP substitution. Colorimetric evaluation did not show a significant difference between the treatments. The intera-day and inter-day relative standard deviation (RSD%) was 5.9% and 4.1% for HMF and furosine, respectively. The recovery rates were 85% and 91% and the LOD values for HMF and furosine were 0.05 and 0.02 ppm, respectively. The markers were realized effective and applicable for detecting SMP addition adulteration in pasteurized and sterilized cow’s milk.

Primary Investigation into the Occurrence of Hydroxymethylfurfural (HMF) in a Range of Smoked Products

5-Hydroxymethylfurfural (HMF) is produced in foods through many different pathways. Recently, studies have revealed its potential mutagenic and carcinogenic properties. Determination of HMF was originally used as an indicator of both the extent of thermal processing a food had undergone and food quality. It has been identified in a variety of food products such as bread, breakfast cereals, fruit juices, milk, and honey. In addition to the thermal processes that lead to the formation of HMF during thermal treatment, food smoking also creates conditions that result in the formation of HMF. This can take place within the food due to the elevated temperatures associated with hot smoking or by the proximity of the products of the pyrolysis of the wood matrix that is used for smoking (cold smoking). This may lead to further contamination of the product by HMF over and above that associated with the rest of the preparation process. Until now, there have been no studies examining the relation between the smoking procedure and HMF contamination in smoked food. This study is a primary investigation measuring HMF levels in three categories of smoked food products, cheese, processed meat, and fish, using HPLC-UV. The amount of HMF found in all three product categories supports our hypothesis that HMF levels are due to both internal pathways during processing and external contamination from the smoke generation matrix (wood) employed. The results ranged from 1 ppb (metsovone traditional Greek smoked cheese) to 4 ppm (hot-smoked ready-to-eat mackerel). Subsequently for smoked cheese products, a correlation was found between HMF and phenolic compounds generated by the smoking procedures and identified by SPME-GCMS. It was observed that cheese samples that had higher concentrations of HMF were also found to have higher concentrations of syringol and cresols. It is important therefore to understand the smoking procedure’s effect on HMF formation. This will aid in the development of mitigation strategies to reduce HMF formation while retaining the flavour of the smoked products.

Furosine and HMF determination in prebiotic-supplemented infant formula from Spanish market

Evaluation of Maillard reaction (MR) in commercial prebiotic-supplemented and not supplemented infant formulas (IFs) was carried out through determination of furosine (2-furoylmethyl-ε-lysine) and hydroxymethylfurfural (HMF). Furosine was present in all studied IFs, ranging from 94 to 1226 and 315 to 965 mg 100 g−1 of protein, in samples without prebiotics and prebiotic-supplemented IFs respectively. HMF was found in all IFs in the range 62–510 μg 100 g−1 product. No statistical differences in HMF and furosine contents between prebiotic-supplemented and not supplemented IFs were observed. Storage of six representative IFs, with and without prebiotics, at room temperature for 15 months, did not produce changes in HMF content after 8 months of storage, while furosine content increased significantly throughout the storage time. The high amounts of furosine found in some IFs may be attributed to excessive heat treatment during processing, inadequate storage of IFs or ingredients used in their manufacturing process. The use of furosine and HMF as thermal indicators allows evaluation of the quality of prebiotic-supplemented IFs, which was similar to IFs without prebiotics. Finally, two supervised classification methods (support vector machines and random forests) were applied to classify IFs according to protein and carbohydrate source and IF type.

Hydroxymethylfurfural in fruit puree and juice: preconcentration and determination using microextraction method coupled with high-performance liquid chromatography and optimization by Box–Behnken design

In the present study, a sensitive and rapid method for separation and determination of hydroxymethylfurfural (HMF) in fruit puree and juices was proposed. Dispersive liquid–liquid microextraction (DLLME) coupled with high-performance liquid chromatography (HPLC) was used for extraction and quantitative determination of HMF in fruit puree and juices. The effective parameters such as the type and volume of extraction and dispersive solvents, pH and salt amount (NaCl) were studied and optimized with the aid of response surface methodology based on Box–Behnken design to obtain the best condition for HMF extraction. At the optimized conditions, parameter values were 60 µL extracting solvent, 600 µL dispersive solvent, 2 g NaCl and pH 5. Repeatability of the method, described as the relative standard deviation, was 3.1% (n = 6) and the recovery was 98.4%. The limit of detection and limit of quantitation were 1.47 and 5.28 µg L−1, respectively. The merit figures of DLLME–HPLC–UV method showed that the proposed method can be noticed as a new, fast and good alternative method for investigation of HMF in various fruit puree and juice samples.

Determination of Hydroxymethylfurfural (HMF) in Honey Based on p-Toluidine as a Reagent Using Spectrophotometric Method

Spectrophotometric determination of hydroxymethylfurfural (HMF) based on p-toluidine as a reagent has been studied. The absorption intensities were measured at a wavelength range of 250 to 500 nm to record the absorption spectra before and after reaction with the HMF. The solution response was obtained at pH 3. The concentration of HMF was 5 × 10-3M, whereas for p-toluidine was 8 × 10-3M .The relative standard deviation (R.S.D.) of reproducibility was 3.33% when concentration of p-toluidine 3 × 10-3M was used .The photostability was found to be good with 1.9 %. M was used . The photostability was found to be good with 1.9 %.

