Experimental design to optimization of beta cyclodextrin production from ungelatinized sago starch

The aim of this study is to produce beta cyclodextrin (β-CD) from ungelatinized, but annealed (65 °C) sago starch using cyclodextrin glucosyltransferase (CGTase). The optimization processes were conducted at three stages using Response Surface Methodology. Preliminary data have shown that the three (3) highest points for each of the studied parameters were pH, concentration of sago starch and enzyme, and also agitation. In the second stage, two level full factorial design (2ⁿ FFD) was applied to determine the significant parameters affecting the production of β-cyclodextrin. Statistical analyses showed that pH, enzyme and sago starch concentration were the significant parameters. The final stage of optimization involved the use of Central Composite Design to determine and predict the optimum yield of β-cyclodextrin. The optimum condition for production cyclodextrin was at pH 8.62 (Glycine–NaOH buffer 0.05 M), 0.65% v/v sago starch and 15% w/v enzyme concentration, where 8.43 g β-cyclodextrin/L was produced after 4 h of reaction.     

醇酸降解淀粉制备糊精的研究

采用醇酸水解大米淀粉、高直链玉米淀粉和木薯淀粉,发现：在相同条件下,正丁醇-盐酸水解的木薯淀粉溶解性最大,且在水解3 d后无显著增加。因此,从颗粒结构、晶体结构和分子结构等方面系统地研究醇酸降解木薯淀粉制备糊精过程。经正丁醇-盐酸水解后,木薯淀粉颗粒破坏程度严重,且随水解时间的增加,大部分木薯淀粉颗粒均失去了原有的颗粒形状;经正丁醇-盐酸水解7 d后,木薯淀粉的粒径下降了42.0%。X-射线衍射结果表明正丁醇-盐酸水解木薯淀粉在2θ为20°处出现了衍射峰,证明淀粉在正丁醇-盐酸水解过程中形成了直链淀粉-正丁醇络合物。高效分子排阻色谱和淀粉-碘全波长扫描分析表明：木薯淀粉经过正丁醇-盐酸水解后分子量在4 h内急剧下降,水解4 h后下降趋势减缓,水解3 d后分子量无显著变化并趋于稳定。上述结果表明,采用正丁醇-盐酸水解木薯淀粉3 d为制备糊精的最佳条件。     

Production and physicochemical properties of resistant starch from hydrolysed wrinkled pea starch

The content and physicochemical properties of resistant starches (RS) from wrinkled pea starch obtained by different molecular mass reduction processes were evaluated. Native and gelatinised starches were submitted to acid hydrolysis (2 m HCl for 2.5 h) or enzymic hydrolysis (pullulanase, 40 U g^?1 for 10 h), followed by hydrothermal treatment (autoclaving at 121 °C for 30 min), refrigeration (4 °C for 24 h) and lyophilisation. Native starch showed RS and total dietary fibre contents of 39.8% and 14.3%, respectively, while processed ones showed values from 38.5% to 54.6% and from 22.9% to 37.1%, respectively. From these, the highest contents were among acid‐modified starches. Processed starches showed endotherms between 144 and 166 °C, owing to the amylose retrogradation. Native and processed starches showed low viscosity, which is inversely proportional to the RS concentration in samples. The heat treatment promoted an increase in the water absorption index. The pea starch is a good source for obtaining resistant starch by acid hydrolysis.     

Effect of crosslinking reagents and hydroxypropylation levels on dual-modified sago starch properties

Chemical modification is usually carried out to overcome the unstable properties of native sago starch and improve its physical properties during processing. In this study, dual-modification of sago starch was carried out. The first stage of modification was hydroxypropylation, using propylene oxide at levels ranging from 6 to 12%. This was followed by crosslinking, using three different types of crosslinking agents: a mixture of sodium trimetaphosphate (STMP) and sodium tripolyphosphate (STPP), phosphorus oxychloride and epichlorohydrin. Through hydroxypropylation, it was found that there was a significant increase in molar substitution which in turn induces an increase in crosslinking and this was seen from the marked increase in phosphorus content and degree of substitution. This was accompanied by a significant decrease in paste clarity, swelling power and solubility compared to that of the native starch. Starch that was hydroxypropylated with 10–12% propylene oxide and crosslinked by a mixture of 2% STMP and 5% STPP produced modified starch with the most desirable properties in that it exhibited no viscosity breakdown, high acid resistance, high freeze-thaw stability and improved gel texture.     

