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Olorunsola et al., Nig. Journ. Pharm. Sci., March, 2011 Vol. 9 No. 2, P.


Nigerian Journal of Pharmaceutical Sciences Vol.10, No. 1, March, 2011, ISSN: 0189-823X All Rights Reserved

Department of Pharmaceutics and Pharmaceutical Microbiology, Ahmadu Bello University, Zaria Author for correspondence:, +2348035067306, +2348052196033 ABSTRACT Acid hydrolysis has been shown to be one of the methods of improving the functional properties of native starch. Starch was extracted from sweet potato tubers and hydrolyzed. The microcrystalline starch (MCS) was produced using 6 N HCl at varying temperatures (48 and 54 OC) and exposure times (6 - 24 hr). The physicochemical properties namely :- organoleptic properties, pH, solubility, hydration and swelling capacities, moisture sorption capacity, % moisture loss, particle size analysis, angle of repose, flow rate, true density, bulk and tapped densities, Carrs index and Hausners ratio of the native and microcrystalline starches were evaluated. The results showed that at 48 0C and exposure time of 12 hr, the highest yield (97.22 %) of MCS was obtained. However, hydrolysis at 54 0C and exposure time of 6 hr gave the best material with excellent flow (angle of repose 27.23 0 and flow rate 20.6 g/s); Carrs index and Hausners ratio of 16.4 % and 1.2 respectively; and hydration and swelling capacities of 2.36 and 1.7 respectively. The study has shown that the physicochemical properties of microcrystalline starch obtained from Ipomoea batatas were better than those of the native starch; and the optimum hydrolyzing conditions were 54 OC temperature and exposure time of 6 hr. Keywords: Acid hydrolysis, microcrystalline starch, physicochemical properties, sweet potato.

INTRODUCTION Sweet potato, which originated from South America is now grown throughout the tropics. About 129 million tons is produced annually (Bender, 1990). The tuber contains about 69 % moisture, 23 % starch, 1 % protein, 0.3 % fat, 0.0008 % iron, 0.00015 % carotene, 0.00008 % Vitamin B1, 0.00004 % Vitamin B2, 0.0005 % nicotinic acid, 0.02 % vitamin C and 6 % other substances (Bender, 1990). Tubers of sweet potato are potential starch sources that are useful in food, paper, textile and pharmaceutical industries. In tableting, starch is useful as diluent, binder, disintegrant and lubricant due to its physicochemical properties and relative

inertness (Odeku and Itiola, 2007). The use of starch is however limited by its poor functional properties of flow, compressibility and compactability. Several modifications have been shown to improve these functional properties (Bos et al., 1992). The different types of modifications include:- heat gelatinization, acid hydrolysis, enzymatic hydrolysis and various forms of chemical modifications (Okafor et al.,2000; Bello-Perez et al., 2000) Acid hydrolysis affects both the physical and chemical nature of starch and improves its suitability for both pharmaceutical and non-pharmaceutical use (Yiu et al., 2008). During acid hydrolysis, glycosidic bonds of the starch

Olorunsola et al., Nig. Journ. Pharm. Sci., March, 2011 Vol. 9 No. 2, P.7380

are broken leading to the formation of mixtures of anomeric sugars. At elevated temperatures especially with limited water, dextrin molecules are formed. Acid hydrolysis imparts better physical properties (flow, compressibility and compactability) to native starch and makes it amenable to direct compression (Ocheja, 2000). This study was aimed at producing microcrystalline starches by acid hydrolysis at varying temperatures (48 and 54 OC) and exposure times (6 - 24 hr) and determining the effects of varying conditions of hydrolysis on some of the physicochemical properties of the starch. MATERIALS AND METHODS Materials Sweet potato tubers obtained from Samaru, Zaria and identified by Institute of Agricultural Research, A.B.U. Zaria were used as the source of starch. Chemicals used included sodium hydroxide, hydrochloric acid, acetone, chloroform, ethanol and xylene; all from BDH Chemicals Ltd. Poole - England. Methods Extraction of starch from sweet potato tubers: Potato tubers of total weight 4 kg were washed and peeled. This was followed by cutting, grating and blending. The blended mass was suspended in 20 litres of water and the starch recovered using calico cloth. The starch was treated with 250 ml of 0.1 N sodium hydroxide and washed three times with waters. The starch suspension was centrifuged, supernatant liquid decanted and the upper brown layer was scrapped off. The tightly packed starch was dried in air then in an oven (BS size 3, Gallenkamp, England) at 40 0C for 1 hr. Determination Temperature: of The Gelatinization temperature of

