Determination of total dietary fiber in foods and food products: collaborative study

A collaborative study was conducted to determine the total dietary fiber (TDF) content of food and food products, using a combination of enzymatic and gravimetric procedures. The method was basically the same as published earlier (J. Assoc. Off. Anal. Chem. (1984) 67, 1044-1052), with changes in the concentration of alcohol and buffers, time of incubation, sample preparation, and some explanatory notes, all with the intent of decreasing the coefficient of variation (CV) of the method. Duplicate blind samples of soy isolate, white wheat flour, rye bread, potatoes, rice, wheat bran, oats, corn bran, and whole wheat flour were analyzed by 9 collaborators. TDF was calculated as the weight of the residue minus the weight of protein and ash. CV values of the data from all laboratories for 7 of the samples ranged from 1.56 to 9.80%. The rice and soy isolate samples had CV values of 53.71% and 66.25%, respectively; however, each sample contained only about 1% TDF. The enzymatic-gravimetric method for determining TDF has been adopted official first action.     

Near-infrared analysis of soluble and insoluble dietary fiber fractions of cereal food products

The use of near-infrared (NIR) reflectance spectroscopy for the rapid and accurate measurement of soluble and insoluble dietary fiber was explored in a diverse group of cereal products. Ground samples were analyzed for soluble and insoluble dietary fiber (AOAC Method 991.43) and scanned (NIRSystems 6500 monochromator) to obtain NIR spectra. Modified PLS models were developed to predict insoluble and soluble dietary fiber using data sets expanded to include products with high fat and high sugar contents. The models predicted insoluble dietary fiber accurately with an SECV of 1.54% and an R(2) of 0.98 (AOAC determined range of 0-48.77%) and soluble dietary fiber less accurately with an SECV of 1.15% and an R(2) of 0.82 (AOAC determined range of 0-13.84%). Prediction of independent validation samples by the soluble fiber model resulted in a bias that may be related to the way the reference method treats samples with different soluble fiber constituents. The insoluble fiber model can be used to rapidly monitor insoluble dietary fiber in cereal products for nutrition labeling.     

Determination of total dietary fiber in Japanese foods.

Total dietary fiber was determined in Japanese foods by the Prosky-AOAC method. To accomplish the analyses of unsuitable samples, we introduced a few minor modifications to the versions for (i) seaweed and fruits, (ii) cereals, and (iii) fish and meats. These modified methods were used together with the standard method to obtain results with reasonably good relative standard deviation for 231 foods and 21 groups of mixed foods. In this study, dietary fiber was defined so as not to exclude the nondigestible polysaccharide portions of animal foods. A method was proposed which could estimate more accurately the fiber components of animal foods by measuring the "nondigestible protein" of the fiber sample of the fiber sample by the Biuret colorimetric method, instead of the Kjeldahl method, to avoid deducting the values for aminopolysaccharides. In Japanese diets, the amount of fiber obtained from animals foods was less than 5% of the total intake of dietary fiber.     

Determination of total dietary fiber of intact cereal food products by near-infrared reflectance

Near-infrared reflectance spectra of cereal food products were acquired with a commercial dual-diode-array (Si, InGaAs) spectrometer customized to allow rapid acquisition of scans of intact breakfast cereals, snack foods, whole grains, and milled products. Substantial gains in the performance of multivariate calibration models generated from these data were obtained by a computational strategy that systematically analyzed the performance of various spectral windows. The calibration model based on 137 cereal food products determined the total dietary fiber (TDF) content of a test set of 45 intact diverse cereal food products with root-mean-squared error of cross-validation of between 1.8 and 2.0% TDF, relative to the laborious enzymatic-gravimetric reference method. The calibration performance is adequate to estimate TDF over the range of values found in diverse types of cereal food products (0.7-50.1%). The method requires no sample preparation and is relatively unaffected by specimen moisture content.     

