Determination Of Acrylamide In Foods Research Articles

An ultrasensitive liquid crystal aptasensing chip assisted by three-way junction DNA pockets for acrylamide detection in food samples

Acrylamide, an unsaturated amide found in heat-processed foods, poses serious risks to human health due to its neurotoxicity, carcinogenicity, and genotoxicity. This highlights the importance of quantitative determination of acrylamide in foods and the environments to ensure public health safety. Therefore, there is an urgent need for simple, rapid, and highly sensitive methods to accurately quantify acrylamide. In the present study, a user-friendly aptasensor was designed to quantify ultra-low levels of acrylamide in nuts for the first time. This innovative approach utilizes chemical engineering of a glass slide as a portable sensing platform, which incorporates liquid crystal (LC) molecules and a three-way junction (TWJ) DNA pocket. The immobilized TWJ pocket can disrupt the vertical alignment of LCs, turning the dark polarized background of the aptasensor to a colorful state. The binding of the specific aptamer to acrylamide disrupts the TWJ structure, enabling the LCs to return to their homotropic alignment. This structural change restores the dark polarized view of the sensing platform. The TWJ-engineered LC aptasensor effectively detects ultra-low concentrations of acrylamide in the range of 0.0005 to 50 fmol/L, with a detection limit of 0.106 amol/L. The aptasensor was successfully applied to real roasted nut samples, including peanut, almond, pistachio, and hazelnut, achieving recovery values ranging from 96.84 % to 99.61 %. With its simplicity, portability, ease of use, and cost-effectiveness, this aptasensor is a powerful sensing device for food safety monitoring.

A ratiometric fluorescent “off-on” sensor for acrylamide detection in toast based on red-emitting copper nanoclusters stabilized by bovine serum albumin

Acrylamide, as a Class 2A carcinogen, poses serious threats to human health. To achieve rapid and accurate determination of acrylamide in food, a ratiometric fluorescent “off–on” sensor was designed by incorporating red-emitting copper nanoclusters and glutathione. Copper nanoclusters with bimodal emission at 395 nm and 650 nm (excited at 310 nm) were synthesized by using bovine serum albumin as the ligand and ascorbic acid as the reductant. With glutathione addition, the fluorescence intensity at 650 nm gradually decreased, while the case at 395 nm slightly increased. The quenched fluorescence at 650 nm was subsequently restored by acrylamide through thiol-ene Michael addition reaction between acrylamide and glutathione. The constructed sensor showed excellent performance towards acrylamide detection in the range of 5–300 μM with a detection limit of 1.48 μM, and was further applied to real-sample detection of acrylamide in toast and exhibited good recoveries (90.29–101.30 %), indicating potential applications of this sensor.

Towards a consensus LC-MS/MS method for the determination of acrylamide in food that prevents overestimation due to interferences

ABSTRACT Acrylamide is prone to misquantification, and critical steps in the analytical procedures need to be identified and controlled to ensure a reliable determination. Four methods were considered to illustrate misquantification issues with acrylamide. For two methods varying by the extent of their sample preparations, cases of overestimation in cocoa samples reaching up to a 20-fold factor are shown. A second example, applied to a variety of food products, includes two other methods varying by their chromatographic conditions. As a follow up of a study conducted in 2020 about the identification of N-acetyl-ß-alanine as an interference of acrylamide in coffee, the extent of this interference was evaluated in a selection of coffee samples, cereal-based products and baby foods. The ultimate objective of this manuscript was to resolve such cases of misquantification and validate a wide scope and robust method allowing an interference free acrylamide analysis. To do so, an extraction procedure based on the EN 16618:2015 standard with water extraction and two consecutive solid phase extraction (SPE) steps was applied with modified liquid chromatographic conditions. The method was validated in coffee, cereals, baby foods, cocoa and pet foods with excellent performance in terms of recovery (97–108%) and precision (RSDr and RSDiR <12 %). The breath of scope was further proved through trueness determination in quality control materials and reference materials including French fries, potato crisps, vegetable crisps, instant coffee, infant food and biscuit (cookie), with trueness values found within a 94–107% range.

Biomedical rationale for acrylamide regulation and methods of detection.