Spontaneous fermentation of traditional sago starch in Papua New Guinea

Sago starch is an important dietary carbohydrate in lowland Papua New Guinea (PNG). An investigation was conducted to determine whether microbes play a role in its preservation using traditional methods. In 12 stored sago samples collected from PNG villages, lactic acid bacteria (LAB) were present (≥3.6 × 10⁴ cfu/g) and pH ranged from 6.8 to 4.2. Acetic and propionic acids were detected in all samples, while butyric, lactic and valeric acids were present in six or more. In freshly prepared sago, held in sealed containers in the laboratory at 30 °C, spontaneous fermentation by endogenous microflora of sago starch was observed. This was evident by increasing concentrations of acetic, butyric and lactic acids over 4 weeks, and pH reducing from 4.9 to 3.1: both LAB and yeasts were involved. Survival of potential bacterial pathogens was monitored by seeding sago starch with ∼10⁴/g of selected organisms. Numbers of Bacillus cereus, Listeria monocytogenes and Staphylococcus aureus fell to <30/g within 7 days. Salmonella sp. was present only in low numbers after 7 days (<36/g), but Escherichia coli was still detectable after three weeks (>10²/g). Fermentation appeared to increase the storability and safety of the product.     

Physicochemical properties and in vitro digestibility of resistant starch from mung bean (Phaseolus radiatus) starch

RS from mung bean starch was prepared by autoclaving, pullulanase debranching, and retrogradation. Physicochemical properties, crystalline structure, and in vitro digestibility of selected RS samples with different RS content were investigated. Compared to native starch, AAM content of RS increased but MW decreased greatly. SEM clearly showed RS samples exhibited irregular shaped fragments with compact structure. XRD pattern indicated that RS samples had typical B‐type pattern with sharp peaks at 17.0°, 22.2°, and 23.9° 2θ. The relative crystallinity, gelatinization temperatures, and enthalpy increased with increasing RS content. The α‐amylase digestibility of RS was lower than that of native starch. The results suggested that the decrease in enzymatic digestion of RS might due to compact and ordered crystalline structures after debranching and recrystallization.     

A facile approach for controlled synthesis of hydrophilic starch‐based nanoparticles from native sago starch

A facile approach for the preparation of hydrophilic starch‐based spherical nanoparticles from native sago (Metroxylon sagu) starch using the drop‐wise solvent exchange method was reported. Starch‐maleate monoester (SM) was initially synthesized from native sago starch and maleic anhydride in an aqueous medium, and SM nanoparticles was subsequently precipitated in absolute ethanol under controlled conditions. The present study was focused mainly on modulating of the solvent and non‐solvent systems to prepare SM nanoparticles of different morphologies. The pH of the solvent system and the nature of surfactants being added into the solvent system could influence the morphology of regenerated SM nanoparticles. SM nanoparticles of discrete and spherical shape were regenerated from a basic SM sample solution, or an acidic sample solution in the presence of an appropriate surfactant. SM nanoparticles with mean diameter of about 250 nm was obtained by precipitation in absolute ethanol in the presence of Brij 35 as the surfactant.     

Effect of Pullulanase Debranching of Sago (Metroxylon sagu) Starch at Subgelatinization Temperature on the Yield of Resistant Starch