Effect of heat treatment of dietary fiber: interlaboratory study

The effects of thermal treatments on the dietary fiber composition of cereal and potato samples were studied at 8 laboratories using different analytical methods. Thermal treatments included extrusion cooking for cereals, and boiling and frying for potatoes. No changes in the amounts of dietary fiber or starch were observed in the extruded samples. Heat-treated potato samples contained significantly more water-insoluble dietary fiber (cellulose) and less starch than did raw potato. However, this may be due, at least in part, to the sample preparation procedure rather than the heat treatment alone. The study indicates that gravimetric and sequential hydrolysis methods give similar results, but the variation in most cases is still wide. Further standardization of methods is evidently needed, especially if legislative measures for setting limits on the fiber content of foods are to be introduced. Standardization of starch analysis should also be of primary importance in future work on carbohydrate methodology. This can be concluded from the variation in results concerning this extremely important food constituent. It should be noted that the sample matrix in the present study was simpler than that of complex meals or diets.     

Simplified method for determination of total dietary fiber in foods

A simplified method, based on the same principles as the AOAC enzymatic-gravimetric method for determining total dietary fiber (TDF) (43.A14-43.A20), has been tested on 12 food samples which had been used in other collaborative studies. TDF values obtained in our laboratory for these 2 methods were in good agreement (y = 0.96x + 0.39; r = 0.999). The simplified method uses a single incubation period and only 1 enzyme (amyloglucosidase), and thus yields smaller blank and ash corrections but a higher protein correction.     

Analysis of foods for iodine: interlaboratory study

An accurate, reproducible method for less than or equal to 1 ppm iodine in foods is required for nutritional labeling. In order to ascertain the current status of iodine analysis in foods, 7 samples, representing different food classes, were analyzed by 8 laboratories. Six laboratories used their modifications of the Ce-As-I catalytic method preceded by alkaline dry ashing. Two laboratories used neutron activation analysis (NAA), with differing radiochemical separations. The study showed wide discrepancy in analytical results. Mean relative standard deviation for all laboratories was 77.9% between laboratories; 19.1% within-laboratories. Laboratories using NAA had only slightly better precision than did laboratories using the chemical method. The lowest level reported on the entire group of samples ranged among laboratories from 0.0089 to 0.65 ppm. Figures reported by a laboratory are, in general, consistently high or consistently low. The only differences in methodology which may possibly correlate with level of iodine obtained are the use of NAA technique and use of manual, rather than automated, colorimetry.     

Biochemical and microstructural Ccharacteristics of insoluble and soluble dietary fiber prepared from mushroom sclerotia of Pleurotus tuber-regium, Polyporus rhinocerus, and Wolfiporia cocos

The proximate composition of sclerotia of Pleurotus tuber-regium, Polyporus rhinoceros, and Wolfiporia cocos, together with the yield, purity, monosaccharide profile, and microstructure of their insoluble dietary fiber (IDF) and soluble dietary fiber (SDF) fractions prepared from AOAC enzymatic-gravimetric methods were investigated and compared. All three sclerotia were typical carbohydrate rich sclerotia [ranging from 90.5 to 98.1% dry matter (DM)] with an exceptionally low amount of crude lipid content (ranging from 0.02 to 0.14% DM). Besides, all three sclerotia possessed substantial amounts of IDF (ranging from 77.4 to 94.6% DM) with notably high levels of nonstarch polysaccharides (NSP) (89.9-92.2% DM) in which glucose was the predominant sugar residue (90.6-97.2% of NSP DM). On the contrary, both the yield (only ranging from 1.45 to 2.50% DM) and the amount of NSP (ranging from 22.4 to 29.6% DM) of the three sclerotial SDF fractions were very low. Scanning electron micrographs showed fragments of interwoven hyphae and insoluble materials in the three sclerotial IDF fractions, but only an amorphous structure of soluble materials was observed in the SDF fractions. The potential use of these fiber preparations was discussed.     

