Modification to AOAC Official Methods 2009.01 and 2011.25 to Allow for Minor Overestimation of Low Molecular Weight Soluble Dietary Fiber in Samples Containing Starch

2014 ◽  
Vol 97 (3) ◽  
pp. 896-901 ◽  
Author(s):  
Barry V McCleary

Abstract AOAC Official Methods 2009.01 and 2011.25 have been modified to allow removal of resistant maltodextrins produced on hydrolysis of various starches by the combination of pancreatic α-amylase and amyloglucosidase (AMG) used in these assay procedures. The major resistant maltodextrin, 63,65-di-α-D-glucosyl maltopentaose, is highly resistant to hydrolysis by microbial α-glucosidases, isoamylase, pullulanase, pancreatic, bacterial and fungal α-amylase and AMG. However, this oligosaccharide is hydrolyzed by the mucosal α-glucosidase complex of the pig small intestine (which is similar to the human small intestine), and thus must be removed in the analytical procedure. Hydrolysis of these oligosaccharides has been by incubation with a high concentration of a purified AMG at 60°C. This incubation results in no hydrolysis or loss of other resistant oligosaccharides such as FOS, GOS, XOS, resistant maltodextrins (e.g., Fibersol 2) or polydextrose. The effect of this additional incubation with AMG on the measured level of low molecular weight soluble dietary fiber (SDFS) and of total dietary fiber in a broad range of samples is reported. Results from this study demonstrate that the proposed modification can be used with confidence in the measurement of dietary fiber.

2010 ◽  
Vol 93 (1) ◽  
pp. 221-233 ◽  
Author(s):  
Barry V McCleary ◽  
Jonathan W De Vries ◽  
Jeanne I Rader ◽  
Gerald Cohen ◽  
Leon Prosky ◽  
...  

Abstract A method for the determination of total dietary fiber (TDF), as defined by the CODEX Alimentarius, was validated in foods. Based upon the principles of AOAC Official MethodsSM 985.29, 991.43, 2001.03, and 2002.02, the method quantitates high- and low-molecular-weight dietary fiber (HMWDF and LMWDF, respectively). In 2007, McCleary described a method of extended enzymatic digestion at 37C to simulate human intestinal digestion followed by gravimetric isolation and quantitation of HMWDF and the use of LC to quantitate low-molecular-weight soluble dietary fiber (LMWSDF). The method thus quantitates the complete range of dietary fiber components from resistant starch (by utilizing the digestion conditions of AOAC Method 2002.02) to digestion resistant oligosaccharides (by incorporating the deionization and LC procedures of AOAC Method 2001.03). The method was evaluated through an AOAC collaborative study. Eighteen laboratories participated with 16 laboratories returning valid assay data for 16 test portions (eight blind duplicates) consisting of samples with a range of traditional dietary fiber, resistant starch, and nondigestible oligosaccharides. The dietary fiber content of the eight test pairs ranged from 11.57 to 47.83. Digestion of samples under the conditions of AOAC Method 2002.02 followed by the isolation and gravimetric procedures of AOAC Methods 985.29 and 991.43 results in quantitation of HMWDF. The filtrate from the quantitation of HMWDF is concentrated, deionized, concentrated again, and analyzed by LC to determine the LMWSDF, i.e., all nondigestible oligosaccharides of degree of polymerization 3. TDF is calculated as the sum of HMWDF and LMWSDF. Repeatability standard deviations (sr) ranged from 0.41 to 1.43, and reproducibility standard deviations (sR) ranged from 1.18 to 5.44. These results are comparable to other official dietary fiber methods, and the method is recommended for adoption as Official First Action.


2012 ◽  
Vol 95 (3) ◽  
pp. 824-844 ◽  
Author(s):  
Barry V McCleary ◽  
Jonathan W DeVries ◽  
Jeanne I Rader ◽  
Gerald Cohen ◽  
Leon Prosky ◽  
...  

