Gluten: properties and nonfood potential.

Gluten, the storage protein of wheat endosperm, was reviewed at the annual meeting of the American Association of Cereal Chemistry. Many studies have shown that gluten consists mainly of two protein subclasses, gliadin and glutenin. Each of these is a complex mixture of several protein types with unusual structures. These proteins interact, in the kernel and upon subsequent processing, through disulfide and noncovalent bonds to form complex gluten polymers. Upon rehydration and mixing, gluten orients and further associates into a unique viscoelastic network. These properties explain gluten's critical importance in breadmaking: the protein network expands to retain gas generated during fermentation and stabilizes upon heating into a light, porous structure. A major industry exists to isolate functional gluten. `Vital' gluten is used primarily in foods, but has many other possible industrial uses because of its elastic, viscous, adhesive, film-forming, and thermosetting properties. Native or modified gluten can be used in films, plastics, adhesives, graft polymers, and many other products. However, most nonfood applications seem little used, mostly because of competition from petrochemical-based alternatives. Today, interest in such new uses is growing again, for many reasons. Gluten is abundant, renewable, domestically available, easily isolated, low in cost, `natural', and biodegradable. Further research on gluten's applications and more fundamental information about its properties are necessary to enhance gluten's industrial utilization, benefiting everyone from producer to consumer.

Capillary electrophoresis: a state-of-the-art technique for wheat protein characterization.

Capillary electrophoresis (CE), a modern instrumental method of protein analysis, now gives excellent separations of wheat gluten proteins. Methods were developed first to analyze gliadin. Variables examined include protein extractant; buffer type, source, and pH; buffer additives (SDS, acetonitrile, reducing agents, polymeric matrices); capillary length and diameter; voltage; temperature; and injection mode. The best separations were at 22 kV with 0.1M phosphate buffer, pH 2.5, containing a linear hydrophilic polymer, using a `20 cm x 20 µm' i.d. uncoated silica capillary. Resolution in 10 min is as good as or better than that of reversed-phase high-performance liquid chromatography (RP-HPLC). However, the major advantage of CE is that it complements RP-HPLC, as shown by analyzing isolated RP-HPLC peaks. CE also is the first automated and accurately quantifiable electrophoresis method. Excellent inter-laboratory reproducibility can be achieved, but buffer composition is critical. CE can readily differentiate wheat varieties, including sister lines, and should be useful for selection during breeding and in genetic studies. Modified ProSort(c) technology (Werner et al. Cereal Chem 1994 91:397) also was used to reveal variation among Glu-D1 high molecular weight glutenin subunits in several cultivars. Observed heterogeneity paralleled that shown by SDS-PAGE, but some differences in relative mobility of protein bands were observed. These and other separation modes will make CE an indispensable analytical tool for wheat protein analysis.

Capillary electrophoresis (CE): reproducibility and resolution of cereal proteins in uncoated capillaries.

Two of the most important factors in optimizing reproducibility and resolution of cereal proteins in uncoated capillaries are rinsing (cleaning) protocols and buffer makeup. Various capillary cleaning procedures were studied to improve migration time reproducibility: water only; sodium hydroxide (0.1 M) only; phosphoric acid (1 M) only; and a combination of phosphoric acid, sodium hydroxide, and water. The optimum reproducibility was obtained with a rinsing protocol of 4 min with 1 M phosphoric acid. Resolution was improved by the addition of certain organic solvents to the buffer. Various concentrations of acetonitrile, dimethylformamide, dimethylsulfoxide, ethylene glycol, methanol, and 2-propanol were studied: 20 % acetonitrile produced the highest resolution (best baseline resolved peaks). Separations on a `27 cm x 20 µm' (i.d.) capillary were completed in 18 min with relative standard deviations of 0.1 % on 15 peaks.

A fast method for wheat cultivar differentiation using capillary zone electrophoresis (CZE).

CZE conditions for the shortest analysis time include: capillary inside diameter, 20 µm; shortest possible capillary length, 27 cm (20 cm to detector); temperature, 45_C; voltage, 22 kV; and pressure injection for 4 sec (0.25 nL). Three alcohol-water-based solvent systems were studied to improve extraction and analysis of gliadins; 30 % ethanol-water was optimum. Gliadins were extracted from cultivars representative of hard red winter, hard red spring, and soft wheat classes and separated by CZE. Three separate sets of cultivars that were not distinguished by PAGE at pH 3.1 were differentiated in less than 10 min each by CZE. Cultivars that were related closely (sister lines or intercrossings) were differentiated readily, and cultivars that were not genetically close exhibited quite different CZE patterns.

