Determination Trial of Nondigestible Oligosaccharide in Processed

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Determination trial of nondigestible oligosaccharide in processed foods by improved AOAC method 2009.01 using porcine small intestinal enzyme Kenichi Tanabe, Sadako Nakamura, Katsuhisa Omagari, and Tsuneyuki Oku J. Agric. Food Chem., Just Accepted Manuscript • Publication Date (Web): 31 May 2015 Downloaded from http://pubs.acs.org on May 31, 2015

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Journal of Agricultural and Food Chemistry

Determination trial of nondigestible oligosaccharide in processed foods by improved AOAC method 2009.01 using porcine small intestinal enzyme

Kenichi Tanabe*†,‡, Sadako Nakamura§, Katsuhisa Omagari‡ and Tsuneyuki Oku‡,§

†

Department of Food Science and Nutrition, Nagoya Women's University, 3-40, Shioji,

Mizuho-ku, Nagoya, 4678610, Japan ‡

Graduate School of Human Health Science, University of Nagasaki Siebold,

1-1-1Manabino, Nagayo, Nagasaki, 8512195, Japan §

Institute of Food, Nutrition & Health, Jumonji University, 2-1-28 Sugasawa, Niiza,

Saitama, 3528510, Japan

*Corresponding author: Kenichi Tanabe, Ph.D., Department of Food Science and Nutrition, Nagoya Women's University, 3-40, Shioji, Mizuho-ku, Nagoya, 4678610, Japan. Tel & Fax: +81 52 852 1499. Email: [email protected]

1

ACS Paragon Plus Environment


1

ABSTRACT

2

We have previously shown that the Association of Official Analytical Chemists (AOAC)

3

method 2001.03 and 2009.01 not able to measure accurately nondigestible

4

oligosaccharide because they are incapable of hydrolyzing digestible oligosaccharide,

5

leading to overestimation of nondigestible oligosaccharide. Subsequently, we have

6

proposed the improved AOAC methods 2001.03 and 2009.01 using porcine small

7

intestinal disaccharidases instead of amyloglucosidase. In the present study, we tried to

8

determine nondigestible oligosaccharide in marketed processed foods using the

9

improved AOAC method 2009.01 (improved method), and the results were compared

10

with those by AOAC method 2009.01. “In improved method, the percentage of the

11

recovery of fructooligosaccharide, galactooligosaccharide, and raffinose to the label of

12

processed food was 103.0%, 89.9%, and 102.1%, respectively. However, the AOAC

13

method 2009.01 overestimated more than 30% of the quantity of nondigestible

14

oligosaccharide in processed foods, since the margin of error was accepted ±20% on the

15

contents of nondigestible oligosaccharides in processed foods for Japanese Nutrition

16

Labeling, the improved method thus provided accurate quantification of nondigestible

17

oligosaccharides in processed food and allows a comprehensive determination of

18

nondigestible oligosaccharides.

19 20

KEYWORDS: improved AOAC method 2009.01; determination method; nondigestible

21

oligosaccharide; porcine small intestinal enzyme


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INTRODUCTION

23

Various oligosaccharides distribute naturally in foods such as fruits,

24

vegetables, milk, and honey, and can be technically produced by enzymatic hydrolysis.

25

Some oligosaccharides are artificially synthesized from glucose, fructose, galactose or

26

starch hydrolysate using bacterial enzymes.1 Oligosaccharides are added to processed

27

foods to improve sensory characteristics such as taste, texture, and foam stability.1

28

Moreover, fructooligosaccharide (FOS),2 galactooligosaccharide (GOS),3 raffinose,4

29

lactulose5 and xylooligosaccharide6, which are not digested by small intestinal enzyme,

30

have attracted interest as prebiotics and have been added to processed foods to provide

31

health benefits.

32

Nondigestible oligosaccharides, which are not digested by human small

33

intestinal enzymes, increase selectively the total count of beneficial bacteria, improve

34

intestinal microflora, and contribute to human health promotion.7-11 Intestinal microbes

35

play

36

anti-inflammatory,13 uptake of energy from the host diet,14 production of short chain

37

fatty acid by fermentation,15 alteration of human glucose and fatty acid metabolism,16

38

regulation of intestinal permeability,17 production of vitamins18 and stimulation of

39

mineral absorption by the large intestine.19 Previous studies on intestinal microbes have

40

suggested that microbial environments play critical roles in both health and disease.20,21

41

Therefore, with the expectation of increased consumption of prebiotic nondigestible