The effects of pullulanase debranching of sago (Metroxylon sagu) starch in the granular state and subsequent physical treatments on the formation and yield of type III resistant starch (RS 3) have been investigated. Sago starch was enzymatically debranched with pullulanase at 60°C and at pH 5.0 using different enzyme concentrations (24, 30, 40, 50 PUN/g dry starch) which was added to 20% (w/v) starch slurry and incubated for 0 to 48 h. Optimum enzyme concentration of 40 PUN/g dry starch and three debranching times (8, 16 and 24 h) have been selected for subsequent preparation of RS. Granule morphology and molecular weight distribution (MWD) of the debranched and resistant starch were examined. Debranched starch samples showed blurred birefringence patterns, a decrease in amylopectin fraction, an increase in low molecular weight fraction and a broadening of MWD. Debranched starch samples with a maximum RS yield of 7% were obtained at 8 h debranching time. Temperature cycling and incubation at certain temperature and storage time enhanced the formation of RS. Under the conditions used in this study, the optimum conditions to obtain the highest RS yield (11.6%) were 8 h of debranching time, followed by incubation at 80°C for seven days. The MWD analysis showed that RS consisted of material with relatively low degree of polymerization. This study showed that pullulanase treatment of starch in the granular state resulted in limited debranching of amylopectin but the subsequent physical treatments (incubation time/temperature) can be manipulated to promote crystallization and enhance formation of RS 3.     

Producing novel sago starch based food packaging films by incorporating lignin isolated from oil palm black liquor waste

Poor mechanical and barrier properties of starch-based films can be improved by incorporating natural polymer such as lignin. In the present study, novel food packaging films were prepared by casting method from sago palm (Metroxylon sagu) starch (as film matrix with 30% w/w glycerol as plasticizer) by adding lignin isolated from oil palm black liquor waste (from empty fruit bunch), as a reinforcing material (1, 2, 3, 4 and 5% v/w). Results showed packaging films produced by incorporation of isolated lignin to improve selected thermo-mechanical and barrier properties with significant reduction in water vapor permeability, and improved water resistance and seal strength. It is concluded that lignin isolated from oil palm black liquor waste to have great potential to be explored for food packaging purposes. Moreover, this packaging film will be more economical and environmental friendly.     

Structural and physicochemical characterization of RS prepared using hydrolysis and heat treatments of chickpea starch

The aim of this study was to evaluate the production and the structural and physicochemical properties of RS obtained by molecular mass reduction (enzyme or acid) and hydrothermal treatment of chickpea starch. Native and gelatinized starch were submitted to acid (2 M HCl for 2.5 h) or enzymatic hydrolysis (pullulanase, 40 U/g per 10 h), autoclaved (121°C/30 min), stored under refrigeration (4°C/24 h), and lyophilized. The hydrolysis of starch increased the RS content from 16% to values between 20 and 32%, and the enzymatic treatment of the gelatinized starch was the most efficient. RS showed an increase in water absorption and water solubility indexes due to hydrolytic and thermal process. The processes for obtaining RS changed the crystallinity pattern from C to B. Hydrolysis treatments caused an increase in relative crystallinity due to the greater retrogradation caused by the reduction in MW. RS obtained from hydrolysis showed a reduction in viscosity, indicating the rupture of molecules. The viscosity seemed to be inversely proportional to the RS content in the sample.     

Antimicrobial,rheological, and physicochemical properties of sago starch films filled with nanorod-rich zinc oxide

The effects of zinc oxide nanorod incorporation on the flow properties of sago starch solution and antimicrobial, sorption isotherm, water vapor permeability, and UV transmission of sago starch films were investigated. The nanorod-rich ZnO (ZnO-N) was homogenized by sonication and incorporated into sago starch solutions at different concentrations (e.g. 1%, 2%, 3%, and 5% w/w dried starch). Introduction of low concentration ZnO-N to starch solutions significantly increased the viscosity of the solution and significantly decreased the permeability of the films to water vapor by less than one third. Solubility, moisture content, and monolayer water content of the films were decreased, whereas contact angle was increased with higher ZnO-N concentration. ZnO-N starch films had 0% UV transmittance and were able to absorb more than 80% of Near Infrared spectra. ZnO-N sago starch films exhibited excellent antimicrobial activity against Staphylococcus aureus. These properties suggest that ZnO nanorod has the potential as a filler in starch-based films for use as active packaging materials in the pharmaceutical and food industries.     

