Food Chemistry 179 (2015) 270–277
Contents lists available at ScienceDirect
Food Chemistry journal homepage: www.elsevier.com/locate/foodchem
Optimization of extraction efficiency by shear emulsifying assisted enzymatic hydrolysis and functional properties of dietary fiber from deoiled cumin (Cuminum cyminum L.) Mengmei Ma a, Taihua Mu a,⇑, Hongnan Sun a, Miao Zhang a, Jingwang Chen a, Zhibin Yan b a Laboratory of Food Chemistry and Nutrition Science, Institute of Agro-Products Processing Science and Technology, Chinese Academy of Agricultural Sciences, Key Laboratory of Agro-products Processing, Ministry of Agriculture, No. 2 Yuan Ming Yuan West Road, Haidian District, Beijing 100193, PR China b Research Institute of Dunhuang Seed, Dunhuang Seed Co., Ltd., No. 28 Suzhou Road, Suzhou District, Jiuquan 0937, PR China
a r t i c l e
i n f o
Article history: Received 26 August 2014 Received in revised form 23 December 2014 Accepted 31 January 2015 Available online 7 February 2015 Chemical compounds used in this study: Sodium hydroxide (PubChem CID: 14798) Phosphoric acid (PubChem CID: 1004) Lignin (PubChem CID: 73555271) Sodium dihydrogen phosphate dehydrate (PubChem CID: 23673460) Disodium hydrogen phosphate dodecahydrate (PubChem CID: 61456) Hydrochloric acid (PubChem CID: 313) Glucose (PubChem CID: 79025) Taurocholic acid sodium salt hydrate (PubChem CID: 23687511) Cholesterol (PubChem CID: 5997) Methanol (PubChem CID: 887)
a b s t r a c t This study evaluated the optimal conditions for extracting dietary fiber (DF) from deoiled cumin by shear emulsifying assisted enzymatic hydrolysis (SEAEH) using the response surface methodology. Fat adsorption capacity (FAC), glucose adsorption capacity (GAC), and bile acid retardation index (BRI) were measured to evaluate the functional properties of the extracted DF. The results revealed that the optimal extraction conditions included an enzyme to substrate ratio of 4.5%, a reaction temperature of 57 °C, a pH value of 7.7, and a reaction time of 155 min. Under these conditions, DF extraction efficiency and total dietary fiber content were 95.12% and 84.18%, respectively. The major components of deoiled cumin DF were hemicellulose (37.25%) and cellulose (33.40%). FAC and GAC increased with decreasing DF particle size (51–100 lm), but decreased with DF particle sizes 4.5%. At constant E/S, DF extraction efficiency increased with increasing reaction time (X4) from 120 to 150 min, but decreased with higher reaction times. DF extraction efficiency and purity were higher when compared to the traditional acidbase or alkali-base extraction and sequential enzymatic extraction methods (Meyer et al., 2009; Sowbhagya et al., 2007; Thomassen, Vigsnæs, Licht, Mikkelsen, & Meyer, 2011). Fig. 1b shows the effects of pH (X3) and reaction temperature (X2) on DF extraction efficiency. There was a significant interaction between pH and reaction temperature. In this study, pH had a significant quadratic effect on DF extraction efficiency in the response surface plot. DF extraction efficiency increased with increasing pH from 7.00 to 7.75, but decreased with higher pH values. These results suggest that higher pH values (>7.75) affect the enzymatic space-conformation and negatively impact enzyme activity. Additionally, higher pH values might inhibit the combination of substrate with the active center of the enzyme. At constant pH, the effect of reaction temperature on DF extraction efficiency had similar trends; high reaction temperature (>58 °C) reduced enzyme activity. Fig. 1c shows that it takes a longer time to achieve a high DF extraction efficiency at low pH values. More covalent cross-linking between the enzyme and proteins can be formed with increasing reaction time, thereby improving DF extraction efficiency. The effects of E/S (X1) and reaction temperature (X2) on DF extraction efficiency are shown in Fig. 1d. A parabolic curve was obtained between E/S and reaction temperature; the effect of the reaction temperature on DF extraction efficiency was more significant than that of E/S. 3.2.4. Verification of predictive models The optimum extraction condition was determined by the canonical analysis of the response surface. The canonical analysis predicted that the optimum extraction conditions consisted of
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M. Ma et al. / Food Chemistry 179 (2015) 270–277
Table 3 ANOVA results of DF extraction efficiency. Source
Sum of squares
Degree of freedom
Mean square
F-value
P-value
Model X1 X2 X3 X4 X1X2 X1X3 X1X4 X2X3 X2X4 X3X4 X21 X22 X23 X24 Total error Lack of Fit Pure error Total SS Predicted R2 = 0.9909
557.80 21.60 100.17 73.41 49.98 2.84 1.05 4.24 3.35 2.07 5.64 72.89 142.74 128.43 109.76 5.10 2.12 2.97 562.90
14 1 1 1 1 1 1 1 1 1 1 1 1 1 1 14 10 4 28
39.84 21.60 100.17 73.41 49.98 2.84 1.05 4.24 3.35 2.07 5.64 72.89 142.74 128.43 109.76 0.36 0.21 0.74 0.74
109.45 59.34 275.17 201.66 137.30 7.80 2.89 11.66 9.20 5.70 15.50 200.24 392.11 352.82 301.51