Determination of water-insoluble cell walls in feeds: interlaboratory study

A collaborative study was conducted to test a new rapid procedure for determination of water-insoluble cell wall (WICW) content in feeds. In the method, starch is solubilized near boiling temperature with Termamyl, a heat-stable alpha-amylase, and proteins are solubilized at 40 degrees C with sodium dodecylsulfate and Pronase. Then, the organic matter of the residue is determined by incineration. Three hours were required to treat 12 different samples, including solubilization treatments, filtrations, and rinses. Eleven unknown products including 9 common feedstuffs of various origin and 2 mixed diets for poultry were analyzed by 7 analysts in France. Coefficients of variation ranged from 2.3 to 6.1%. The results were compared to those for water-insoluble dietary fiber (WIDF), total dietary fiber, and neutral detergent fiber. Agreement was best with the water-insoluble dietary fiber procedure. For most samples, the ratios of WIDF/WICW ranged from 0.981 to 0.842. The differences between WICW and WIDF values correspond to cell wall protein which is accounted for in WICW, but not in WIDF.     

NMR characterization of lignins isolated from fruit and vegetable insoluble dietary fiber

Compositional information for lignins in food is rare and concentrated on cereal grains and brans. As lignins are suspected to have important health roles in the dietary fiber complex, the confusing current information derived from nonspecific lignin determination methods needs to be augmented by diagnostic structural studies. For this study, lignin fractions were isolated from kiwi, pear, rhubarb, and, for comparison, wheat bran insoluble dietary fiber. Clean pear and kiwi lignin isolates allowed for substantive structural profiling, but it is suggested that the significance of lignin in wheat has been overestimated by reliance on nonspecific analytical methods. Volume integration of NMR contours in two-dimensional (13)C-(1)H correlation spectra shows that pear and wheat lignins have comparable guaiacyl and syringyl contributions and that kiwi lignins are particularly guaiacyl-rich (approximately 94% guaiacyl) and suggest that rhubarb lignins, which could not be isolated from contaminating materials, are as syringyl-rich (approximately 96% syringyl) as lignins from any known natural or transgenic fiber source. Typical lignin structures, including those newly NMR-validated (glycerols, spirodienones, and dibenzodioxocins), and resinols implicated as possible mammalian lignan precursors in the gut are demonstrated via their NMR correlation spectra in the fruit and vegetable samples. A novel putative benzodioxane structure appears to be associated with the kiwi lignin. It is concluded that the fruits and vegetables examined contain authentic lignins and that the detailed structural analysis exposes limitations of currently accepted analytical methods.     

超声辅助提取水不溶性大豆膳食纤维及其物理特性

为研究超声辅助提取对豆渣中水不溶性大豆膳食纤维提取效率及物理特性的影响,该文以超声波为辅助,在液料比、超声功率强度、超声温度和超声时间4个单因素试验的基础上,通过四元二次通用旋转组合设计试验优化超声辅助提取水不溶性大豆膳食纤维的工艺条件,并采用扫描电镜、红外光谱仪等对超声辅助、酸溶碱沉、酶解辅助提取所获得的水不溶性大豆膳食纤维产品进行了物理特性表征。优化试验结果表明,在液料比35 mL/g、超声功率强度600 W/g、超声温度50℃、间歇性超声处理累计时间50 min条件下水不溶性大豆膳食纤维提取率较高,达92.11%。物性分析结果显示,与酸溶碱沉、酶解辅助提取的水不溶性大豆膳食纤维相比,超声辅助提取的水不溶性大豆膳食纤维具有更高的持水力、溶胀力、结合水力和结合脂肪能力以及更丰富的空间网状结构。研究结果揭示,超声辅助提取法不仅能够提高豆渣中水不溶性大豆膳食纤维的提取率,而且对其加工性能有很好的改进作用。     

Determination of sulfur amino acids and tryptophan in foods and food and feed ingredients: collaborative study

