Proximate composition
The moisture content of the chitosan varied from 3.35% to 7.58%. It has been reported that commercial chitosan has more than 10% moisture content (
Abdel-Rahman et al., 2015). The nitrogen content of chitin and chitosan generally fall between 5-8% which makes them suitable for application in various sectors
(Nessa et al., 2011). In the present study, the chitosan nitrogen content ranged from 4.22 to 6.64%. The ash content ranged from 0.49% to 1.43%. It has been reported that high quality chitin and chitosan have ash contents of less than 1%
(Rasweefali et al., 2021). Accordingly, these results indicate the good quality of chitin used in this study. The physical and chemical properties of microwave and sundried chitosan are given in Table 1
. The drying time of chitosan under different process conditions varied from 23 to 120 min. The lowest drying time (23 min) was achieved for chitosan processed under microwave drying at 1600 watts than the sundried sample (120 min). Instrumental color analysis showed that L* (whiteness) values ranged from 71.22 to 74.70. The a* (redness) value ranged from 2.02 to 3.38. The b* (yellowness) value ranged from 16.42 to 18.57. The results indicated that sundried chitosan had a higher L* value (74.70) and lower b* (16.42) values than the others. The higher L* values observed in sun-dried chitosan indicate superior whiteness retention compared to microwave-dried samples. This may be primarily attributed to the photolytic effects of sunlight during the drying process. In addition, the gradual and mild moisture removal associated with sun drying minimizes thermal stress and suppresses browning reactions. In contrast, microwave drying involves rapid volumetric heating which may accelerate pigment degradation and browning reactions, leading to comparatively lower L* values. Therefore, while microwave drying offers improved drying efficiency and shorter processing time, sun drying appears to favor better visual quality through sunlight-induced photolytic bleaching effects
(Youn et al., 2007) .
Rasweefali et al., (2021) reported a lower L* value (68.99) for chitosan dried under sunlight. It has been reported that the color value of chitosan is influenced by the processing method, time, presence of carotenoid pigment in the shell
etc.
(Seo et al., 2007; Dornish et al., 2001).
Functional properties of microwave and sundried chitosan
Degree of deacetylation
The degree of deacetylation measures the free amino group content of the polymer chain
(Matica et al., 2019). It is one of the most important quality parameters that determines the physico-chemical and functional properties of chitosan and its application
(Shirvan et al., 2019; Knaul et al., 1998). Degree of deacetylation was used to differentiate between chitin and chitosan. Generally, the degree of deacetylation of commercial chitosan ranges from 70-95%. In this study, the degree of deacetylation ranged from 77.3%-80.8%. If the degree of deacetylation is above 70%, it is termed chitosan
(Sagheer et al., 2009). The degree of deacetylation is influenced by several factors including the species, alkali concentration, process time and temperature
(Knaul et al., 1998; El
Knidri et al., 2018; Hargono et al., 2010; Aranaz et al., 2021). The functional properties of microwave and sundried chitosan are given in Table 2.
Viscosity
Viscosity is an important functional property of chitosan that determines its industrial application. The viscosity of chitosan depends on its degree of deacetylation, molecular weight, particle size and storage time (
Chattopadhyay and Inamdar, 2010). In this study, the viscosity ranged from 828.50cP to 2117cP.
Aranaz et al., (2021) reported that viscosity increased with an increase in the degree of deacetylation. In the present study, sundried chitosan showed a lower viscosity of 828.50 cP than the microwaved dried chitosan. However, it does not follow this trend with respect to microwave power treatment. Moreover, there is a drop in viscosity for chitosan dried at1600W power. The increased viscosity observed in microwave-dried chitosan flakes may be attributed to structural and molecular modifications induced during microwave-assisted drying. Rapid volumetric heating generated by microwave energy can enhance intermolecular interactions among chitosan chains, promoting greater chain entanglement and reduced molecular mobility, which subsequently increases resistance to flow. Moreover, the accelerated moisture removal associated with microwave drying may facilitate the formation of a more compact and densely aggregated polymer network, contributing to higher apparent viscosity.
Mahmoud and Billa (2024) reported that microwave treatment can modify the physicochemical and molecular characteristics of chitosan, including its viscosity and structural organization.
Siddhartha et al., (2020) observed a decrease in the viscosity with respect to the irradiation dose. Furthermore, they reported that when the irradiation dose level is increased, depolymerization or degradation or polymer chain length is reduced, which influence the decrease in viscosity.
Water binding and Fat binding capacity
Water binding and fat binding capacity also determines chitosan applications. It has been reported that the water binding capacity of shrimp chitosan varies from 581% to 1150% (
Hossain and Iqbal, 2014). The water binding capacity of chitosan varies with the process and reaction time applied during chitosan preparation
(Mohanasrinivasan et al., 2014; Jeon et al., 2002; No et al., 2000). In the present study, the water binding capacity of chitosan varied from 169.86% to 399.65%. The highest water binding capacity was observed for the 1400W processed chitosan sample.
No et al., (2000) reported a water binding capacity of 355 to 611% for chitosan prepared from crab shells.
Rasweefali et al., (2021) observed the highest water binding capacity of 800% for deep sea mud shrimp. The difference in the water binding capacity of the samples is due to the difference in the protein content, crystallinity and amount of salt forming groups in the product (
Knorr, 1982). Unlike WBC, the fat binding capacity of chitosan also depends on the process and reaction time applied during chitosan preparation (
Hossain and Iqbal, 2014). In the present study, FBC is varied from 541.41 to 933.51%.
Rasweefali et al., (2021) observed an FBC of 700-820% for chitosan from deep sea mud shrimp. Chitosan with a high fat binding capacity can be used as a dietary ingredient and anti-cholesterolemic agent in functional food product development
(Garcia et al., 2015).
Thermal behaviour of chitosan
A DSC thermograph of chitosan dried using different drying methods is shown in Fig 1. The DSC analysis showed an endothermic peak at aaproxmately109.41°C-150.65°C which indicated evaporation of moisture content from the sample.
Garcia et al., (2015) observed a similar pattern for chitosan treated with different irradiation doses. The second thermal event exhibited an exothermic peak between 303.03°C-313.53°C. This may be due to the decomposition pattern of chitosan including the degradation of glucopyranose units and their subsequent oxidation
Garcia et al. (2015).
Andrade et al., (2012) observed a decomposition pattern for shrimp chitosan between 300-400°C. The results indicated that there was no significant change in the thermal behavior of chitosan dried under different conditions, indicating that the structural pattern of chitosan was not affected by the microwave drying process.
FTIR Structural pattern of chitosan
In the present study, all chitosan samples had similar characteristic bands (Fig 2) which indicated that there was no significant change in the structural pattern of chitosan under different drying methods. The FTIR spectrum showed a band at 3353 represent the amine group. The band at 2863 represent C-H stretching. Moreover, in the range of 1900-1660 cm
-1 range no band was observed confirming the absence of carbonyl and carboxyl groups
(Nessa et al., 2011). The presence of a band at 1646 cm
-1 indicated the presence of primary amine groups, confirming the deacetylation of chitin
(Nessa et al., 2011; Islam et al., 2014). The band at 1374 cm
-1 indicated the presence of amide III bands, C-N stretch. The absorbance at 893 and 1149 cm
-1 confirmed the presence of pyranose and the saccharide structure of chitosan
(Islam et al., 2014).