42

oligosaccharides, a validated and accurate method for quantification of nondigestible

43

oligosaccharides in foods is essential for public health and dietary guidelines.

important

roles

in

the

development of

the

host

immune

system,12

44

Association of Official Analytical Chemists (AOAC) method 985.29,22 AOAC

45

method 991.4323 and AOAC method 2001.0324 were official methods of analysis for the 3



46

determination of the dietary fiber content in food products. However, these methods

47

appear to be inappropriate for the determination of the upcoming new category of

48

dietary fiber.25 Then, AOAC method 2009.01 (the existing AOAC method) was based

49

on the AOAC 2001.03 method, and was developed as an integrated determination

50

method for dietary fiber, including nondigestible oligosaccharides and resistant starch.26

51

Measurement principle of the existing AOAC method relies on complete hydrolysis of

52

digestible saccharides by porcine pancreatic α-amylase and amyloglucosidase from

53

Aspergillus niger. However, amyloglucosidase used in the existing AOAC method

54

cannot hydrolyze completely digestible saccharides such as sucrose, lactose and panose.

55

As a result, these digestible saccharides are detected as nondigestible oligosaccharides

56

in HPLC analysis.27 Therefore, incomplete hydrolysis by amyloglucosidases leads to

57

inaccurate determination of nondigestible oligosaccharides using the existing AOAC

58

method. The quantitation of nondigestible oligosaccharides requires complete

59

hydrolysis of digestible saccharides to meet the definition in Codex Alimentarius

60

Commission (CAC) of dietary fiber, including nondigestible oligosaccharides.28 We

61

have already proposed the improved AOAC 2009.01 method using porcine small

62

intestinal enzyme instead of amyloglucosidase (improved method).27 The content of

63

FOS, GOS and raffinose were accurately determined as nondigestible oligosaccharides

64

by the improved method, whereas sucrose, isomaltulose, panose, and maltotriose were

65

completely hydrolyzed, and did not affect the determination of nondigestible

66

oligosaccharides.27 Although the improved method was superior to the existing AOAC

67

method in terms of determining oligosaccharides, its application in nondigestible

68

oligosaccharide in marketed processed foods remains untested.

69

In the present study, we applied the improved method to measure 4


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nondigestible oligosaccharides in processed foods and made comparisons with the

71

existing AOAC method. Here, we show that the improved method using porcine small

72

intestinal enzyme, instead of amyloglucosidase, accurately determined nondigestible

73

oligosaccharides contents in currently-marketed food products.

5



74

MATERIALS AND METHODS

75

1. Test samples and preparation We analyzed two types of test samples by the improved method and the

76 77

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existing AOAC method.

78

In first, we prepared five different cookies with added oligosaccharides.

79

Cookies (Morinaga & Co. Ltd, Tokyo, Japan) were chosen as test sample without

80

nondigestible oligosaccharide by evidence based on our previous experiments.29,30

81

Cookies were crushed using a mortar and pestle, and were passed through a mesh sieve

82

of 500 µm. Each oligosaccharide (1.000 g) and cookies (9.000 g) were accurately

83

weighed and mixed using a mortar. Added oligosaccharides were FOS, GOS, or

84

raffinose as nondigestible oligosaccharides as well as isomaltooligosaccharide (IMO) or

85

sucrose as digestible oligosaccharides. FOS (purity > 98%) was donated by Meiji Co.,

86

Ltd (Tokyo, Japan). GOS (purity > 90%) was donated by Nissin Sugar Manufacturing

87

Co., Ltd. (Tokyo, Japan). IMO (purity > 90.8%) was donated by Showa Sangyo Co.

88

(Tokyo, Japan). Raffinose (purity > 98.0%) and sucrose (purity > 99.5%) were

89

purchased from Wako Pure Chemical Industries Ltd (Osaka, Japan. In

90

the

second

analytical

experiment,

we

employed

three

91

commercially-available syrups containing nondigestible oligosaccharide. In Japan, two

92

syrups approved as “Food for Specified Health Uses” and one so-called healthy food

93

was

94

oligosaccharide are shown in Table 1. Syrup samples were purchased over the Internet.

used.

Nutrient compositions

of

three

syrups

95 96

2. Analytical method

97

1) AOAC method 2009.01 (the existing AOAC method) 6


containing

nondigestible

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98

Chemicals

99

All chemicals were of analytical grade or of the highest grade available. The

100

Integrated Total Dietary Fibre kit specified in the existing AOAC method was purchased

101

from Megazyme International Ireland, Ltd. (Wicklow, Ireland). The kit contains

102

pancreatic α-amylase from swine, amyloglucosidase from Aspergillus niger, and

103

protease from Bacillus licheniformis. Ion-exchange resin (Amberlite MB-4),

104

diatomaceous earth, and Trizma® Base were purchased from Japan Organo Co., Ltd.

