Development of an Assay to Determine the Amount of Ca-Fatty Acid Soaps in Feces

Background The quantification of fecal Ca-fatty acid soaps is important to understand how fatty acids behave in the gastrointestinal tract. Objective As current methods to extract Ca-fatty acid soaps from feces give low recoveries an accurate assay to determine the amount of fatty acid soaps in feces was developed. Method Ca-fatty acid soaps are determined indirectly after non-soap fatty acid compounds have been extracted from the feces. Synthetic Ca-fatty acid soaps of different chain lengths (C12–C18) and degree of saturation (C18:0–C18:2) were incubated with several solvents to find the solvents that least-solubilize the Ca-fatty acid soaps. A three-step extraction was devised using extractions with hexane, hexane-isopropanol and water either at room temperature or at 60°C, 37°C, or 80°C, respectively. Feces were spiked with free fatty acids, Ca-fatty acid soaps, Na-fatty acid salts, and phospholipids. Results All of the free fatty acids and phospholipids and almost all of the Na-fatty acid salts were removed and 98% of Ca-lauric acid soap, 99% of Ca-stearic acid soap, and 93% of oleic acid soap were recovered. Conclusions The method is suitable for determining fatty acids in the form of Ca-fatty acid soaps in feces. Highlights New method to determine fecal Ca-fatty acid soaps. Consistent and high recovery of fatty acid-soaps.

Infrared chemical mapping of degradation products in cross-sections from paintings and painted objects

Paintings and painted objects are quite susceptible to degradation, as paint layers are usually composed of complex mixtures of materials that can participate in chemical degradation processes. The identification of the constituent materials in paint (including binders, pigments, and fillers) and the degradation products within paint layers is of particular importance to ensuring the conservation of paintings, by providing important information both about their material history as well as their state of conservation. Metal fatty acid salts (metal soaps) are degradation products that can form in situ from interactions between inorganic pigments and free fatty acids in oil-based binding media, and can cause significant condition issues in paintings. Fourier transform infrared (FTIR) spectroscopy is one of the leading analytical techniques for the study of metal soaps. In this article, the materials analysis of several cross-sections from paintings and painted objects from works in Canadian collections is presented. Recent results on the use of external reflection FTIR (R-FTIR) spectroscopy to identify and map the distribution of paint components and metal soap degradation products is presented. In particular, zinc, lead, calcium, and copper fatty acid salts were all readily identified in paint cross-sections by R-FTIR spectroscopy, along with several pigments and the oil binding medium. The results shown here are among the first detailed examinations of these metal soaps in paint cross-sections using R-FTIR spectroscopy. The use of highly polished samples in which specular reflection is dominant allowed for spectral transformations to be applied to generate transmission/absorption-like spectra which facilitated identification of these species. The distribution of these species across the cross-sections was mapped by integrating characteristic absorption features in the R-FTIR spectra. Attenuated total internal reflection (ATR) FTIR spectroscopy was also performed on several samples, which provided additional compositional details at the interface of paint layers and degradation products.