REV. CHIM. (Bucharest) ♦ 66 ♦ No. 2 ♦ 2015 http://www.revistadechimie.ro 265 Study of Solid - State Behaviour of Some Human Gallstones CODRUT IVAN 1 , IONUT LEDETI 2 *, GABRIELA VLASE 3 , TITUS VLASE 3 , ADRIANA FULIAS 2 , SORIN OLARIU 1 1 University of Medicine and Pharmacy “Victor Babeº”, Faculty of Medicine, Department of Surgery II, First Surgical Clinic, 2 Eftimie Murgu Sq., 300041, Timiºoara, Romania 2 University of Medicine and Pharmacy “Victor Babeº”, Faculty of Pharmacy, Department of Pharmacy I, E2 Eftimie Murgu Sq., 300041, Timiºoara, Romania 3 West University of Timisoara, Research Centre for Thermal Analysis in Environmental Problems, 16 Pestalozzi Str., 300115, Timisoara, Romania This study presents the results obtained after analysis of solid-state behaviour of eight samples of gallstones from human subjects by the use of instrumental techniques, namely thermal analysis, FTIR spectroscopy and PXRD patterns. Keywords: biliary stone, gallstone, cholesterol, thermal analysis; FTIR spectroscopy PXRD * email: ionut.ledeti@umft.ro Cholelithiasis is nowadays considered a frequent disease which is affecting a considerable large group of patients all over the world. The crystalline and/or semicrystalline concretions formed by aggregation of bile components within the gallbladder are usually known as gallstone (GS). As solid compounds, these gallbladder-formed calculi can distally pass into other regions of the biliary system, such as the cystic duct, common bile duct, pancreatic duct or the hepatopancreatic ampulla and in cases of severe inflammation, GS can determine an obstruction of ileus [1,2]. Along the medical problems created due to mechanical obstruction, in some cases GS can induce a medical condition known as acute cholecystitis [3] which is an inflammatory phenomena usually associated with infections by microorganisms such as Enterobacter, Klebsiella, Escherichia coli and Bacteroides species [4]. Other risks, beyond obstruction of bile ducts [5] associated with the formation and development of gallstones include ascending cholangitis or pancreatitis [6]. These medical conditions are nowadays considered emergencies that can be life-threatening [7]. Regarding chemical composition (both qualitative and quantitative), GS are mainly consisting in cholesterol (CH), with a content between 41 and 100%, the average being around 86.3% [8]. The human gallstones are generally multifaceted, mulberry shaped, ovoid or even spherical, while the texture can be regular or irregular. The colour of the stones is dependent in the content of pigments, varying from pure white to black. Generally, situations of local pigmented centres or layers were observed. Cholesterol (CH) is an endogenous sterol ((3β)-cholest- 5-en-3-ol) produced by biosynthesis, but as well introduced in human body by intake of food. CH is a precursor for the biosynthesis of steroid hormones, vitamin D and bile acids. The chemical structure of CH is presented in figure 1. The analysis of qualitative/quantitative composition of biliary calculi was previously reported by the use of instrumental techniques, such as thermal analysis (TG/ DTG/DTA data, DSC data) and scanning electron microscopy (SEM) [8], X-ray diffraction (XRD) [9] and FTIR spectroscopy [10]. However, literature data is poor in reporting the use of these analysis techniques for gallstones comparative to those reported for urinary calculi. Our research group employed analysis of biological samples [11], potential active compounds [12-17] and pharmaceuticals [18-23], by thermal analysis and spectroscopic techniques. In this study, we set our goal in the analysis by thermal analysis, FTIR and PXRD of eight samples of human gallstones collected from six subjects. Experimental part Materials and methods Gallbladder stones (GS) were collected intraoperative from six patients of different ages hospitalized at the Department of Surgery II, First Surgical Clinic (Timiº). All the analyses were carried out with patients agreement. In order to keep the confidentiality of identities, the samples were labelled as Gallbladder stones (GS), from GS1 to GS8. The samples were selected from a collection of gallstones, extracted from patients, as presented in table 1: All the samples were washed with an ethanol–water mixture and then dried at about 40°C for 24h. All the stones were identically processed, namely were mechanically crushed, milled and sieved, then kept in closed recipients until the analysis were carried out. The FTIR spectra were recorded using UATR technique, on the Perkin Elmer SPECTRUM 100 spectrometer using over 4000-650 cm -1 spectral range, after a number of 16 acquisitions. The powder X-ray diffraction was carried out using a Rigaku Ultima IV instrument operating at 40kV and 40 mA. The X-ray diffraction patterns were recorded using the monochromated CuK α radiation. The thermal behaviour of the samples (TG/DTG/HF) was recorded on a Perkin-Elmer DIAMOND device. Samples between 5.50-7.50 mg were heated in aluminum crucibles, from ambient temperature up to 550°C using a heating rate β=10 °C·min -1 , under a dynamic flow of synthetic air (100 mL·min -1 ). HO H H H Fig. 1. The chemical structure of cholesterol (CH)