105

(Tokyo, Japan), Kishida Chemical Co., Ltd. (Osaka, Japan), and Sigma–Aldrich Japan

106

Co. LLC. (Tokyo, Japan), respectively.

107 108

Procedure

109

Nondigestible oligosaccharide contents in test samples were determined using

110

the existing AOAC method.26 The apparatus for the existing AOAC method was used.

111

HPLC analyses were performed using a liquid chromatography system (LC-20AD,

112

Shimadzu Corp., Kyoto, Japan) with a refractive index detector (RID-10A, Shimadzu

113

Corp.) and a Shodex SUGAR KS-802 column (8.0 φ × 300 mm, Showa Denko Co.,

114

Tokyo, Japan), and analyses were conducted at a column temperature of 40°C. Samples

115

were eluted with deionized distilled water at a flow rate of 0.5 mL/min. The limit of

116

detection for glucose was 10 µg/mL in HPLC analysis.

117 118

2) Improved AOAC method 2009.01 (improved method)

119

Chemicals

120

Using chemicals were same as the existing AOAC method.

121 7



122

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Preparation of porcine small intestinal brush border membrane vesicles (PSIBBMVs)

123

PSIBBMVs were prepared using the method described by Kessler et al.31 with

124

modifications. Small intestine from the pylorus to the ileocecal junction with the

125

mesentery of an adult swine was obtained from the Isahaya Prefectural Office of Meat

126

Inspection (Isahaya, Japan). PSIBBMVs were suspended in sufficient volumes of

127

50-mM sodium maleate buffer containing 2 mM CaCl2 and 0.02% sodium azide (pH

128

6.0) and were stored at −80°C until assay.

129 130

Determination of α-glucosidase and disaccharidase activities The α-glucosidase activity (units/mg protein) was determined using the

131 132

method

described

by

Robertson

and

Halvorson

with

133

p-nitrophenyl-α-D-methyl-glucopyranoside as a substrate.32 One unit of α-glucosidase

134

activity per mg of protein was defined as the amount of enzyme that produced 1 µmol of

135

glucose from p-nitrophenyl-α-D-methyl glucopyranoside per min.

136

Assays of disaccharidase activity in PSIBBMVs were performed according to

137

the methods described by Oku et al,33 which were modified from the method described

138

by Dahlqvist et al.34 Sucrose, maltose, trehalose, lactose, and isomaltulose used

139

substrates included. Specific activity (SA) per mg of protein was defined as the activity

140

of enzyme that hydrolyzed 1 µmol of glucose from substrate per hour (µmol substrate

141

hydrolyzed/mg protein/h). Concentrations of protein were determined using the

142

Bradford assay with bovine serum albumin as a standard.35

143 144 145

Procedure Nondigestible oligosaccharide contents of test samples were determined 8


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146

according to the method of Tanabe et al.27 Digestible saccharides were hydrolyzed using

147

an enzyme mixture containing pancreatic α-amylase (50 units/mL) and PSIBBMVs

148

(2,720 units/mL as α-glucosidase; SA: sucrase, 125.8; maltase, 453.2; trehalase, 35.3;

149

lactase, 8.7; isomaltulase, 14.4) for 16 h at 37°C. Test samples were added to enzyme

150

mixtures and nondigestible oligosaccharide contents were determined using the method

151

described by Tanabe et al.27

152 153

3. Calculation of the recovery of nondigestible oligosaccharides in processed food

154

Each nondigestible oligosaccharide in added oligosaccharides in processed

155

food was assayed once in duplicate. On the other hand, each nondigestible

156

oligosaccharide in commercially-available processed food was assessed by 5 times, and

157

it was expressed mean ± standard deviation (SD). Nondigestible oligosaccharide

158

contents were measured according to the calculation for nonprecipitable soluble dietary

159

fiber using the existing AOAC method.26 Nondigestible oligosaccharides were defined

160

as saccharides with degrees of polymerization (DP) of ≥2, according to the definition of

161

“luminacoid” which is comprehensive concept of nondigestible component, from the

162

Japanese Association for Dietary Fiber Research suggesting,36 nondigestible

163

oligosaccharide was defined as saccharide with DP 2 or more than DP 2. The margin of

164

error was accepted ±20% on the contents of nondigestible oligosaccharides in processed

165

foods for Japanese Nutrition Labeling,37 accurate determination thus was accepted

166

±20% on the contents of nondigestible oligosaccharides in processed foods on the label.