Contents lists available at ScienceDirect
Food Chemistry journal homepage: www.elsevier.com/locate/foodchem
Optimization of extraction efficiency by shear emulsifying assisted enzymatic hydrolysis and functional properties of dietary fiber from deoiled cumin (Cuminum cyminum L.) Mengmei Ma a, Taihua Mu a,⇑, Hongnan Sun a, Miao Zhang a, Jingwang Chen a, Zhibin Yan b a Laboratory of Food Chemistry and Nutrition Science, Institute of Agro-Products Processing Science and Technology, Chinese Academy of Agricultural Sciences, Key Laboratory of Agro-products Processing, Ministry of Agriculture, No. 2 Yuan Ming Yuan West Road, Haidian District, Beijing 100193, PR China b Research Institute of Dunhuang Seed, Dunhuang Seed Co., Ltd., No. 28 Suzhou Road, Suzhou District, Jiuquan 0937, PR China
a r t i c l e
i n f o
Article history: Received 26 August 2014 Received in revised form 23 December 2014 Accepted 31 January 2015 Available online 7 February 2015 Chemical compounds used in this study: Sodium hydroxide (PubChem CID: 14798) Phosphoric acid (PubChem CID: 1004) Lignin (PubChem CID: 73555271) Sodium dihydrogen phosphate dehydrate (PubChem CID: 23673460) Disodium hydrogen phosphate dodecahydrate (PubChem CID: 61456) Hydrochloric acid (PubChem CID: 313) Glucose (PubChem CID: 79025) Taurocholic acid sodium salt hydrate (PubChem CID: 23687511) Cholesterol (PubChem CID: 5997) Methanol (PubChem CID: 887)
a b s t r a c t This study evaluated the optimal conditions for extracting dietary fiber (DF) from deoiled cumin by shear emulsifying assisted enzymatic hydrolysis (SEAEH) using the response surface methodology. Fat adsorption capacity (FAC), glucose adsorption capacity (GAC), and bile acid retardation index (BRI) were measured to evaluate the functional properties of the extracted DF. The results revealed that the optimal extraction conditions included an enzyme to substrate ratio of 4.5%, a reaction temperature of 57 °C, a pH value of 7.7, and a reaction time of 155 min. Under these conditions, DF extraction efficiency and total dietary fiber content were 95.12% and 84.18%, respectively. The major components of deoiled cumin DF were hemicellulose (37.25%) and cellulose (33.40%). FAC and GAC increased with decreasing DF particle size (51–100 lm), but decreased with DF particle sizes 4.5%. At constant E/S, DF extraction efficiency increased with increasing reaction time (X4) from 120 to 150 min, but decreased with higher reaction times. DF extraction efficiency and purity were higher when compared to the traditional acidbase or alkali-base extraction and sequential enzymatic extraction methods (Meyer et al., 2009; Sowbhagya et al., 2007; Thomassen, Vigsnæs, Licht, Mikkelsen, & Meyer, 2011). Fig. 1b shows the effects of pH (X3) and reaction temperature (X2) on DF extraction efficiency. There was a significant interaction between pH and reaction temperature. In this study, pH had a significant quadratic effect on DF extraction efficiency in the response surface plot. DF extraction efficiency increased with increasing pH from 7.00 to 7.75, but decreased with higher pH values. These results suggest that higher pH values (>7.75) affect the enzymatic space-conformation and negatively impact enzyme activity. Additionally, higher pH values might inhibit the combination of substrate with the active center of the enzyme. At constant pH, the effect of reaction temperature on DF extraction efficiency had similar trends; high reaction temperature (>58 °C) reduced enzyme activity. Fig. 1c shows that it takes a longer time to achieve a high DF extraction efficiency at low pH values. More covalent cross-linking between the enzyme and proteins can be formed with increasing reaction time, thereby improving DF extraction efficiency. The effects of E/S (X1) and reaction temperature (X2) on DF extraction efficiency are shown in Fig. 1d. A parabolic curve was obtained between E/S and reaction temperature; the effect of the reaction temperature on DF extraction efficiency was more significant than that of E/S. 3.2.4. Verification of predictive models The optimum extraction condition was determined by the canonical analysis of the response surface. The canonical analysis predicted that the optimum extraction conditions consisted of
274
M. Ma et al. / Food Chemistry 179 (2015) 270–277
Table 3 ANOVA results of DF extraction efficiency. Source
Sum of squares
Degree of freedom
Mean square
F-value
P-value
Model X1 X2 X3 X4 X1X2 X1X3 X1X4 X2X3 X2X4 X3X4 X21 X22 X23 X24 Total error Lack of Fit Pure error Total SS Predicted R2 = 0.9909
557.80 21.60 100.17 73.41 49.98 2.84 1.05 4.24 3.35 2.07 5.64 72.89 142.74 128.43 109.76 5.10 2.12 2.97 562.90
14 1 1 1 1 1 1 1 1 1 1 1 1 1 1 14 10 4 28
39.84 21.60 100.17 73.41 49.98 2.84 1.05 4.24 3.35 2.07 5.64 72.89 142.74 128.43 109.76 0.36 0.21 0.74 0.74
109.45 59.34 275.17 201.66 137.30 7.80 2.89 11.66 9.20 5.70 15.50 200.24 392.11 352.82 301.51