Samples of 4 foods, 1 animal feed, isolated soy protein, and beta-lactoglobulin were analyzed by 9 laboratories to determine concentrations of cysteine as cysteic acid, methionine as methionine sulfone, and tryptophan. Sulfur amino acids were determined by AOAC method 43.A08-43.A13 for food and feed ingredients, in which samples are oxidized with performic acid before protein hydrolysis with 6N HCl. Tryptophan was determined after protein hydrolysis with 4.2N NaOH. In both methods, free amino acids were separated by ion-exchange or reverse-phase chromatography. Each laboratory was provided with detailed methods and with sealed vials containing solutions of standards. Samples were analyzed in duplicate, and variation between laboratories was determined. Coefficients of variation between laboratories for the 6 samples ranged from 5.50 to 11.8% for methionine as methionine sulfoxide, 8.59 to 17.3% for cysteine as cysteic acid, and 3.87 to 16.1% for tryptophan. Amino acid recoveries were determined by analysis of beta-lactoglobulin and were based on expected levels of each amino acid obtained from amino acid sequence data. The mean recovery of cysteine was 97% with a range of 88-119%. For methionine, mean recovery was 98% (range 89-115%) and for tryptophan, 85% (range 59-102%). Method 43.A08-43.A13 for food and feed ingredients has been adopted official first action for determination of cysteine and methionine in processed foods. The alkaline hydrolysis method has been adopted official first action for determination of tryptophan in foods and food and feed ingredients.     

Determination of natamycin in cheese and cheese rind: interlaboratory collaborative study

A collaborative test on the determination of natamycin in cheese and cheese rind was conducted. Participants were from 37 laboratories in 13 countries. Eight samples, consisting of 4 duplicates, were investigated by a spectrometric method and a liquid chromatographic (LC) method. The spectrometric method gave good results (coefficient of variation [CV] = 12%) and the LC method with ultraviolet detection gave reasonable results (CV = 25%) for levels down to 15 mg/kg (0.9 mg/dm2). For very low levels, a preconcentration step is necessary, but even then quantitation is poor (CV = 35-37%) for both methods at 1.7 mg/kg, although the presence of natamycin can be detected qualitatively. For a level of 0.3 mg/kg, quantitation is poor (CV = 39%) for the LC method and impossible (CV = 60%) for the spectrometric method.     

Comparative contents of dietary fiber, total phenolics, and minerals in persimmons and apples

Dietary fibers, major phenolics, main minerals, and trace elements in persimmons and apples were analyzed and compared in order to choose a preferable fruit for an antiatherosclerotic diet. Fluorometry and atomic absorption spectrometry following microwave digestion were optimized for the determination of major phenolics and minerals. Total, soluble, and insoluble dietary fibers, total phenols, epicatechin, gallic and p-coumaric acids, and concentrations of Na, K, Mg, Ca, Fe, and Mn in whole persimmons, their pulps, and peels were significantly higher than in whole apples, pulps, and peels (P < 0.01-0.0025). Conversely, the contents of Cu and Zn were higher in apples than in persimmons. In persimmons and apples all of the above components were higher in their peels than in whole fruits and pulps. The relatively high contents of dietary fibers, total and major phenolics, main minerals, and trace elements make persimmon preferable for an antiatherosclerotic diet.     

Treatment of cereal products with a tailored preparation of trichoderma enzymes increases the amount of soluble dietary fiber

Nutritionists recommend increasing the intake of soluble dietary fiber (SDF), which is very low in most cereal-based products. Conversion of insoluble DF (IDF) into SDF can be achieved by chemical treatments, but this affects the sensorial properties of the products. In this study, the possibility of getting a substantial increase of SDF from cereal products using a tailored preparation of Trichoderma enzymes is reported. Enzymes were produced cultivating Trichoderma using durum wheat fiber (DWF) and barley spent grain (BSG) as unique carbon sources. Many Trichoderma strains were screened, and the hydrolysis conditions able to increase by enzymatic treatment the amount of SDF in DWF and BSG were determined. Results demonstrate in both products that it is possible to triple the amount of SDF without a marked decrease of total DF. The enzymatic treatment also causes the release of hydroxycinnamic acids, mainly ferulic acid, that are linked to the polysaccharides chains. This increases the free phenolic concentration, the water-soluble antioxidant activity, and, in turn, the phenol compounds bioavailability.     