167 168 169

4. Ethics Porcine experiments were performed according to the guidelines for the care 9



170

and use of laboratory animals of the University of Nagasaki, Siebold. All experiments

171

were performed at the Laboratory of Public Health Nutrition, University of Nagasaki,

172

Siebold.

10


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173

RESULTS

174

Quantification of oligosaccharides added to processed foods by the improved

175

method and the existing AOAC method

176

Nondigestible oligosaccharide fractions were recovered from cookies using

177

the improved method and the existing AOAC method (Figure 1). After the treatment of

178

cookies containing 10% of FOS, GOS and raffinose by hydrolyzing enzymes in the

179

improved method, recoveries of these nondigestible oligosaccharides were 10.1%,

180

10.7% and 9.7%, respectively. When IMO and sucrose were hydrolyzed by enzymes in

181

the improved method, the content of IMO which was recovered as nondigestible

182

oligosaccharide fraction was only 0.1%, and sucrose was not detected. It was reported

183

that IMO with α-1,4- and α-1,6-glucosidic linkages was digested readily by human

184

intestinal disaccharidases.38 This suggests that the improved method is able to measure

185

accurately quantity of nondigestible oligosaccharide in foods.

186

In contrast, when oligosaccharides in same samples were determined by the

187

existing AOAC method, the recovery as nondigestible oligosaccharide was 14.2% for

188

FOS, 13.8% for GOS, 12.6% for raffinose, and 15.3% for sucrose, respectively.

189

Especially, the recovery of IMO was only 4.0%. Thus, results demonstrate that the

190

existing AOAC method overestimates more than the quantity of nondigestible

191

oligosaccharide in foods.

192 193

Quantification of nondigestible oligosaccharide in the syrups by the improved

194

method and the existing AOAC method

195

Nondigestible oligosaccharides were determined in the syrups using the

196

improved method and the existing AOAC method (Table 2). The improved method 11



197

provided the concentrations of FOS and raffinose in the syrups similar to those stated on

198

the label, but the level of GOS lower than that stated on the food label. In contrast,

199

treatment with hydrolyzing enzymes in the existing AOAC method gave approximately

200

30% greater than values of FOS, GOS and raffinose in the label.

201

12


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202

DISCUSSION

203

In the previous study on the improved method, PSIBBMVs completely

204

hydrolyzed digestible oligosaccharide and distinguished nondigestible oligosaccharide

205

from digestible oligosaccharide.27 Although the improved method was superior to the

206

existing AOAC method in terms of determining oligosaccharides, its application to

207

nondigestible oligosaccharides in marketed processed foods remains untested. We

208

previously have confirmed that cookies used in the present study do not contain

209

nondigestible oligosaccharides.29, 30 Here, cookies were added digestible (sucrose or

210

IMO) or nondigestible oligosaccharides (FOS, GOS or raffinose) at the level of 10%. As

211

shown Figure 1, the improved method hydrolyzed digestible oligosaccharides such as

212

sucrose and IMO in cookies, and gave almost complete recovery of added nondigestible

213

oligosaccharides such as FOS, GOS and raffinose

214

Next, the improved method was applied to marketed syrups, and contents of

215

FOS and raffinose were shown to be similar to those indicated on food label (Table 2).

216

According to the improved method, the concentration of GOS in the syrups was lower

217

than that stated on the food label (Table 2). This discrepancy may reflect the accepted

218

±20% margin of error for Japanese Nutrition Labeling;37 the content of GOS in the

219

syrup would be between 35.5 g and 53.2 g in case of 44.4 g GOS in the product. The

220

value (37.2±2.5) by the improved method was within the value accepted by Japanese

221

Nutrition Labeling. Although porcine small intestinal disaccharidases may hydrolyze

222

GOS with low efficiency, GOS added to cookies was not hydrolyzed (Figure 1),

223

indicating that the improved method accurately measure GOS. Therefore, it is

224

concluded that the improved method is proper to determine GOS in processed foods.