gelatinization was determined by preparing 10 ml of 0.2 % w/v starch suspension in 25 ml beaker and heating in a thermostated water bath at 40 0C. The temperature was raised stepwise by 2 0C and samples were taken after each rise. The withdrawn samples were observed under a light microscope (No.061270 Ceti, Belgium) to ascertain the temperature at which the granules lost their polarization crosses totally (Mohammed et al., 2009). Production of microcrystalline starch: To 450 g suspension of 36 % w/w starch, 28 ml of 6 N HCl was added and the reaction was allowed to proceed at 48 0C. One hundred gram sample each of this was taken at 6 hr, 12 hr, 18 hr and 24 hr for processing and examination. Processing involved vacuum filtration, suspension of the microcrystalline starch in 250 ml water, adjustment to pH 6 with 0.1 N NaOH, vacuum filtration with 750 ml water and dehydration with ethanol. The process was repeated at reaction temperature of 54 0C at the same exposure times (Mohammed et al., 2009). Determination of percentage yield and organoleptic properties: The percentage yield, taste, colour and texture of the microcrystalline starches at the various hydrolyzing conditions were determined. This was to determine the conditions (temperatures and exposure times) that would produce good yield and acceptable organoleptic properties. Determination of solubility: The solubility of the samples was determined using the following solvents: cold water, hot water, acetone, ethanol and chloroform. Two grams starch sample was dispersed in 10 ml solvent and left overnight. The supernatant solution was filtered and 5 ml sample of the filterate was taken and heated to dryness at 110 OC on a Gallenkamp hot plate. The residue left was weighed and the solubility was

Olorunsola et al., Nig. Journ. Pharm. Sci., March, 2011 Vol. 9 No. 2, P.7380

calculated as % w/v (Iwuagwu and Onyekweli, 2002). Determination of hydration capacity: The method used by Sung and Stone (2004) was used for the determination of hydration capacity. One gram starch sample was dispersed in 10 ml distilled water, mixed on a vortex mixer for 2 minutes and centrifuged for 5 minutes. The supernatant was decanted and the sediment weighed. The hydration capacity (H.C) was calculated using the equation:H .C W2 ------------ (i) W1

Particle size analysis: Twenty grams starch sample was placed on a nest of sieves (Endecott, United Kingdom) containing sieves arranged in descending order (500, 250, 150, 90 and 75 m) and the shaker vibrated for 15 min. The weight of starch retained on each of the sieve was taken and % cumulative weight oversize was plotted against particle size. Determination of powder flow properties: For the angle of repose, 20 g starch was poured inside a funnel of orifice diameter 0.8 cm clamped at height 10 cm from the table surface and was allowed to flow freely. The angle of repose, , was calculated from the equation:

where W1 = initial weight of starch and W2= weight of sediment. Determination of swelling capacity: The tapped volume occupied by 5 g starch in a measuring cylinder was noted as V1. This was dispersed in 100 ml distilled water and left for 24 hr. The volume of sediment was then noted as V2. The swelling capacity (S.C) was calculated using the equation:-