Acrylamide is the product of the Maillard reaction, which occurs when starchy, asparagine-rich foods including potato or grain products and coffee are fried, baked, roasted, or heated. Studies in rodents provide evidence that acrylamide is carcinogenic and a male reproductive harmful agent when administered in exceedingly high levels. A 2002 study identified acrylamide in popular consumer food and beverage products, stimulating the European Union (EU) and California to legislate public notice of acrylamide presence in fried and baked foods, and coffee products. The regulatory legislation enacted in the EU and California has scientists working to develop foods and processes aimed at reducing acrylamide formation and advancing rapid and accurate analytical methods for the quantitative and qualitative determination of acrylamide in food and beverage products. The purpose of this review is to survey the studies performed on rodents and humans that identified the potential health impact of acrylamide in the human diet, and provide insight into established and emerging analytical methods used to detect acrylamide in blood, aqueous samples, and food.

Determination of acrylamide in foods by automatic accelerated solvent extraction and gas chromatography-mass spectrometry

AbstractThe aim of the experiment is to establish a method for the determination of acrylamide in food by automatic accelerated solvent extraction-gas chromatography-mass spectrometry. D3-acrylamide was used as isotope internal standard, crushed samples were extracted and purified by automatic accelerated solvent, acrylamide was derivatized into 2,3-dibromopropanamide by potassium bromide and potassium bromate under acidic conditions, and then the derivative was extracted by ethyl acetate and detected by gas chromatography-mass spectrometry. The method had a good linear relationship in the concentration range of 10–2000 ng/mL, and the coefficient of determination (R2) was 0.9997. The detection limit of the method was 3 μg/kg. The quantification limit of the method was 10 μg/kg. The standard addition recovery of acrylamide was between 105 and 120%, and the relative standard deviation of the recovery of acrylamide was less than 3.0%. The experimental result showed that the method was simple, sensitive, efficient and accurate, and could be used for the determination of acrylamide in food.

Review of Research into the Determination of Acrylamide in Foods.

Acrylamide (AA) is produced by high-temperature processing of high carbohydrate foods, such as frying and baking, and has been proved to be carcinogenic. Because of its potential carcinogenicity, it is very important to detect the content of AA in foods. In this paper, the conventional instrumental analysis methods of AA in food and the new rapid immunoassay and sensor detection are reviewed, and the advantages and disadvantages of various analysis technologies are compared, in order to provide new ideas for the development of more efficient and practical analysis methods and detection equipment.

Determination of acrylamide in food using a UPLC–MS/MS method: results of the official control and dietary exposure assessment in Cyprus

ABSTRACTThe determination of acrylamide in potato products, bakery products and coffee, and the human dietary exposure is reported. The method reported is based on a single extraction step with water, followed by the clean-up of the extract using solid phase extraction columns and finally, the determination of acrylamide using UPLC–MS/MS. The MS/MS detection was carried out using an ESI interface in positive ion mode. Internal calibration was used for the quantification of acrylamide, because of the suppression/enhancement matrix effects due to the complex nature of the samples. The method performance characteristics were determined after spiking blank samples. The mean recoveries in spiked coffee samples, potato chips, breakfast cereals and crispbread ranged from 93% to 99%, with RSDs lower than 5% for both repeatability and reproducibility conditions. The estimated limits of detection and quantification of the method were 10 and 32 μg kg−1, respectively. The method was used for monitoring acrylamide in 406 samples. Acrylamide amounts ranged from <32 to 2450 μg kg−1. A total of 360 samples (89%) were contaminated with acrylamide, but only 14% of the samples exceeded the benchmark levels of the EU legislation. Foods with the highest mean acrylamide amounts were potato crisps (642 μg kg−1), French fries (383 μg kg−1) and biscuits (353 μg kg−1). The mean and 95th percentile acrylamide exposures of adolescents in Cyprus were 0.8 and 1.8 μg kg−1 body weight per day, respectively. The estimated levels of dietary exposure to acrylamide are not of concern with respect to neurotoxicity. However, the margins of exposure (MOEs) indicate a concern for carcinogenicity. Potato fried products (45%), fine bakery ware (21%) and potato chips (14%) contributed the most to overall acrylamide exposure.