225

When commercially-available processed foods and cookies with added 13



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226

oligosaccharides were treated with the hydrolyzing enzymes, amyloglucosidase, of the

227

existing AOAC method, nondigestible oligosaccharide contents were overestimated

228

(Figure 1 and Table 2). These results indicate that the existing AOAC method cannot

229

hydrolyze digestible saccharides such as sucrose and starch-decomposed products, and

230

maltodextrin in processed foods, consequently quantifying digestible saccharides as

231

nondigestible oligosaccharides. In agreement, Brunt and Sanders showed that the

232

existing

233

maltooligosaccharide fractions into glucose, leading to an erroneous quantification of

234

partially hydrolyzed digestible starch as dietary fiber.39 Our previous study showed that

235

digestible oligosaccharides are barely hydrolyzed by either the AOAC method 2001.03

236

or 2009.01 using amyloglucosidase,27,40 which also failed to hydrolyze digestible

237

saccharides.41 Taken together, these studies show that the hydrolyzing activity of

238

enzymes from bacteria do not reflect the hydrolyzing activities of enzymes of the

239

human gastrointestinal tract.

AOAC

method

does

not

fully

convert

digestible

starch

and

240

Pigs are omnivorous with physiological characteristics that allow to use as a

241

model of human digestive functions.42 Many studies have characterized hydrolyzing

242

specificity of small intestinal disaccharidases in pigs.43-45 In particular, pigs have been

243

used as models in studies of dietary fiber and nondigestible oligosaccharide

244

digestion.46-48 Porcine small intestinal disaccharidases could substitute with those in

245

human. Moreover, pigs are common low cost domestic animals. Therefore, porcine

246

small intestinal disaccharidases may be suitable for determining nondigestible

247

oligosaccharides in foods for human consumption.

248

Prebiotic agents are not digested in the human gastrointestinal tract and their

249

effectiveness is dependent on the quantity of fermentable nondigestible saccharides in 14


Page 15 of 27


large

intestine.49

250

the

Therefore,

a

precise

quantification

of

nondigestible

251

oligosaccharides in food is necessary to find out good source of prebiotic agents and to

252

accurately label the content of nondigestible oligosaccharides in food.

253

In conclusion, we developed the improved method for the accurate

254

quantification of nondigestible oligosaccharides in processed foods using porcine small

255

intestinal disaccharidases. The present improved method may be used to

256

comprehensively determine nondigestible oligosaccharides in commercially available

257

processed foods. An appropriate quantification of nondigestible oligosaccharides in

258

foods is essential to estimate health benefits. Moreover, an accurate determination

259

method for newly developed nondigestible oligosaccharides is imperative for nutrition

260

labeling, which indicates prebiotic contents to help consumer chose healthy foods.

261

Improved AOAC method 2009.01 could be the determination method for nondigestible

262

oligosaccharide, dietary fiber. Furthermore, the partially purified enzymes isolated from

263

PSIBBMVs and a stable supply of these enzymes should be required to make the

264

improved method as a commercial dietary fiber assay kit.

15



265

ABBREVIATIONS USED

266

AOAC, Association of Official Analytical Chemists; CAC, Codex Alimentarius

267

Commission; DP, Degree of Polymerization; FOS, Fructooligosaccharide; GOS,

268

Galactooligosaccharide; IMO, Isomaltooligosaccharide; N.D., Not Detected;

269

PSIBBMVs, porcine small intestinal brush border membrane vesicles; SA, Specific

270

Activity; SD, Standard Deviation

271 272

ACKOWLEDGEMENTS

273

The authors would like to thank Meiji Co., Ltd. (ex-Meiji Seika Kaisha, Ltd.,

274

Tokyo, Japan) for providing FOS, Nissin Sugar Manufacturing Co., Ltd. (Tokyo, Japan)

275

for providing GOS, Showa Sangyo Co. (Tokyo, Japan) for providing IMO. This study

276

was supported in part by a Grant-in-Aid for Challenging Exploratory Research

277

24650498. We thank the Isahaya Prefectural Office of Meat Inspection (Nagasaki,

278

Japan) for supplying porcine intestines.