Abstract A method for the determination of insoluble (IDF), soluble (SDF), and total dietary fiber (TDF), as defined by the CODEX Alimentarius, was validated in foods. Based upon the principles of AOAC Official MethodsSM 985.29, 991.43, 2001.03, and 2002.02, the method quantitates water-insoluble and water-soluble dietary fiber. This method extends the capabilities of the previously adopted AOAC Official Method 2009.01, Total Dietary Fiber in Foods, Enzymatic–Gravimetric– Liquid Chromatographic Method, applicable to plant material, foods, and food ingredients consistent with CODEX Definition 2009, including naturally occurring, isolated, modified, and synthetic polymers meeting that definition. The method was evaluated through an AOAC/AACC collaborative study. Twenty-two laboratories participated, with 19 laboratories returning valid assay data for 16 test portions (eight blind duplicates) consisting of samples with a range of traditional dietary fiber, resistant starch, and nondigestible oligosaccharides. The dietary fiber content of the eight test pairs ranged from 10.45 to 29.90%. Digestion of samples under the conditions of AOAC 2002.02 followed by the isolation, fractionation, and gravimetric procedures of AOAC 985.29 (and its extensions 991.42 and 993.19) and 991.43 results in quantitation of IDF and soluble dietary fiber that precipitates (SDFP). The filtrate from the quantitation of water–alcohol-insoluble dietary fiber is concentrated, deionized, concentrated again, and analyzed by LC to determine the SDF that remains soluble (SDFS), i.e., all dietary fiber polymers of degree of polymerization = 3 and higher, consisting primarily, but not exclusively, of oligosaccharides. SDF is calculated as the sum of SDFP and SDFS. TDF is calculated as the sum of IDF and SDF. The within-laboratory variability, repeatability SD (sr), for IDF ranged from 0.13 to 0.71, and the between-laboratory variability, reproducibility SD (sR), for IDF ranged from 0.42 to 2.24. The within-laboratory variability sr for SDF ranged from 0.28 to 1.03, and the between-laboratory variability sR for SDF ranged from 0.85 to 1.66. The within-laboratory variability sr for TDF ranged from 0.47 to 1.41, and the between-laboratory variability sR for TDF ranged from 0.95 to 3.14. This is comparable to other official and approved dietary fiber methods, and the method is recommended for adoption as Official First Action.


2010 ◽  
Vol 93 (1) ◽  
pp. 234-242
Author(s):  
Brett E Post ◽  
Michael R Marshak ◽  
Jonathan W DeVries

Abstract Dietary fiber and its quantitation in foods have been of significant interest in the nutrition community for over 50 years. A number of AOAC Official Methods of AnalysisSM have been adopted for the analysis of dietary fiber and some of its fractions and components commensurate with the evolving discoveries of dietary fiber nutrition research. Quantitation of low-molecular-weight soluble dietary fiber (LMWSDF) has been difficult due to high solubility in a precipitating solvent mixture of four parts alcohol and one part water. AOAC Method 2001.03 effectively quantitates LWMSDF subsequent to gravimetric removal of high-molecular-weight dietary fiber using LC. However, deionization and concentration of the enzymatic digestate, necessary to assure accurate LC quantitation, requires substantial time and manual labor. A modification to the method and resulting method performance is presented that describes a means of simultaneously deionizing the digestate and quantitating the LMWSDF in a single LC injection, eliminating a number of time-consuming manual preparation steps.


Proceedings ◽  
2020 ◽  
Vol 70 (1) ◽  
pp. 105
Author(s):  
Clarice Silva e Souza ◽  
Pamella Cristine Anunciação ◽  
Ceres Mattos Della Lucia ◽  
Rosana Gonçalves Rodrigues das Dôres ◽  
Regina Célia Rodrigues de Miranda Milagres ◽  
...  

Citrus fruit is preferred in the choice of consumers. Kumquat (F. margarita) is an unconventional citrus of increasing consumer interest because of its exotic flavor, and its functional potential that offers health benefits to consumers. It is a fruit traditionally consumed by whole fruit (peel and pulp), giving this fruit a distinctive flavor. For this reason, this study analyzed the physical, chemical, and nutritional characteristics of kumquat (peel and pulp). The physicochemical analysis was performed according to the Adolfo Lutz Institute. Analysis of moisture, ashes, macronutrients, and total dietary fiber was carried out according to AOAC. Minerals were analyzed by inductively coupled plasma optical emission spectrometry. Vitamins C and E, carotenoids and flavonoids were analyzed by HPLC. Phenolic compounds (Folin-Ciocalteu) and antioxidant capacity (DPPH) were determined by spectrophotometry. The kumquat had low pH, soluble solids content and low caloric value. It was a source of dietary fiber, minerals (K, Ca, P, Mg) and carotenoids; the most expressive was α-carotene (661.81 μg 100 g−1). The ascorbic acid concentration was 2326.24 μg 100 g−1. α-tocopherol (569.00 μg 100 g−1) was the most expressive component of vitamin E. There was a presence of apigenin and eriodictyol. The fruit (peel and pulp) has a high concentration of total phenolic compounds (98.55 ± 1.93 mg GAE 100 g−1) and good antioxidant capacity (62%) was found. Kumquat is a good source of fiber and vitamin A, and due to its antioxidant capacity and the presence of other essential and beneficial nutrients for a diet, consumption of kumquat can be suggested to complement the diet. This fruit is a viable food alternative, and its consumption should be encouraged, contributing a source of income, sovereignty, and food security.