Separation and characterization of wheat protein fractions by high-performance capillary electrophoresis (HPCE).

Wheat protein fractions, separated by the Osborne Solvent Fractionation Procedure, were characterized by HPCE. Each fraction was separated on a 27-cm fused-glass capillary (20 µm, i.d.) using 0.1 M phosphate buffer (pH 2.5) containing hydroxypropylmethylcellulose, a polymer additive, at 45_C and 22 kV constant voltage. Albumins and globulins migrated in the first 4 min, whereas gliadins and glutenins migrated after 4 min. Individual alpha, beta, gamma, and omega gliadin proteins, which were collected from RP-HPLC separations, also were separated by HPCE. Combined results of this study and our previous studies provide a catalog of individual gliadin information from HPCE, HPLC, acid (A)-PAGE, and SDS-PAGE, relating class, relative molecular size, hydrophobicity, relative charge, and separation times of each gliadin subclass by HPLC and HPCE. The main advantages of HPCE are: 1) the complementing of other electrophoretic and chromatographic protein separation methods and 2) safety, because no toxic acrylamides and only minute amounts of organic solvents and buffers are used.

Differentiation of 1AL-1RS from 1BL-1RS wheat-rye translocation lines by capillary electrophoresis.

Wheat-rye translocations, 1BL-1RS and 1AL-1RS, have been used to transfer desirable genes from rye to wheat. Both beneficial and deleterious influences on wheat end-use quality have been identified. The most commonly cited difficulties encountered with 1BL-1RS are reduced gluten strength (diminished mixing tolerance) and dough `stickiness'. CE was used to differentiate 1AL-1RS from 1BL-1RS wheat lines in less than 15 min by analyzing 30 % ethanol or water extracts. Samples analyzed included both near-isogenic lines and a large number of advanced breeding lines from USDA-ARS regional testing nurseries, with and without the rye chromosome segment. Differences in the omega secalins were found. The CE pattern of the 1AL-1RS lines exhibited a doublet with equal peak heights, whereas the pattern of the 1BL-1RS lines had a doublet consisting of a larger peak followed by a one-half size peak, both around 13 min. However, the 1AL-1RS doublet migrated slightly slower than the 1BL-1RS doublet. Sample size ranged from bulk flour to one-half of single wheat kernel.

Development of a supercritical fluid extraction (SFE) method for wheat starch lipids and of a high-performance liquid chromatography (HPLC) method for analysis.

A cooperative study on starch lipids (SL) was conducted between Kansas State University (KSU) and the ARS. A commercial wheat starch (Type I, unmodified, Sigma Chem. Co.) was purified to remove starch surface lipids by stirring for 4 hr at room temperature with a mixture of 1-propanol and water (3:1 v/v). SL were extracted by the SFE method using an ISCO two pump modifier SFE system: the optimum SFE method developed for SL was to use a carbon dioxide SFE at 9,950 psi at 100 C with 30 % 1-propanol-water (3:1, v/v) as a modifier and to decompress just before the dynamic stage. SL were analyzed by a HPLC method, which was developed by us for quantifying lysophosphatidylcholines (LPC) and lysophosphatidylethanolamines (LPE) in SL. The optimum HPLC method was to use a silica column (200 x 4.6 mm, si 100 with a 10 µm bead size), and a gradient elution with Phase A (hexane-2-propanol-water, 48:50:2 v/v/v) and Phase B (35:50:15), starting with 100 % A, going to 25 % B in 7 min, then to 100 % B in 2 min, and holding at 100 % B for 6 min. We reduced SL extraction time from 12 to 2 hr by using an optimum SFE method and HPLC analysis time from 80 to 15 min.

Chromatographic separation of wheat flour glycolipids.