Direct determination of acrylamide in food by gas chromatography with nitrogen chemiluminescence detection

A method of gas chromatography with nitrogen chemiluminescence detection and using standard addition is described for the determination of acrylamide in heat-processed foods. Using a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) sample preparation method removes the acrylamide precursors completely, and the risk of overestimating acrylamide concentration due to additional analyte formation in the hot gas chromatograph inlet is also avoided. Sample preparation is rapid and inexpensive. A Deans switch device is utilized to heart-cut acrylamide and to prevent interferences from the solvent and matrix from reaching the detector. The pre-column is backflushed at high temperature to maintain a clean baseline and shorten the cycle time compared to baking out the column. Quantitation using standard addition is employed for compensation of potential variability in the acrylamide extraction efficiency in acetonitrile. The limit of detection and the limit of the quantification obtained for this method are 27 and 81 μg/kg, respectively, in food samples (equivalent to 3.5 and 10.6 μg/L in acetonitrile, respectively), and the linear range is 76-9697 μg/kg in food samples (equivalent to 10-1280 μg/L in acetonitrile) with an R(2) value of 0.9999.

DETERMINATION AND SEPARATION MECHANISM OF ACRYLAMIDE BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

High-performance liquid chromatography using the negative peak method was developed for the determination and separation of acrylamide in food with methanol-water containing a background reagent of 0.01 mmol L−1 5-sulfosalicylic acid (15/85, v/v) as the mobile phase with an ultraviolet-visible detector (λsig = 320 nm, λref = 210 nm). The method was simple, the correlation coefficients exceeded 0.9990, and the limit of detection for acrylamide was 0.07 μg kg−1. The concentrations of acrylamide in food were between 81 and 910 μg kg−1. The recoveries were greater than 81.0% and the relative standard deviation was between 0.24 and 3.6%. The results showed that this method was suitable for the determination of acrylamide in food.

Determination of acrylamide in food using adsorption stripping voltammetry

A new electroanalytical method for the determination of acrylamide in food has been developed. It was found that a complex of acrylamide and Ni&lt;sup&gt;2+&lt;/sup&gt; is suitable for the electrochemical determination of acrylamide. Ammonia buffer of pH&amp;nbsp;= 9.5 was found to provide convenient conditions for the determination. optimal concentration of Ni&lt;sup&gt;2+&lt;/sup&gt; was 500&amp;nbsp;&amp;micro;mol/l. The sample preparation procedure was optimised. The best results were found for an ethanol/water mixture (1:2) and pH = 1.4. The samples were extracted in an ultrasound bath, and after centrifugation 0.2 ml of the extract was taken for the measurement. Voltammetric measurements were done using the hanging mercury drop electrode. The peak height was a function of acrylamide concentration and deposition time. The accuracy of the method was verified by the use of standard reference materials. &amp;nbsp;

Validation of a novel derivatization method for GC–ECD determination of acrylamide in food

This paper proposes a new method for quantitative analysis of acrylamide in cereal-based foods and potato chips. The method uses reaction with trifluoroacetic anhydride, and analyses the resulting derivative by use of gas chromatography with electron-capture detection (GC-ECD). The effects of derivatization conditions, including temperature, reaction time, and catalyst, on the acylation reaction were evaluated. Chromatographic analysis was performed on an SE-54 capillary column. Under the optimum conditions, good retention and peak response were achieved for the acrylamide derivative. The analytical method was fully validated by assessment of LODs and LOQs (1 ng g(-1) and 25 ng g(-1), with relative standard deviations (RSD) 2.1 and 3.6, respectively), linearity (R = 0.9935 over the range 0.03-10 μg g(-1)), and extraction recovery (>96%, with RSD below 2.0, for acrylamide spiked at 1, 20, 50, and 100 ng g(-1); 99.8% for acrylamide content >1000 ng g(-1)). The method requires no clean-up of the acrylamide derivative before injection. The method has been successfully used to determine acrylamide levels in different commercial cereal-based foods, French fries, and potato chips.

Determination of acrylamide in dry feedstuff for dogs and cats

Acrylamide is considered to be an endogenous contaminant of food and feedstuff. Attention is paid to the acrylamide content in human nutrition products; however, there is lack of data about its concentrations in feedstuff. The aim of this study was to use a newly developed adsorptive stripping voltammetry procedure for determination of acrylamide concentrations in five and three different kinds of dog and cat dry feedstuff, respectively. The applied analytical procedure consists of a solvent extraction in ultrasound bath, followed by voltammetric measurement at the hanging mercury drop electrode in ammonia buffer. The accuracy of the method was verified by use of standard reference materials. The range of acrylamide concentration found in samples of dry dog and cat feedstuff ranged from 106 to 358 μg/kg, and from 66 to 269 μg/kg, respectively. The precision of analyses expressed in form of the relative standard deviations ranged between 0.6–1.7%. The voltammetric procedure appears to be a reliable, sensitive, rapid and low-cost analytical technique for the determination of acrylamide in food and feedstuff. The concentrations of acrylamide found in feedstuff were relatively moderate but it is undoubtedly necessary to monitor its concentrations in future.