New approaches to determination of HMF

Several techniques have been used for hydroxymethylfurfural (HMF) detection in foods. Most of these involve the protein hydrolysation step process to determine the presence of organic acid with heat treatment. The affinity and separability of HMF to/from some proteins were exhibited in this study. Also, the dependency of HMF level was determined in the presence of some substances such as reductive and non-reductive sugars, gums and polysaccharides due to high temperature and acidity during the hydrolysation stage. Consequently, the HMF levels of the samples were evaluated separately either by no treatment or by the acid-heat treated method. The HMF amount which was measured by the conventional method was found to be dependent on the sample amount. The binding capacity of HMF to casein was about 10% but did not bind to the gluten in the model system. However it was not released from the caseine by acid hydrolysation in the solvent.

Hydroxymethylfurfural determination in infant milk-based formulas by micellar electrokinetic capillary chromatography

Abstract A procedure for determining hydroxymethylfurfural (HMF) in milk-based products by micellar electrokinetic capillary chromatography (MECC) was settled on. The effect of the trichloroacetic acid on the migration time of HMF and presence of interference peaks were investigated. MECC procedure was applied on commercial liquid infant formulas and compared with the classical reversed-phase high performance liquid chromatography method, giving similar values of repeatability and recovery. HMF peak was well-resolved by using an uncoated fused-silica capillary (48.5 cm×50 μm i.d.) with 50 mM phosphate buffer (pH 7.5) containing 100 mM SDS as electrolyte, voltage at 20 kV (25°C). Sample injection was by pressure (50 mbar, hydrodynamic) for 2.5 s. HMF analysis by MECC was suitable for routine analysis since separation was completely achieved at 5 min.

Reduction of Tetrazolium Salt XTT with UHT-Treated Milk: Its Relationship with the Extent of Heat-Treatment and Storage Conditions.

UHT-treated milk reduced 3'-{1-[(phenylamino)-carbonyl]-3,4-tetrazolium}-bis(4-methoxy-6-nitro)benzenesulfonic acid hydrate (XTT). The reducibility was caused by the Maillard reaction intermediate between milk protein and lactose. First, the assay procedure of the XTT reduction was optimized using the heated model solution containing casein and lactose and UHT-treated milk. When the XTT reduction assay was applied to two kinds of UHT-treated milks under optimum conditions, the ability of each milk sample to reduce XTT significantly reflected the extent of the heat treatment as well as the evaluation method using the hydroxymethylfurfural (HMF) value. In contrast to the HMF value, the ability of UHT-treated milk gradually decreased depending upon the storage period and temperature. These results suggest not only that the present XTT assay is applicable to estimate the extent of heat treatment but also that the reducibility of the milk sample heat-treated under a given condition can serve to estimate the storage period if the storage temperature is known or vice versa. The method is much simpler (only mixing of the XTT solution containing menadione with milk sample) and quicker (about 20 min) with a satisfactory reproducibility than the conventional methods to estimate the extent of the Maillard reaction such as the lactulose or HMF determination.

Determination of Hydroxymethylfurfural in Baby Cereals by High Performance Liquid Chromatography

Abstract A liquid chromatography method for the detection and quantification of 5-hydroxymethyl-2-furaldehyde (HMF) in baby cereals is described. HMF was obtained by centrifugation and the supernatant was clarified by the addition of Carrez solution. The mixture was centrifuged for 5 min at 5,000 rpm. The samples were analysed on a reverse-phase C18 column and ultraviolet detector (284 nm) in isocratic elution with 95:5 water-acetonitrile. Average recovery of HMF by the standard addition method was 96.9%. The variation coefficients for three levels of concentration, (3.24, 22.82 and 65.50 ppm) were 2.40. 2.14 and 1.09% respectively. Limit of detection was ≥0.09 ppm. This method was applied by determination of HMF in commercial baby cereals.

Liquid Chromatographic Determination of Hydroxymethylfurfural in Fruit Juices and Concentrates After Separation on Two Columns

Abstract A liquid chromatographic (LC) method is described for the detection and quantitation of 5-hydroxymethyl-2-furaIdehyde (HMF) in fruit juices and juice concentrates. HMF is separated by chromatography in 2 dimensions with different reverse phase columns. The first column is eluted with aqueous solvents, 5% methanol-2.5% acetonitrile-1.5% tetrahydrofuran (1 + 1 + 1). By using an electrically driven, 6-port valve, the collected impure HMF fraction is rechromatographed on the second column with 5% aqueous methanol as mobile phase. The compound was detected at 284 nm under conditions selected to separate HMF in 26 min with very little or no sample preparation. On a series of samples, this method gave lower values than did the colorimetric toluidine-barbituric acid method.

Rapid HPLC Determination of Hydroxymethylfurfural in Tomato Paste

A procedure is presented for the rapid determination of hydroxymethylfurfural in tomato paste. The clear serum obtained from the ultracentrifugation of tomato paste is analyzed by high pressure liquid chromatography using a reverse phase LiChrosorb C8 column, an ultraviolet detector operated at 284 nm, and isocratic elution with water.

Effect of pasteurization, boiling, and sterilization on Buffalo milk. II. Determination of hydroxymethyl furfural (HMF), detection of maltol and changing in color

Effect of pasteurization, boiling, and sterilization on Buffalo milk. II. Determination of hydroxymethyl furfural (HMF), detection of maltol and changing in color