High yield of glucose from cassava starch hydrolysis by poly(4-vinylpyridine) hydrochloride

Cassava is an abundant and cheap source of starch which is largely used to produce sugar and dextrin. In this work, Hydrolysis of cassava starch using some active catalysts: poly(4-vinylpyridine) hydrochloride (PVP, HCl), green clay activated with HCl, Amberlyst 36, Montmorillonite KSF, zeolite and HCl were investigated. Temperature, reaction time, concentration of starch and catalyst amount were the parameters considered during each experience. The catalyst precursor (PVP, HCl) showed to be an efficient, selective, recyclable and gave a high yield of glucose syrup (82%) with 95% of total reducing sugar without pretreatment process. Reactions were carried out at 95 °C with various concentrations of starch, up to 600 g L⁻¹. The consumable glucose syrup obtained with this process was similar to the commercial reference. A small quantity (2%–3%) of 5-hydroxymethylfurfural (HMF) was the only by-product and it could be extracted with ethyl acetate. Bio-fermentation of the non-treated hydrolysate gave a good yield of ethanol (93%) after only 12 h.     

Molecular characteristics of native sago starch and isolated fractions determined using asymmetrical flow field‐flow fractionation

The apparent average molar masses (M_w,app), apparent average radii of gyration (R_g,app), of native sago starch and fractions were determined using asymmetrical flow field‐flow fractionation coupled with multi‐angle light scattering and refractive index detectors (AF4/MALS/RI). Amylose‐type (Fraction A) and amylopectin‐type (Fraction B) were chemically separated from native sago starch. Native sago starch and Fractions (A–B) were dissolved in 1M KSCN using a high pressure microwave vessel. The effect of varying cross flow rates at a fixed channel flow rate upon the M_w,app and R_g,app distributions of native sago starch and Fractions (A–B) were investigated. The average M_w,app values of native sago starch, Fraction (A) and Fraction (B) were 60 × 10⁶, 1.5 × 10⁶ and 60 × 10⁶ g/mol, respectively, with average R_g,app values of 142, 75 and 127 nm, respectively. The sphere‐equivalent hydrodynamic radii (R_h) values for native sago starch and fractions were determined from AF4 experimental parameters.     

Enzymic Extraction of Native Starch from Sago (Metroxylon sagu) Waste Residue

Residual native starch was extracted from sago pith residue using two types of commercial cell‐wall degrading enzymes, Pectinex Ultra SP‐L and Ultrazyme 100G. The first increased starch yield with a shorter incubation period than the second. The superior effect of Pectinex Ultra SP‐L was observed already at 0.5 h, where a wide granule size distribution (8—87 μm) was obtained. A slight increase in the release of granules ranging from 30—60 μm was noted within a 2 h incubation period. However, upon further incubation, the distribution pattern was similar to that of untreated samples. Samples treated with Ultrazyme 100G exhibited a unimodal distribution pattern, with larger granules, ranging from 40—70 μm, being released upon further incubation within a 2 h incubation period. However, all samples exhibited a bimodal distribution upon further incubation.     

Preparation and properties of RS III from waxy maize starch with pullulanase

Waxy maize starch was treated by pullulanase debranching and retrogradation at room temperature to produce resistant starch (RS). Physicochemical properties, crystalline structure and in-vitro digestibility of starch samples with different RS content were investigated. Compared with native starch, apparent amylose content of RS products increased. Based on Gel Permeation Chromatography (GPC) the Molecular Weight Distribution (MWD) of resistant starches significantly changed. Scanning Electron Microscopy (SEM) showed that upon pullulanase debranching and retrogradation treatment the granular structure of native starch was destroyed and all RS samples exhibited irregular shaped fragments. Crystal structure of samples changed from A–type to a mixture of B and V–type. The crystallinity of resistant starch also improved as compared with native starch. Moreover, samples with higher resistant starch showed higher relative crystallinity. Differential Scanning Calorimetry (DSC) determination showed that To、Tp、Tc and ΔH all increased which was in agreement with RS content. The resistance of waxy maize starch with Pullulanase treatment to α-amylase digestibility also increased, while the in-vitro digestibility of products decreased.     