Computer vision-based image analysis for rapid detection of acrylamide in heated foods

Background and Aim High concentrations of acrylamide found in common fried and baked foods attained considerable public concern since it has been classified as a probable human carcinogen. Many analytical methods have been published for the determination of acrylamide in foods. Although these methods perform well for quality control purposes in a food analysis laboratory, they are laborious, costly, and cannot be adopted for process control purposes by the food industry. This study describes a computer vision-based image analysis algorithm using color segmentation for the prediction of acrylamide level in thermally processed foods. Materials and Methods Laboratory made experimental potato crisps and cookies were prepared by frying and baking, respectively. The digital images of potato crisps and cookies were used to extract a meaningful browning parameter. Results and Conclusion The digital images were analyzed using a semiautomatic segmentation algorithm to calculate the browning ratio of potato crisps and cookies. The calculated browning ration were successfully correlated with acrylamide level of cookies and potato crisps. So, it was possible to predict the levels of acrylamide in test samples by means of their browning ratio values. The image analysis technique described here can be used as an online process control tool for frying and baking industry. Gökmen V & Mogol BA (2010). Computer vision-based image analysis for rapid detection of acrylamide in heated foods. Quality Assurance and Safety of Crops & Foods, 2, 203–207.

Determination of acrylamide in food by gas and liquid chromatography-mass spectrometry

Acrylamide in food was determined by gas chromatography - mass spectrometry (GC-MS) after bromination of acrylamide and underivatized acrylamide was quantified by ultra performance liquid chromatography -mass spectrometry (UPLC-MS). Two different sample preparation methods were used and optimised. The GC-MS method was used for various food matrices like breads, potato crisps, potato crackers, french fries. The UPLC-MS method was used for analysis of coffee. The limit of detection and limit of quantification for acrylamide were 7 µg.kg-1 and 20 µg.kg-1 by GC-MS, 9 µg.kg-1 and 30 µg.kg-1 by UPLC-MS. For both methods the reproducibility, given as relative standard deviation was &lt; 5% , and the recovery was close to 100 %.

Development of Two Certified Reference Materials for Acrylamide Determination in Foods

Certified reference materials (CRMs) are a versatile tool for quality assurance in the chemical laboratory. In the case of acrylamide analysis, the availability of appropriate materials was rather limited. This lack of acrylamide matrix CRMs has now been overcome by the development of two European reference materials (ERM) for the determination of acrylamide in food (crispbread, ERM-BD272, and rusk, ERM-BD274). This article describes the preparation of the materials, provides the results of the homogeneity and stability studies, and presents and discusses the outcome of the certification studies. Expert laboratories from different European countries took part in the certification studies using various analytical methods. The acrylamide mass fractions were certified to 980 microg kg(-1) for crispbread and 74 microg kg(-1) for rusk.

Multiple-stage extraction strategy for the determination of acrylamide in foods

The effects of single- and multiple-stage extraction procedures were studied on the extraction yield of acrylamide for various cereal- and potato-based thermally processed foods. In the multiple-stage procedure, extraction of ground sample was sequentially performed up to four times using 10 mM formic acid or methanol as the extraction solvents. The extraction yield of acrylamide was determined for each stage. Single-stage extraction resulted in lower acrylamide concentrations for all food matrices regardless of the type of extraction solvent, solvent-to-sample ratio, prior defatting, extraction temperature and time. The results revealed that a single-stage procedure underestimated the concentration of acrylamide in foods by a factor of up to 50% depending on the type of solvent applied during the extraction. The extractability was an exponential function which can be used to optimize the multiple extraction conditions during the analysis of foods for acrylamide. In general, the aqueous extraction using 10 mM formic acid was found to be more effective than the methanol extraction, and required lesser number of extraction steps for a complete extraction of acrylamide from food.

