Amino Acid Fingerprinting of Authentic Nonfat Dry Milk and Skim Milk Powder and Effects of Spiking with Selected Potential Adulterants.

A collaborative study was undertaken in which five international laboratories participated to determine amino acid fingerprints in 39 authentic nonfat dry milk (NFDM)/skim milk powder (SMP) samples. A rapid method of amino acid analysis involving microwave-assisted hydrolysis followed by ultra-high performance liquid chromatography-ultraviolet detection (UHPLC-UV) was used for quantitation of amino acids and to calculate their distribution. The performance of this rapid method of analysis was evaluated and was used to determine the amino acid fingerprint of authentic milk powders. The distribution of different amino acids and their predictable upper and lower tolerance limits in authentic NFDM/SMP samples were established as a reference. Amino acid fingerprints of NFDM/SMP were compared with selected proteins and nitrogen rich compounds (proteins from pea, soy, rice, wheat, whey, and fish gelatin) which can be potential economically motivated adulterants (EMA). The amino acid fingerprints of NFDM/SMP were found to be affected by spiking with pea, soy, rice, whey, fish gelatin and arginine among the investigated adulterants but not by wheat protein and melamine. The study results establish an amino acid fingerprint of authentic NFDM/SMP and demonstrate the utility of this method as a tool in verifying the authenticity of milk powders and detecting their adulteration.

Validation of the Biofish-300 SUL Enzymatic Biosensor for the Detection of Sulfite in Crustacean.

Background: Sulfites are some of the oldest and most widespread preservatives in our food supply. They are food additives that have antioxidant properties, but they are also recorded as allergens by the main international regulatory bodies on food safety because of their adverse health effect. Hence, sulfites maximum concentration in foodstuff is regulated and they must be ensured by the agro-food processing industries. The most widely used technique for the quantification of sulfites is the Modified Monier-Williams (AOAC Official Method 990.28). Objective: In this method, SO2 is released from sulfites and some bound compounds when the sample is mixed with an acid (normally hydrochloric acid, but sometimes phosphoric acid) and heated. The SO2 is distilled using a stream of nitrogen gas, which carries the gaseous SO2 into an absorbing solution of hydrogen peroxide (H2O2) where it is oxidised to sulphuric acid. The amount of SO2 distilled into the H2O2 is determined by titration with 0.1M sodium hydroxide. Apart from being time consuming (at least 2 h) and the usage of toxic solvents, the method presents some other disadvantages that make it inappropriate as a routine-control technique for the agro-food industry. Hence, the industry demands simple, fast and accurate methods for sulfite level monitoring. Methods: BIOLAN is a SME that develops and commercializes biosensors for quantitative analysis of food quality and safety parameters, based on its proprietary enzyme-based electrochemical biosensor technology platform. This technology enables high accurate and robust analysis with a compact device that help the users to control the quality in an easy and safety manner. Biofish-300 SUL method is a highly specific enzimatic biosensor for the rapid quantification of sulfite, measured as SO2 content, in crustaceans. It consists on the extraction of sulfite in an aqueous based solution, by the aid of an Ultra-turrax or similar, and its subsequent quantification by the biosensor after previous calibration (3 min). Results: Sulfite in raw shrimp head-on, raw shrimp head-off, and boiled shrimp was analyzed, and performance was examined using naturally contaminated and spiked samples by comparisons with AOAC Official Methods of AnalysisSM (OMA) 990.28. Linearity, selectivity, matrix, consistency, and robustness were evaluated. All results were within acceptable ranges except robustness, which reflected deviation in the sample volume and ultraturrax time compared with the standard assay procedures described in the Biofish 300 SUL Instruction Manual. Accuracy, assessed as a comparison of the Biofish results with the OMA results, ranged from 82 to 115% in all samples except for fortified raw shrimp head-on, in which the low level yielded an accuracy of 138%. The method bias was in general negative in both incurred and fortified high levels, and slightly positive in incurred low levels. Repeatability was very good as shown by the low RSDr values, demonstrating acceptable repeatability precision with results <10% in most of the evaluated values. Regression analyses showed a good correlation between the Biofish and OMA methods with R² = 0.99 in all cases. Conclusions: As a whole, accuracy, recovery and bias within range results indicate that the kit provides accurate and precise sulfite quantification for all the evaluated matrices, confirming that sample preparation and assay procedures produce acceptable results. Biofish 300 SUL has proved to be a suitable tool for monitoring sulfite levels in quality control routines due to its high accuracy, precision, rapid response and ease of use. Highlights: With a simple sample preparation, results are obtained in approximately 3 min, making a big difference with other technologies that require specific skills or tedious sample pretreatments and analysis procedures.

Total Folate in Infant Formula and Adult Nutritionals by Trienzyme Extraction and LC-MS/MS Quantitation: A Multilaboratory Testing Study, Final Action 2011.06.

Background: The need for an updated reference method for folate was identified as a priority by the AOAC's Stakeholder Panel on Infant Formula and Adult Nutritionals (SPIFAN) in 2011. An Expert Review Panel (ERP) found AOAC Official MethodSM 2011.06 suitable for the purpose and approved it as a First Action Official Method. Objective: To determine the repeatability and reproducibility of Method 2011.06: Total Folate in Infant Formula and Adult Nutritionals by Trienzyme Extraction and LC-MS/MS Quantitation. Methods: A multilaboratory collaborative study was conducted. Eleven laboratories located in five countries participated and completed analysis of all multilaboratory testing (MLT) samples. The study was divided into two parts. In the first part, the laboratories analyzed two practice samples (blindly coded) using the updated folate Method 2011.06. The laboratories providing results within the expected range qualified for part two, in which they analyzed 11 MLT samples in blind duplicates. Results: The results were compared with the Standard Method Performance Requirements (SMPR 2011.006) established for folate. The precision results met the requirements stated in the SMPR for all of the samples. Repeatability and reproducibility relative standard deviations ranged from 3.5 to 6.6 and from 9.0 to 15.7%, respectively. Horwitz ratio values for all of the samples were well below 2 (0.61-1.06). Conclusions: The ERP determined that the method performance met the SMPR requirements in September 2017 after reviewing the presented MLT data. Highlights: The ERP recommended the method for Final Action status.