Biscuit Testing

Faraji, M., Hamdamali, M., Aryanasab, F., & Shabanian, M. (2018). Journal of Chromatography A, 1558, 14-20.

A method was developed for the determination of polyacrylamide (AA) in bread and biscuit samples, utilizing ultrasonic-assisted extraction, 2-phthalothiol derivatization, and dispersive liquid-liquid microextraction. This method serves as a simple and sensitive sample preparation technique for high-performance liquid chromatography (HPLC) analysis of AA. Under optimal conditions for derivatization and microextraction, the method produced a linear calibration curve spanning 10 to 1000 µg L⁻¹, with a determination coefficient (R²) of 0.9987. The limits of detection (LOD) and quantitation (LOQ) are 3.0 and 9.0 µg L⁻¹, respectively. The within-day (n=6) and between-day (n=3) precision of AA extraction and determination, based on relative standard deviation percentage (RSD%), is less than 9.0% at AA levels of 50 and 500 µg L⁻¹. Finally, the method was evaluated for the determination of AA in selected bread and biscuit samples, yielding satisfactory results (relative recovery greater than 90%).

Wu, C., Wang, L., Guo, X., Li, H., & Yu, S. (2019). Food Control, 105, 64-70.

A method based on ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was developed and validated for the simultaneous analysis of 4(5)-methylimidazole (4-MI) and acrylamide (AA) in biscuit products. Samples were extracted with methanol and then purified using primary secondary amine (PSA) dispersive solid-phase extraction. The analytes were separated by reversed-phase liquid chromatography, detected by tandem mass spectrometry in multiple reaction monitoring (MRM) mode, and quantified using deuterium-labeled internal standards d6-4-MI and d3-AA. The method was validated for linearity, limit of quantification, precision, accuracy, and measurement uncertainty. All calibration curves showed good linearity (R² > 0.999). The average recoveries of the analytes ranged from 93% to 108%, with a coefficient of variation of less than 9.2%. The limits of quantification for 4-MI and AA were 5 ng/g and 10 ng/g, respectively. The expanded measurement uncertainties for these compounds were less than 19%. Finally, the method was applied to the analysis of 17 commercially available biscuit samples, revealing the widespread presence of 4-MI and AA in biscuit products.