以机械活化玉米淀粉为原料酶法制备低DE值麦芽糊精

以机械活化玉米淀粉为原料制备低DE（Dextrose Equivalent）值麦芽糊精,通过单因素实验研究了机械活化时间、反应时间、反应温度、酶添加量、底物浓度、pH对产品DE值的影响,并在此基础上进行了正交实验。结果表明,经机械活化预处理后的淀粉酶解反应活性明显提高,酶解速度加快,酶解时间大大缩短,而原淀粉在相同条件下几乎不与酶作用。正交实验确定了制备工艺的最佳条件为：酶添加量3u·g-1淀粉干基,pH6.5,水解温度45℃,底物浓度10%,水解时间4min,按此条件所得的麦芽糊精DE值为2.35%。并用红外光谱和X-射线衍射对麦芽糊精进行了分析。     

Production of resistant starch from acid-modified amylotype starches with enhanced functional properties

Amylotype corn starches, Hylon V and Hylon VII, were acid-hydrolyzed followed by autoclaving-storing cycles and drying in an oven or freeze-dryer. Molecular weights of the samples decreased with increasing hydrolysis time. Resistant starch (RS) contents of acid-hydrolyzed samples did not differ from those of native starches. RS contents of oven-dried samples were higher than those of freeze-dried samples. Onset (T_O) and peak (T_P) transition temperatures of hydrolysates were lower than those of respective native starches. Autoclaving-storing increased in T_O and T_P and decreased in ΔH values as compared to acid-hydrolyzed starches. Water binding and solubility values of hydrolysates were higher than those of respective native starches. Autoclaved-stored samples had higher water binding and solubility values than those of respective acid-hydrolyzed samples. Acid-hydrolyzed and autoclaved-stored samples increased the emulsion capacity and stability values of albumin. The RVA viscosity values of the autoclaved-stored samples were higher than those of the hydrolysates.     

Effect of heat-moisture treatment on the formation and physicochemical properties of resistant starch from mung bean (Phaseolus radiatus) starch

Mung bean starch was subjected to a range of heat-moisture treatments (HMT) based on different moisture contents (15%, 20%, 25%, 30%, and 35%) all heated at 120 °C for 12 h. The impact on the yields of resistant starch (RS), and the microstructure, physicochemical and functional properties of RS was investigated. Compared to raw starch, the RS content of HMT starch increased significantly, with the starch treated at 20% moisture having the highest RS content. After HMT, birefringence remained at the periphery of the granules and was absent at the center of some granules. The shape and integrity of HMT starch granules did not change but concavity was observed under scanning electronic microscopy. Apparent amylose contents of HMT starch increased and the HMT starch was dominated by high molecular weight fraction. Both the native and HMT starches showed A-type X-ray diffraction pattern. Relative crystallinity increased after HMT. The gelatinization temperatures (To, Tp, and Tc), gelatinization temperature range (Tc–To) and enthalpies of gelatinization (ΔH) increased significantly in HMT starch compared to native starch. The solubility increased but swelling power decreased in HMT starches. This study clearly shows that the HMT exhibited thermal stability and resistance to enzymatic hydrolysis owing to stronger interactions of starch chains in granule.     

In vitro starch hydrolysis and estimated glycaemic index of bread substituted with different percentage of chempedak (Artocarpus integer) seed flour

Chempedak (Artocarpus integer) seed flour (CSF) was substituted for wheat flour at different levels (0%, 10%, 20%, 30% w/w) in bread. Assessment on the in vitro starch hydrolysis was carried out to evaluate the hydrolysis index (HI) and estimated glycaemic index (EGI) of bread substituted with different levels of CSF. Kinetics of in vitro starch hydrolysis in all bread samples (with the exception for white bread) indicated a gradual increase with respect to time intervals. Bread of 30% CSF exhibited significantly lower (p < 0.05) in vitro starch hydrolysis, as compared with the other samples. Results showed that HI value decreased significantly (p < 0.05) as the levels of CSF substitution increased. Resistant starch (RS) content in bread samples was inversely related with HI value as CSF substitution levels increased, thus lowering the EGI value.