16


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REFERECES 1) Rastall, R. A. Functional oligosaccharides: application and manufacture. Annu. Rev. Food Sci. Technol. 2010, 1, 305–339. 2) Bornet, F. R.; Brouns, F.; Tashiro, Y.; Duvillier, V. Nutritional aspects of short-chain fructooligosaccharides: natural occurrence, chemistry, physiology and health implications. Dig. Liver Dis. 2002, 34 Suppl 2, S111-120. 3) Depeint, F.; Tzortzis, G.; Vulevic, J.; I’Anson, K.; Gibson, G. R. Prebiotic evaluation of a novel galactooligosaccharide mixture produced by the enzymatic activ¬ity of Bifidobacterium bifidum NCIMB 41171, in healthy humans: a randomized, double-blind, crossover, placebo-controlled intervention study. Am. J. Clin. Nutr. 2008, 87, 785-791. 4) Martínez-Villaluenga, C.; Frías, J.; Vidal-Valverde, C.; Gómez, R. Raffinose family of oligosaccharides from lupin seeds as prebiotics: application in dairy products. J. Food Prot. 2005, 68, 1246-1252. 5) Terada, A.; Hara, H.; Kataoka, M.; Mitsuoka, T. Effect of lactulose on the composition and metabolic activity of the human faecal flora. Microb. Ecol. Health Dis. 1992, 5, 43-50. 6) Aachary, A. A.; Prapulla, S. G. Xylooligosaccharides (XOS) as an Emerging prebiotic: microbial synthesis, utilization, structural characterization, bioactive properties, and applications. Compr. Rev. Food Sci. F. 2011, 10, 2-16. 7) Gibson, G. R.; Roberfroid, M. B. Dietary modulation of the human colonic microbiota: introducing the concept of prebiotics. J. Nutr. 1995, 125, 1401–1412. 8) Oku, T.; Nakamura, S. Digestion, absorption and fermentation of newly developed sugar substitutes and their available energy. Pure Appl. Chem. 2002, 74, 1253– 17



1261. 9) Roberfroid, M. B. Prebiotics: the concept revisited. J. Nutr. 2007, 137, 830S–837S. 10) Sanders, M. E.; Lenoir-Wijnkoop, I.; Salminen, S.; Merenstein, D. J.; Gibson, G. R.; Petschow, B. W.; Nieuwdorp, M.; Tancredi, D. J.; Cifelli, C. J.; Jacques, P.; Pot, B. Probiotics and prebiotics: prospects for public health and nutritional recommendations. Ann. N. Y. Acad. Sci. 2014, 1309, 19–29. 11) Kellow, N. J.; Coughlan, M. T.; Reid, C. M. Metabolic benefits of dietary prebiotics in human subjects: a systematic review of randomised controlled trials. Br. J. Nutr. 2014, 111, 1147–1161. 12) Chung, H.; Kasper, D. L. Microbiota-stimulated immune mechanisms to maintain gut homeostasis. Curr. Opin. Immunol. 2010, 22, 455–460. 13) Ding, S.; Chi, M. M.; Scull, B. P.; Rigby, R.; Schwerbrock, N. M.; Magness, S.; Jobin, C.; Lund, P. K. High-fat diet: bacteria interactions promote intestinal inflammation which precedes and correlates with obesity and insulin resistance in mouse. PLoS ONE 2010, 5, e12191. 14) Bäckhed, F.; Manchester, J. K.; Semenkovich, C. F.; Gordon, J. I. Mechanisms underlying the resistance to diet-induced obesity in germ-free mice. Proc. Natl. Acad. Sci. USA 2007, 104, 979–984. 15) Havenaar, R. Intestinal health functions of colonic microbial metabolites: a review. Benef. Microbes 2011, 2, 103–114. 16) Cani, P. D.; Neyrinck, A. M.; Fava, F.; Knauf, C.; Burcelin, R. G.; Tuohy, K. M.; Gibson, G. R.; Delzenne, N. M. Selective increases of bifidobacteria in gut microflora improve high-fat-diet-induced diabetes in mice through a mechanism associated with endotoxaemia. Diabetologia 2007, 50, 2374–2383. 18


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17) Cani, P. D.; Possemiers, S.; Van de Wiele, T.; Guiot, Y.; Everard, A.; Rottier, O.; Geurts, L.; Naslain, D.; Neyrinck, A.; Lambert, D. M.; Muccioli, G. G.; Delzenne, N. M. Changes in gut microbiota control inflammation in obese mice through a mechanism involving GLP-2-driven improvement of gut permeability. Gut 2009, 58, 1091–1103. 18) Hill, M. J. Intestinal flora and endogenous vitamin synthesis. Eur. J. Cancer Prev. 1997, 6 Suppl 1, S43–S45. 19) Scholz-Ahrens, K. E.; Ade, P.; Marten, B.; Weber, P.; Timm, W.; Açil, Y.; Glüer, C. C.; Schrezenmeir, J. Prebiotics, probiotics, and synbiotics affect mineral absorption, bone mineral content, and bone structure. J. Nutr. 2007, 137, 838S–846S. 20) Blumberg, R.; Powrie, F. Microbiota, disease, and back to health: a metastable journey. Sci. Transl. Med. 2012, 4, 137rv7. 21) Bäckhed, F.; Fraser, C. M.; Ringel, Y.; Sanders, M. E.; Sartor, R. B.; Sherman, P. M.; Versalovic, J.; Young, V.; Finlay, B. B. Defining a healthy human gut microbiome: Current concepts, future directions, and clinical applications. Cell Host Microbe 2012, 12, 611–622. 22) Prosky, L.; Asp, N. G.; Furda, I.; DeVries, J. W.; Schweizer, T. F.; Harland, B. F. Determination of total dietary fiber in foods and food products: collab orative study. J. Assoc. Off. Anal. Chem. 1985, 68, 677-679. 23) Prosky, L.; Asp, N.G.; Schweizer, T. F.; DeVries, J. W.; Furda, I.; Lee, S. C. Determination of soluble