An improved method validation for rapid determination of acrylamide in foods by ultra-performance liquid chromatography combined with tandem mass spectrometry

An improved method was validated for the determination of acrylamide in foods using ultra-performance liquid chromatography (UPLC) coupled to eletrospray ionization tandem mass spectrometry (MS/MS) in the present study. This improved method supplies a rapid quantitative procedure of acrylamide with a run time of only 3 min. Results showed a good repeatability (RSD ≤ 4.5%) with 50, 100, 250, 500 and 1000 μg/kg spiked concentrations in potato crisps in within-day ( n = 5) and day-to-day ( n = 10) precision tests. Meanwhile, good recoveries (81.6–99.0%) were obtained with the same spiked concentrations in acrylamide-free cereal samples ( n = 3). The excellent method validation data and proficiency test results ( Z-score: −0.1) of the official Food Analysis Performance Assessment Scheme (FAPAS) suggested that the present quantitative method could be applied for rapid determination of acrylamide in many investigations.

Determination of acrylamide in food by solid-phase microextraction coupled to gas chromatography–positive chemical ionization tandem mass spectrometry

A method has been developed to determine acrylamide in aqueous matrices by using direct immersion solid-phase microextraction (SPME) coupled to gas chromatography–positive chemical ionization tandem mass spectrometry (GC–PCI-MS–MS) in the selected reaction monitoring (SRM) mode. The optimized SPME experimental procedures to extract acrylamide in water solutions were: use of a carbowax/divinylbenzene (CW/DVB)-coated fiber at pH 7, extraction time of 20 min and analyte desorption at 210 °C for 3 min. A detection limit of 0.1 μg L −1 was obtained. The linear range was 1–1000 μg L −1. The relative standard deviation was 10.64% ( n = 7). The proposed analytical method was successfully used for the quantification of trace acrylamide in foodstuffs such as French fries (1.2 μg g −1) and potato crisps (2.2 μg g −1).

Direct determination of acrylamide in food by gas chromatography–high-resolution time-of-flight mass spectrometry

Simple and rapid gas chromatographic (GC) method employing a high-resolution time-of-flight mass analyzer that enables direct analysis (no derivatization) of acrylamide in various heat-processed foodstuffs has been developed and validated. Co-isolation of acrylamide precursors such as sugars and asparagine, constituting the risk of results overestimation due to additional formation of analyte in hot GC injector, is avoided by the extraction with n-propanol followed by solvent exchange to acetonitrile (MeCN). Introduction of a novel purification strategy, dispersive solid phase extraction, based on addition of primary-secondary amine (PSA) sorbent into deffated extract in MeCN, provides a significant reduction of some abundant matrix co-extracts (mainly free fatty acids). Isotope dilution technique (d 3-acrylamide as an internal standard) is employed for compensation of potential target analyte losses and/or matrix-inducted chromatographic response enhancement. Limits of quantifications (LOQs) ranged between 15 and 40 μg kg −1 and recoveries were between 97 and 108% depending on the examined food matrix. The repeatability of measurements (expressed as relative standard deviation, R.S.D.) was as low as 1.9% for potato crisps containing acrylamide at a level of 1 mg kg −1. Slightly higher values (R.S.D. < 4.0%) were achieved for breakfast cereals and crisp bread with approximately 10 times lower content of this processing contaminant. Trueness of results generated by this new method was demonstrated via FAPAS ® (Food Analysis Performance Assessment Scheme) interlaboratory proficiency tests.

Determination of acrylamide in foods by pressurized fluid extraction and liquid chromatography-tandem mass spectrometry used for a survey of Spanish cereal-based foods

An automated and rapid method for the determination of acrylamide in different food products is presented. The method involves pressurized fluid extraction (PFE) of foods with acetonitrile and precipitation with Carrez reagents. The final extract is analysed by liquid chromatography coupled to electrospray ionization tandem mass spectrometry (ESI-MS-MS). The main parameters affecting the performance of ESI-MS-MS and PFE were optimized using a design of experiments approach. The limit of quantification of the method was 5 µg kg−1, and recoveries from incurred samples ranged between 93 and 101%. The accuracy was evaluated using the reference test materials FAPAS T3002, T3005 and T3011. Using the optimized method, 62 food samples of potato chips, snacks, biscuits, breakfast cereals and crisp bread sampled from Valencia, Spain, supermarkets were surveyed for acrylamide levels. The levels were similar to those reported in the European Union and USA.