Blood screening is a fundamental part of disease diagnosis and monitoring health. Attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy offers an innovative solution to streamlining the process, especially for multianalyte detection in aqueous samples. However, samples always undergo a storage phase before they are processed for testing and blood transfusion. In this study, we investigated the effect of standard storage procedures on the macromolecular composition of whole blood, and plasma collected in blood tubes for diagnostic purposes and initial screening of blood products. Periphery blood samples were collected from 10 volunteers and then stored for 14 days at 4 °C. Samples were stored as isolated plasma and whole blood to provide three different datasets, namely: (1) plasma stored independently, (2) plasma stored with other blood components and (3) whole blood. ATR-FTIR spectra of aqueous blood were acquired every 24 h from the time of collection on a portable ATR-FTIR spectrophotometer to monitor the evolution of the macromolecular composition in each blood component. Principal component analysis (PCA), partial least squares regression (PLS-R) and multi-curve resolution alternate least squares (MCR-ALS) models were built to study changes in the spectra with the storage time and identify the key bands. Isolated plasma stored without red blood cells (RBCs) showed no changes over the 14 day period indicating limited degradation. By contrast, plasma stored with the other blood components showed visual and spectroscopic signs of degradation including increasing lipid bands and the amide I and II bands from haemoglobin (Hb). Ideally, for the application of IR spectroscopy in blood diagnostics and for initial screening of blood products, whole blood and isolated red blood cells can be stored for a maximum of 4 days at 4 °C in lithium-heparin anticoagulant tubes prior to spectral analysis before any signs of degradation. Isolated plasma, on the other hand, can be stored for much longer periods and shows no evidence of degradation in the spectra after 14 days.