Fish species identification using PCR-RFLP analysis and lab-on-a-chip capillary electrophoresis: application to detect white fish species in food products and an interlaboratory study

Identification of 10 white fish species associated with U.K. food products was achieved using PCR-RFLP of the mitochondrial cytochrome b gene. Use of lab-on-a-chip capillary electrophoresis for end-point analysis enabled accurate sizing of DNA fragments and identification of fish species at a level of 5% (w/w) in a fish admixture. One restriction enzyme, DdeI, allowed discrimination of eight species. When combined with NlaIII and HaeIII, specific profiles for all 10 species were generated. The method was applied to a range of products and subjected to an interlaboratory study carried out by five U.K. food control laboratories. One hundred percent correct identification of single species samples and six of nine admixture samples was achieved by all laboratories. The results indicated that fish species identification could be carried out using a database of PCR-RFLP profiles without the need for reference materials.     

提高大豆渣膳食纤维中可溶性成分的方法研究

以大豆渣为原料,采用微生物发酵、微射流均质机高压均质处理和高温蒸煮的方法来提高大豆膳食纤维中可溶性成分含量,研究不同发酵时间、不同处理压力和蒸煮温度以及蒸煮时间对提高豆渣可溶性膳食纤维（SDF）含量的影响。结果表明：利用发酵法可提高可溶性膳食纤维的含量达15%之多,并且在发酵的前6天,SDF含量增长很快,6 d后SDF的含量变化较少;而高压均质处理法提高可溶性膳食纤维含量的幅度在10%～28%之间,并随着处理压力的升高而增大;高温蒸煮法能提高可溶性膳食纤维的含量20%,121℃,20 min为较理想的蒸煮条件。     

Heavy metal, total arsenic, and inorganic arsenic contents of algae food products

The total arsenic, inorganic arsenic, lead, cadmium, and mercury contents of 18 algae food products currently on sale in Spain were determined. The suitability of the analytical methodologies for this type of matrix was confirmed by evaluating their analytical characteristics. The concentration ranges found for each contaminant, expressed in milligrams per kilogram of dry weight, were as follows: total arsenic, 2.3-141; inorganic arsenic, 0.15-88; lead, < 0.05-1.33; cadmium, 0.03-1.9; and mercury, 0.004-0.04. There is currently no legislation in Spain regarding contaminants in algae food products, but some of the samples analyzed revealed Cd and inorganic As levels higher than those permitted by legislation in other countries. Given the high concentrations of inorganic As found in Hizikia fusiforme, a daily consumption of 1.7 g of the product would reach the Provisional Tolerable Weekly Intake recommended by the WHO for an average body weight of 68 kg. A more comprehensive study of the contents and toxicological implications of the inorganic As present in the algae food products currently sold in Spain may be necessary, which might then be the basis for the introduction of specific sales restrictions.     

超声波改善大蒜秸秆不溶性膳食纤维结构及吸附性

为了增强大蒜秸秆膳食纤维的功能特性,采用超声波对大蒜秸秆的不溶性膳食纤维(insoluble dietary fiber,IDF)进行改性处理。以提高葡萄糖吸附能力为目标,利用单因素试验和响应面法优化大蒜秸秆IDF的超声改性条件,通过胆固醇结合力、吸水性、持油性及膨胀能力等来评价改性后IDF的功能特性,并通过扫描电镜和红外光谱分析其结构变化。结果表明:液料质量比30:1、超声功率700 W和超声时间40 min时,大蒜秸秆IDF的葡萄糖吸附能力明显提高,比对照组提高了12.8%,胆固醇吸附力则提高了45.0%(P0.05);超声处理所得IDF的色泽品质和物理化学特性也明显优于对照组(P0.05);超声处理和对照IDF的红外吸收光谱基本相同,电镜结果显示超声波处理使IDF的组织结构变得更加疏松,其表面呈现蜂窝状,有助于表现出较强的吸附性,从而赋予大蒜秸秆IDF更强的功能品质和物理化学特性。