A Novel Technique to Characterize and Quantify Crystalline and Amorphous Matter in Complex Sugar Mixtures
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A Novel Technique to Characterize and Quantify Crystalline and Amorphous Matter in Complex Sugar Mixtures Pankaj Verma 1 & Narendra G. Shah 2 & Sanjay M. Mahajani 1 Received: 23 February 2020 / Accepted: 31 May 2020 # Springer Science+Business Media, LLC, part of Springer Nature 2020
Abstract Sugar-rich foods are the complex mixtures of different carbohydrates in amorphous and crystalline forms. They are mostly not in equilibrium, and transition from amorphous form to crystalline form is very likely during their storage. It is essential to know the crystalline/amorphous fraction of sugars to study these undesirable changes. The existing techniques are not adequate owing to the nonideal interactions among these sugars. In this work, we propose a novel technique, which first segregates crystals from the amorphous matter by dispersing the food material in an appropriate solvent. This is followed by separation of crystals by filtration, and further quantification and characterization by high-performance liquid chromatography, X-ray diffraction, differential scanning calorimeter and microscopy. Non-centrifugal sugar and fondant, which are mixtures of sucrose, glucose and fructose, are chosen as representative examples to demonstrate the efficacy of the proposed method. On an average, 70–90% of the sucrose in NCS samples was found to be in crystalline state. Keywords Sugar mixture . Crystallinity . Amorphous . Differential scanning calorimetry . X-ray diffraction
Introduction Sucrose, glucose and fructose are the main sugars found in most of sugar confectioneries such as fondant, hard-boiled sweets or candy, nougat, marshmallow, toffees and pharmaceutical products including tablets and lozenges. Sugars also have multiple roles in foods such as controlling the sweetness, texture, taste, colour, smell, etc. (Lee 2010). Most of the cooking processes involve mixing of ingredients, along with a cooling and/or heating treatment. These thermally treated sugar confectioneries usually have sugars in both the states—amorphous and crystalline. Amorphous sugars have a tendency to undergo crystallization and achieve thermodynamic equilibrium. In some cases, the
* Sanjay M. Mahajani [email protected] Pankaj Verma [email protected] Narendra G. Shah [email protected] 1
Department of Chemical Engineering, Indian Institute of Technology Bombay, Powai, Mumbai, India
2
Centre for Technology Alternatives in Rural Areas, Indian Institute of Technology Bombay, Powai, Mumbai, India
crystalline matter may also undergo state/phase transition leading to the formation of amorphous matter with solvent evaporation, dissolution or by quenching (Saavedra-Leos et al. 2012). Therefore, it is necessary to study these transitions to maintain the desired quality of the final product. The challenges that are encountered in these studies are related to sample preparation, crystal/amorphous separation, inability to detect amorphous matter below a limit, crystal defects, etc. (Bhandari and Hartel 2002; Lappalainen et al. 2006; Miller and Hartel 2015). S
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