Chemical composition and selected quality characteristics of new types of precooked wheat and spelt pasta products

Journal Pre-proofs Chemical composition and selected quality characteristics of new types of precooked wheat and spelt pasta products Agnieszka Wójtowicz, Anna Oniszczuk, Kamila Kasprzak, Marta Olech, Marcin Mitrus, Tomasz Oniszczuk PII: DOI: Reference:

S0308-8146(19)31800-X https://doi.org/10.1016/j.foodchem.2019.125673 FOCH 125673

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Food Chemistry

Received Date: Revised Date: Accepted Date:

15 March 2019 6 September 2019 7 October 2019

Please cite this article as: Wójtowicz, A., Oniszczuk, A., Kasprzak, K., Olech, M., Mitrus, M., Oniszczuk, T., Chemical composition and selected quality characteristics of new types of precooked wheat and spelt pasta products, Food Chemistry (2019), doi: https://doi.org/10.1016/j.foodchem.2019.125673

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Chemical composition and selected quality characteristics of new types of precooked wheat and spelt pasta products

Agnieszka Wójtowicz1, Anna Oniszczuk2*, Kamila Kasprzak2, Marta Olech3, Marcin Mitrus1, Tomasz Oniszczuk1*

1Department

of Thermal Technology and Food Process Engineering, University of Life Sciences in Lublin, Lublin, Poland

2Department 3Department

of Inorganic Chemistry, Medical University of Lublin, Lublin, Poland

of Pharmaceutical Botany, Medical University of Lublin, Lublin, Poland

* Corresponding authors: Dr. Anna Oniszczuk, Dr. Tomasz Oniszczuk Mailing address: 20-612 Lublin, Głęboka 31, Department of Thermal Technology and Food Process Engineering, University of Life Sciences in Lublin, Poland or 20-093 Lublin, Chodźki 4a, (Collegium Pharmaceuticum), Department of Inorganic Chemistry, Medical University in Lublin, Poland Phone: +48814456127 or +48814487160 E-mail address: [email protected], [email protected], [email protected], [email protected], [email protected], [email protected] Abstract: New types of precooked pasta products have been developed based on refined and wholegrain wheat and spelt flours. The resulting dry pasta was then assessed for chemical composition, including amino acids composition, phenolics content, as well as antioxidant activity. 1

The precooked pasta quality was also evaluated for starch gelatinization degree, physical properties, hardness, color profile of dry and hydrated pasta, and sensory characteristics. We found that the application of the extrusion-cooking technique for wheat and spelt pasta processing allows to achieve instant products with good nutritional characteristics and high degree of gelatinization, as well as attractive quality and sensory profiles. Microstructure showed compact and dense internal structure with visible bran particles if wholegrain flours were used. Wholegrain wheat and wholegrain spelt precooked pasta were characterized by better nutritional composition and greater antioxidant potential, but lower firmness and increased adhesiveness when compared with refined flours.

Keywords: precooked pasta, extrusion-cooking, wheat, spelt, amino acids, antioxidant activity, physical properties, microstructure

Highlights: New types of precooked wheat and spelt pasta products have been developed. Extrusion-cooking apply for treatment of wheat and spelt pasta allows to achieve instant products. Wholegrain pasta showed better nutritional composition and greater antioxidant potential than that from refined flour. The new pasta types showed high gelatinization degree, compact structure and attractive quality.

1. Introduction Over the past few decades, there has been a growing interest in the nutritional quality and other properties of food, the origin of raw materials, and links between quality and the nutritional value of food processed by means of different methods. Research has revealed that wholegrain pasta can be a nutritionally valuable supplement to any diet. The associated health benefits of higher fiber and 2

phenolics consumption are reduced risk of some types of diseases (such as breast cancer and coronary heart disease), stable blood glucose and insulin levels, lower concentration of blood lipids, reduced risk of cardiovascular disease and better control of diabetes, let alone the absence of constipation and better weight management (Katcher et al., 2008). Dieticians, thus, recommend regular consumption of wholegrain cereal products in the form of bread, pasta, biscuits or snacks (Vasanthan, Gaosong, Yeung & Li, 2002). Conventional pasta products are obtained by the pressing of flour (semolina) dough through a die to form the required shape and then drying it. The process of conventional pasta pressing is characterized by low shear values, as well as heat values (30-40°C) that are insufficient to cook the material. Instant pasta from starchy materials requires the dough be prepared differently. Herein, the relevant raw material is mixed with water, then pressed to obtain the desired shape and subsequently treated with hot water, overheated steam or hot oil long enough to lead to starch gelatinization (Kruger, Matsuo & Dick, 1996). An alternative way to produce instant pasta from various raw materials is the extrusion-cooking process. This is a modern HTST (high temperature short time) process of a short-term heating of dough at a high temperature, under high pressure (Mercier, Linko & Harper, 1998). During the processing, several interactions between the components of the dough take place to produce the desired textural and sensory properties (Bouasla, Wójtowicz & Zidoune, 2017; Gull, Prasad & Kumar, 2018; Wójtowicz & Mościcki, 2009, 2014). The use of variable extrusion parameters, such as the length of the plasticizing unit, the screw compression ratio, the intensity of shear rate during processing, the moisture content of raw materials, material residence time in the chamber, the screw speed, the quantity of specific energy supplied to the material, and many other variables may affect the properties of the extrudates (Mercier et al., 1998; Mościcki, 2011).

