In this book, two modified QuEChERS methods based on sol-gel hybrid MTMOS-TEOS and Al2O3 as a new/alternative dSPE sorbent materials to PSA for determination of acrylamide in Sudanese food using direct GC-MS in SIM mode and UHPLC-Orbitrap-MS analysis respectively were successfully developed and first reported. Work using QuEChERS method based on sol-gel hybrid MTMOS-TEOS as dSPE material followed by GC-MS analysis gave comparable results to those obtained from previous studies using PSA as clean-up sorbent. Acrylamide was detected in fried potato and fried eggplant but taamia, minnan, ab.rae/hilumur and gorassa were free from acrylamide. Precursors of acrylamide (amino acids and reducing sugars) were determined in Sudanese foods raw materials. An inexpensive CE-UV method with NBD-Cl as pre-column derivatization agent was proposed for separation and determination of amino acids in food samples. Various derivatization conditions were optimized and then the method was validated. Also the levels of reducing sugars fructose, glucose, sucrose and maltose were determined in foods using HPLC-RI.