where h = height of heap and D is the diameter. It was repeated thrice and the average determined. Also, 20 g starch was placed in a flow rate machine (Erweka Apparatebau GMBH, Germany). The time of flow was determined and the flow rate calculated.
Determination of bulk, tapped and true densities: -The true density was determined using liquid displacement method. An empty 50 ml capacity pycnometer was initially weighed (W), filled with xylene and then reweighed (W1). The difference between W1 and W was calculated as W2. Two grams (W3) starch was transferred into the pycnometer, the excess liquid was wiped off and the system finally weighed (W4) . The true density Dt (g/cm3) was calculated using Iwuagwu and Onyekweli (2002) equation:
Dt = (W2 x W3) / 50(W3 W4 + W2 + W) - (iv)

S .C

V2 V1

--------- (ii)

Determination of moisture sorption capacity: Two grams starch sample was kept in a desiccator containing distilled water (relative humidity 100%) for 5 days after which it was reweighed. The moisture sorption capacity was calculated as a ratio of change in weight to the initial weight. Determination of percentage moisture loss: Five grams starch sample was heated in an oven (BS size 3 Gallenkamp, England) at 105 oC, examined every hour until a constant weight was obtained. Percentage moisture loss was calculated as a ratio of loss in weight to the initial weight of the starch.

For the determination of bulk and tapped densities, 10 g powder was placed in a 50 ml measuring cylinder and the bulk volume noted. After 500 taps (rising to 20

Olorunsola et al., Nig. Journ. Pharm. Sci., March, 2011 Vol. 9 No. 2, P.7380

cm height), the volume was noted. The bulk density (BD) and tapped density (TD) were then calculated. The Carrs index (C.I) and Hausners ratio (H.R) were also calculated using Wells and Aulton (2007) equations:-


T .D B.D X 100% --------(v) T .D T .D B.D


starch were higher than those of the microcrystalline starches. However, the values increased with increase in extent of hydrolysis with the result of microcrystalline starch produced at 54 OC (6 hr) having higher values than the NS. The flow rate increased with increase in extent of acid hydrolysis. The Carrs index and Hausners ratio of the NS were higher than those of the MCS. The native starch contains more of large particles than the microcrystalline starches and the proportion of the large particles decreased with increase in hydrolyzing temperature (Figure 1).
Table 1: Percentage yields and colours of the various microcrystalline starches derived from Ipomoea batatas Hydrolysing conditions 48 oC / 6 hr Yield (%) 91.66 Colour

H .R


The gelatinization temperature of the sweet potato was found to be 56-58 0C. The percentage yields and colours of the microcrystalline starches (MCS) produced at various hydrolyzing conditions are shown in Table 1. The hydrolyzing condition 48 0C (12 hr) gave the highest yield of 97.22 % followed by 54 OC (6 hr) which gave a yield of 93.88 %. The hydrolyzing condition 48 OC (24 hr) gave the lowest yield. The solubility of the native starch and all the MCS were higher in hot water than in cold water. All the starches have equal solubilities (0.4 % w/v) in ethanol. The solubility of the starch in chloroform increased with increase in extent of hydrolysis (Table 2). Some physicochemical properties of the native starch and various microcrystalline starches are shown in Table 3.The hydration capacity; swelling capacity and moisture sorption capacity of the native

White Off white Off white Light brown Light brown Brown Brown Brown

48 oC / 12 hr 48 oC / 18 hr 48 oC / 24 hr 54 oC / 6 hr 54 oC / 12 hr 54 oC / 18 hr 54 oC / 24 hr

97.22 88.89 86.11 93.88 92.22 92.22 88.89


Olorunsola et al., Nig. Journ. Pharm. Sci., March, 2011 Vol. 9 No. 2, P.7380

Table 2: Solubility of the various starches derived from Ipomoea batatas Solubility (%w/v) Starch Native MCS 48 0C/ 6 hr MCS 48 0C/ 12 hr MCS 54 C/ 6 hr