2018 ◽  
Vol 1 (4) ◽  
pp. e00057 ◽  
Author(s):  
A.A Chistov ◽  
A.V. Talanova ◽  
M.V. Melnikova ◽  
S.S. Kuznetsova ◽  
E.F. Kolesanova

Low molecular weight chromogenic thrombin peptide substrates, p-nitroanilides of short peptides protected at their N-terminal amino group, were prepared by solid-phase peptide synthesis on polystyrene-divinylbenzene polymer with trityl groups with preliminary attached p-phenylene diamine moiety. After the cleavage from the resin peptide p-aminoanilides were mildly oxidized to p-nitroanilides with the mixture of potassium sulfate and persulfate. Adsorption onto polymer support Bio-Beads SM-2 with further elution by acetonitrile allowed easy separating peptide p-nitroanilides from the oxidizer and obtaining the thrombin chromogenic substrate preparations with the target substance contents of not less than 95% and yields of 30-40%. Thrombin effectively catalyzed hydrolysis of the prepared substrates with KM and Vmax values of 29-134 mM and 0.03-1/16 mM/s, respectively.


1983 ◽  
Vol 11 (6) ◽  
pp. 720-721
Author(s):  
PETER R. FLATT ◽  
CLIFFORD J. BAILEY ◽  
SARA K. SWANSTON-FLATT

2021 ◽  

This method determines total dietary fiber (TDF) in foods and food ingredients, as defined by Codex Alimentarius. The method measures soluble and insoluble dietary fiber, including resistant starch, as well as nondigestible oligosaccharides. In this method, enzymatic digestion is used to simulate human intestinal digestion. Insoluble dietary fiber (IDF) and soluble dietary fiber that precipitates in 78% ethanol (SDFP) are separated by filtration and quantified gravimetrically. Additionally, highly soluble oligosaccharides (SDFS) are quantified by chromatographic separation. TDF is reported as the sum of the gravimetric and high-performance liquid chromatography (HPLC) results. The digestion and chromatographic conditions of this method have been modified from those of AACC Approved Methods 32-45.01 and 32-50.01 in an attempt to better simulate human digestion and to allow for more exact quantitation.


2020 ◽  
Vol 81 (2) ◽  
pp. 301-308 ◽  
Author(s):  
Wenzhe Song ◽  
Yu Zhang ◽  
Amir Hossein Hamidian ◽  
Min Yang

Abstract The biodegradation of polyacrylamide (PAM) includes the hydrolysis of amino groups and cleavage of the carbon chain; however, the effect of molecular weight on the biodegradation needs further investigations. In this study, biodegradation of low molecular weight PAM (1.6 × 106 Da) was evaluated in two aerobic (25 °C and 40 °C) and two anaerobic (35 °C and 55 °C) reactors over 100 days. The removal of the low molecular weight PAM (52.0–52.6%) through the hydrolysis of amino groups by anaerobic treatment (35 °C and 55 °C) was much higher than that of the high molecular weight (2.2 × 107 Da, 11.2–17.0%) observed under the same conditions. The molecular weight was reduced from 1.6 × 106 to 6.45–7.42 × 105 Da for the low molecular weight PAM, while the high molecular weight PAM declined from 2.2 × 107 to 3.76–5.87 × 106 Da. The results showed that the amino hydrolysis of low molecular weight PAM is easier than that of the high molecular weight one, while the cleavage of its carbon chain is still difficult. The molecular weights of PAM in the effluents from the two aerobic reactors (25 °C and 40 °C) were further reduced to 4.31 × 105 and 5.68 × 105 Da by the biofilm treatment, respectively. The results would be useful for the management of wastewater containing PAM.


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