dietary fiber in foods and

food

products:

collaborative study. J. AOAC Int. 1994, 77, 690-694. 24) Ohkuma, K.; Matsuda, I.; Katta, Y.; Tsuji, K. New method for determining total 19



dietary fiber by liquid chromatography. J. AOAC Int. 2000, 83, 1013-1019. 25) McCleary, B.V. An integrated procedure for the measurement of total dietary fibre (including resistant starch), non-digestible oligosaccharides and available carbohydrates. Anal. Bioanal. Chem. 2007, 389, 291-308. 26) McCleary, B. V.; DeVries, J. W.; Rader, J.I.; Cohen, G.; Prosky, L.; Mugford, D. C.; Ohkuma, K. Determination of total dietary fiber (CODEX definition) by enzymatic-gravimetric method and liquid chromatography: collaborative study. J. AOAC Int. 2010, 93, 221–233. 27) Tanabe, K.; Nakamura, S.; Oku, T. Inaccuracy of AOAC method 2009.01 with amyloglucosidase for measuring non-digestible oligosaccharides and proposal for an improvement of the method. Food Chem. 2014, 151, 539–546. 28) Joint FAO/WHO Food Standards Programme, Codex Committee on Nutrition and Foods for Special Dietary Uses 32th Session (2010) Draft table of Conditions for Methods of Analysis for Dietary Fibre. REP11/NFSDU 2 and Appendix IV. 29) Oku, T.; Nakamura, S. Evaluation of the relative available energy of several dietary fiber preparations using breath hydrogen evolution in healthy humans. J. Nutr. Sci. Vitaminol. 2014, 60, 246-254. 30) Oku, T.; Nakamura, M.; Hashiguchi-Ishiguro, M.; Tanabe, K.; Nakamura, S. Bioavailability and laxative thereshold of 1-kestose in human adults. Dyn. Biochem. Process Biotech. Mol. Biol. 2009, 3 (Special Issue 1), 90-95. 31) Kessler, M.; Acuto, O.; Storelli, C.; Murer, H.; Müller, M.; Semenza, G. A modified procedure for the rapid preparation of efficiently transporting vesicles from small intestinal brush border membranes. Their use in investigating some properties of D-glucose and choline transport systems. Biochim. Biophys. Acta. 1978, 506, 136– 20


Page 20 of 27

Page 21 of 27


154. 32) Robertson, J. J.; Halvorson, H. O. The components of maltozymase in yeast, and their behavior during deadaptation. J. Bacteriol. 1957, 73, 186–198. 33) Oku, T.; Konishi, F.; Hosoya, N. Mechanism of inhibitory effect of unavailable carbohydrate on intestinal calcium absorption. J. Nutr. 1982, 112, 410–415. 34) Dahlqvist, A. Method for assay of intestinal dissacharidases. Anal. Biochem. 1964, 7: 18-25. 35) Bradford, M. M. A rapid and sensitive method for the quantitation of microgram quantities of protein utilizing the principle of protein-dye binding. Anal. Biochem. 1976, 72, 248–258. 36) Kiriyama, S.; Ebihara, K.; Ikegami, S.; Innami, S.; Sugawa-Katayama, Y.; Takehisa, F. Searching for definition, terminology and classification of dietary fiber and the new proposal from Japan. J. Jpn. Assoc. Dietary Fiber Res. 2006, 10, 11–24. 37) Consumer Affairs Agency, Government of Japan. Nutrition Label (In Japanese). (http://www.caa.go.jp/foods/pdf/syokuhin685.pdf) (accessed November 8, 2014). 38) Kohmoto, T.; Tsuji, K.; Kaneko, T.; Shiota, M.; Fukui, F.; Takaku, H.; Nakagawa, Y.; Ichikawa, T.; Kobayashi S. Metabolism of