Cold water

Hot water




0.02 0.02 0.02 0.02

0.2 0.02 0.02 0.02

0.4 0.4 0.4 0.4

0.6 0.02 0.02 0.02

0.02 0.8 1.0 1.2

Table 3: Some physicochemical properties of the various starches derived from Ipomoea batatas

Native Parameter Hydration Capacity Swelling Capacity Moist.Sorp.Cap. (%) Moisture Loss (%) Angle of Repose ( ) Flow Rate (g/sec) True Density (g/cm3) Bulk Density (g/cm3) Tapped Density (g/cm3) Carrs Index (%) Hausners Ratio

MCS 48 C/6 hr 1.32 1.22 26.5 14.4 41.80 1.71 1.42 0.50 0.67 25.4 1.34

MCS 48 C/12h r 1.32 1.22 26.5 16.0 30.60 1.71 1.51 0.48 0.67 28.4 1.40

MCS 54 OC/6 hr 2.36 1.70 27.0 13.2 27.23 20.60 1.31 0.56 0.67 16.4 1.20

Starch 1.96 1.30 30.5 11.6 44.35 1.46 1.51 0.53 0.77 31.2 1.45


Olorunsola et al., Nig. Journ. Pharm. Sci., March, 2011 Vol. 9 No. 2, P.7380

Native starch MCS-48oC/6hr MCS-48oC/12hr MCS-54oC/6hr

Figure 1. Particle size distribution for the various starches derived from Ipomoea batatas


The acid hydrolysis was carried out at 48 and 54 OC which are sub-gelatinization temperatures (Puchongkavarin et al., 2003). The MCS from 48 0C (18 hr), 48 0 C (24 hr), 54 0C (12 hr), 54 0C (18 hr) and 540C (24 hr) were excluded from further examinations because of either poor yield, dark colour or both. The poor yield was due to sub-optimal hydrolyzing conditions while dark colour could be due to production of coloured dextrin ( Yiu et al., 2008). The solubility of starch in water increased with increase in temperature. As temperature increases, water penetrates more into the amorphous region of the

starch granules resulting in more hydration and dissolution (Huijbrecht, 2008). The native and microcrystalline starches are more soluble in ethanol than water. This is in consonance with the work of Yiu et al. (2008). The most common features of all theories of disintegration is that penetration of water must precede disintegration and this can be assessed by determination of hydration capacity, swelling capacity and porosity (Oyi et al., 2009). The MCS obtained at 54 0C (6 hr) with the highest hydration capacity and swelling capacity of 2.36 and 1.70 respectively (Table 3) may have the best water uptake and may intrinsically possess a high disintegration property.

Olorunsola et al., Nig. Journ. Pharm. Sci., March, 2011 Vol. 9 No. 2, P.7380

The moisture sorption capacity of the native starch is higher than those of the microcrystalline starches. Ohwoavworhua and Adelakun (2005) reported that moisture sorption capacity is a measure of moisture sensitivity of a material and it reflects the relative physical stability of the tablet formulated with the material when stored under humid condition. Therefore, microcrystalline starch may form a more stable tablet. The good flow of the MCS produced at 54 0 C (6 hr) may be due to particle size distribution with the highest amount of microcrystals over 50 % content < 75 m (Fig. 1) and also to its lowest moisture content (among the microcrystalline starches). The MCS produced at 54 0C (6 hr) had the best flow indices: angle of repose 27.230, flow rate 20.6 g/s, Carrs index 16.4% and Hausners ratio 1.2 (Table 3). According to Wells and Aulton (2007), these are all indications of a very good flow. This will enable good diefilling and little or no glidant will be required during tableting.
CONCLUSION The study has shown that microcrystalline starches were produced by acid hydrolysis of sweet potato starch. The highest yield was obtained at 48 0C (12 hr) while at 54 0 C (6 hr), microcrystalline starch with the best physicochemical properties was produced. It has also shown that the exposure time and temperature affect the functional properties of microcrystalline starch produced. REFERENCES

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