Free lipids from wheat flour, extracted with petroleum ether on a Soxhlet, were fractionated into nonpolar, glyco-, and phospho-lipids by open column silicic acid chromatography. Nonpolar lipids were eluted first by a mixture of chloroform and acetone (4:1 v/v), instead of 100 % chloroform with which the elution of all nonpolar lipid components, especially free fatty acid, was often incomplete. Two main glycolipids, monogalactosyldiglycerides (MGDG) and digalactosyldiglycerides (DGDG), were separated by normal-phase HPLC using a silica column (250 x 4 mm with 5 µm particle size) within 7 min. We could decrease substantially the retention time and flow rate by using a mini column (10 x 4 mm with 5 µm particle size). The separation of MGDG and DGDG was attained in 3 min at a flow rate of 2.6 ml/min and in 5 min at 1.5 ml/min. Because the intensity of absorbance at a low range of UV spectra was affected by the degree of unsaturation in fatty acids, quantifying lipids containing different unsaturations by a UV detector is difficult. The eluted lipids were detected by an evaporative light scattering detector (ELSD) and UV multidiode array detector (UV-MDAD). The chromatograms obtained by ELSD showed no fluctuation on baseline whereas those obtained by UV-MDAD did show baseline fluctuation.

End-use quality evaluation of wheat: past, present, and future.

(Presented at the ICC Meeting at Vienna, Austria.) Differences between U.S. wheat classes are generally use-oriented, and different wheat classes grow in different regions. By Congressional mandate, four ARS Regional Wheat Quality Laboratories (RWQL) were established for improvement of U.S. wheat quality based on their end uses by evaluating breeding lines. In 1936, the Soft Wheat Quality Laboratory was established at Wooster, OH; in 1937, the Hard Winter Wheat Quality Laboratory at Manhattan, KS; in 1946, the Western Wheat Quality Laboratory at Pullman, WA; and in 1963, the Hard Red Spring and Durum Wheat Quality Laboratory at Fargo, ND. All four RWQL evaluate physical and chemical characteristics of grains; experimental milling; flour quality; dough properties; and baking or other end-product, processing, quality parameters for cookies, cakes, breads, spaghetti with durum wheat semolina, and/or noodles, etc. Based on quality data accumulated by the four RWQL during the past 30-60 years, quality-prediction methods for functional properties have been developed and used to predict certain end-use quality parameters by each lab. All four labs replaced the Kjeldahl Method with the Leco N2 Analyzer; use the USGMRL-developed Single-Kernel Wheat Characterization System for grain characteristics; and use the NIRSystem 6500 for chemical parameters of both wheats and flours and for a complete spectral scanning of whole wheats, meals, and flours over 400-2,500 nm. Knowing that biochemical components are responsible for certain functional properties of end products and experimental processing data, we are working toward developing a quality prediction system. The potential of using end-use quality to estimate whole wheat kernels and as a basis of the wheat marketing system is approaching.

Status of the USGMRL single-kernel wheat characterization system (SKWCS).

(Reviewed at the ICC Meeting at Vienna, Austria.) The need for and development of an objective wheat classification system to be used by the USDA, Federal Grain Inspection Service (FGIS) are reviewed with a historical perspective. This presentation includes a brief description of three single kernel hardness determination methods tested by the FGIS before selecting the USGMRL-SKWCS. The methods described are: grinding as developed by the ARS, Beltsville Instrumentation Laboratory; cutting as developed by Kansas State University; and crushing as developed by the U.S. Grain Marketing Research Laboratory (USGMRL). The presentation primarily describes the following: procedures for single-kernel physical measurements of weight, size moisture and hardness; computer-controlled operation of the system; procedures used to establish calibrations as developed by the USGMRL; classification results obtained by FGIS after sampling the U.S. common market wheats; system performance as determined by the USGMRL; recent steps toward commercialization and evaluation of the system; and several on-going studies to relate single-kernel properties of wheat to milling performance.

Varietal and environmental effects on wheat and flour quality parameters.

Wheat and flour quality parameters were determined using 54 hard winter wheat samples from the Wheat Quality Council, consisting of nine wheat varieties grown at six locations including Akron, CO; Colby and Hutchinson, KS; Clay Center, NE; Lahoma, OK; and Vernon, TX. Nine lines were grown and harvested in 1994 by each of five Agricultural Experiment Station sites. Two-way analysis of variance showed significant effects of both varieties (V) and growing locations (environment, E) on most quality parameters, except for no significant V effects on mixograph and bake water absorptions (WA), dough weights, and dough proof heights and no significant E effects on mixograph mix time (MT). Three broad groups of quality parameters were identified: (A) mixograph and bake MT and mixograph mixing tolerances affected more by V; (B) wheat physical parameters, ash and protein contents, flour yields, and mixograph and bake WA affected more by E; and (C) NIR-hardness, % large kernels, flour color values, and bread volumes and crumb grains affected similarly by both E & V.