13

C-isomaltooligosaccharides in

healthy men. Biosci. Biotechnol. Biochem. 1992, 56, 937-940. 39) Sanders, M. E.; Lenoir-Wijnkoop, I.; Salminen, S.; Merenstein, D. J.; Gibson, G. R.; Petschow, B. W.; Nieuwdorp, M.; Tancredi, D. J.; Cifelli, C. J.; Jacques, P.; Pot, B. Probiotics and prebiotics: prospects for public health and nutritional recommendations. Ann. N. Y. Acad. Sci. 2014, 1309, 19–29. 40) Tanabe, K.; Nakamura, S.; Oku, T. Fatal imperfection of enzymatic-HPLC quantitative method for non-digestible oligosaccharides and its proposed solution 21



Page 22 of 27

strategy newly quantitative method for non-digestible oligosaccharides. Curr. Nutr. Food Sci. 2011, 7, 209–215. 41) Manjunath, P.; Shenoy, B. C.; Raghavendra, Rao, M. R. Fungal glucoamylases. J. Appl. Biochem. 1983, 5, 235–260. 42) Miller, E. R.; Ullrey, D. E. The pig as a model for human nutrition. Ann. Rev. Nutr. 1987, 7, 361–382. 43) Taravel, F. R.; Datema, R.; Woloszczuk, W.; Marshall, J. J.; Whelan, W. J. Purification and characterization of a pig intestinal alpha-limit dextrinase. Eur. J. Biochem. 1983, 130, 147–153. 44) Sørensen, S. H.; Norén, O.; Sjöström, H.; Danielsen, E. M. Amphiphilic pig intestinal microvillus maltase/glucoamylase. Structure and specificity. Eur. J. Biochem. 1982, 126, 559–568. 45) Sjöström, H.; Norén, O.; Christiansen, L.; Wacker, H.; Semenza, G. A fully active, two-active-site,

single-chain

sucrase.isomaltase

from

pig

small

intestine.

Implications for the biosynthesis of a mammalian integral stalked membrane protein. J. Biol. Chem. 1980, 255, 11332–11338. 46) Houdijk, J. G.; Bosch, M. W.; Tamminga, S.; Verstegen, M. W.; Berenpas, E. B.; Knoop, H. Apparent ileal and total-tract nutrient digestion by pigs as affected by dietary nondigestible oligosaccharides. J. Anim. Sci. 1999, 77, 148–158. 47) Smiricky-Tjardes, M. R.; Grieshop, C. M.; Flickinger, E. A.; Bauer, L. L.; Fahey, G. C. Jr. Dietary galactooligosaccharides affect ileal and total-tract nutrient digestibility, ileal and fecal bacterial concentrations, and ileal fermentative characteristics of growing pigs. J. Anim. Sci. 2003, 81, 2535–2545. 48) Urriola, P. E.; Stein, H. H. Effects of distillers dried grains with solubles on amino 22


Page 23 of 27


acid, energy, and fiber digestibility and on hindgut fermentation of dietary fiber in a corn-soybean meal diet fed to growing pigs. J. Anim Sci. 2010, 88, 1454–1462. 49) Oku, T.; Tanabe, K.; Watanabe, Y.; Ono, H.; Naruse, M.; Nakamura, S. Effects of non-digestible oligosaccharides with different properties on Ca and Mg metabolism in rats. J. Jpn. Soc. Nutr. and Food Sci. 2007, 60, 233–240. (In Japanese).

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Figure captions Figure 1. Comparison of nondigestible oligosaccharides in cookies using the improved method and the existing AOAC method

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Tables Table 1. Nutrient composition and carbohydrate ingredients of the syrups per 100 g

FOS, fructooligosaccharide; GOS, galactooligosaccharide.

Table 2.

Analyses of nondigestible oligosaccharides in the syrups using the improved method and the existing AOAC method and comparison with nutritional label values The value in brackets shows relative ratio of nondigestible oligosaccharide determined by each method and that on the label. Analytical values are expressed as the mean± SD in duplicate experiments; Nondigestible fractions, ≥DP 2; FOS, fructooligosaccharide; GOS, galactooligosaccharide. 25



Figures Figure 1.

Data was expressed average of duplicate analysis. The nondigestible oligosaccharide fractions were had DP ≥ 2. N.D., not detected.

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Determination Trial of Nondigestible Oligosaccharide in Processed

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