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Wheat (Triticum aestivum), whether refined or wholegrain, is the most popular raw material in bread and pasta processing. The chemical composition of wheat varies depending on the variety, agronomic conditions and climate area (Konvalina, Capouchová, Stehno, Moudrý & Moudrý, 2011). Refined wheat products are commonly used in the processing of bread, pasta, cookies, bakery products, breakfast cereals, and many other food items. Wheat grains are a good source of nutritionally valuable minerals (especially magnesium), B-group vitamins, vitamin E, several antioxidant compounds (phenolic acids, carotenoids, etc.), as well as many hormonally active compounds (i.e. lignans). Wholegrain wheat flour is especially valuable because of its higher dietary fiber content compared to refined flour. Spelt (Triticum aestivum var. spelta) flour has a delicate nutty flavor that adds an intensive aroma to bread and other baked goods. Wholegrain spelt flour is used for baking bread and for making pastry, as a thickener for soups, sauces, noodles and dumpling products or even in brewing (Bonafaccia, Galli, Francisci, Mair, Skrabanja & Kreft, 2000; Ranhotra, Gelroth, Glaser & Lorenz, 1996). Spelt flour contains nutrients that have a positive impact on the immune system, on minimizing fatigue and energy loss, on removing toxins and lowering the cholesterol level in blood (Kohajdová & Karovičová, 2007). Moreover, it is recommended in the prevention of cancer and cardiovascular disease because of its positive effect on blood circulation. It is helpful in allergy relief and in treating and managing liver and kidney diseases, as well as in preventing the formation of gallstones. Spelt is generating interest due to the aforesaid characteristics, especially in Europe. Furthermore, consumer feedback shows that spelt-based products may be more digestible and therapeutically beneficial compared to those made from common wheat. The aim of this study was to determine the effect of flour type on the chemical composition, nutritional value and selected quality properties of extrusion-cooked pasta products. Refined and wholegrain wheat and spelt flours were used in the experiments. The extrusion-cooking technique 4

was applied for the processing of precooked pasta, ready-to-eat after a short-time hot-water hydration.

2. Materials and Methods

2.1. Materials Several commercial types of flours: common wheat (CW) flour type 500 (Polskie Młyny, Poland), wholegrain wheat (WGW) flour (Lubella SA, Poland), white spelt wheat (SW) flour TBL-70 and wholegrain spelt (WGS) flour TGL-200 (country of origin Hungary, distributor Radix-Bis, Rotmanka, Poland) were used for manufacturing the precooked pasta. The chemical composition of the raw materials, based on producers’ data, is shown in Table 1.

2.2. Precooked pasta preparation The raw materials were moistened to 32% of dough moisture content by adding water corresponding to the initial moisture content of flour, mixed with a laboratory mixer for 15 minutes and rested for 0.5 h to achieve a uniform moisture distribution. The pasta material was processed using a modified single-screw extruder TS-45 (ZMCh Metalchem, Gliwice, Poland) with the length to diameter ratio of L/D=16, at a screw speed of 100 rpm. The process was conducted at a temperature of 85°C in section I, 105°C in section II, 75°C in the cooling section and 65°C at the forming die plate. The cooling section ending the extruder plasticizing unit in the processing of precooked pasta reduces product temperature, limits its expansion and decreases the stickiness of pasta strands (Wójtowicz & Mościcki, 2014). The pasta was formed for spaghetti-type products in a forming die with 12 openings of 0.8 mm in diameter and a depth of 20 mm each. It was subsequently dried in an air oven at 40°C and up to 7% of moisture content, and stored in the dry form in sealed bags for further testing. 5

2.3. Chemical analyses 2.3.1. Proximate chemical composition In dry pasta products, proximate chemical composition was determined in triplicate according to standard AACC methods (2000): protein content in keeping with AACC 46-10 (Nx6.25), fat content as per AACC 30-10, ash content pursuant to AACC 08-01, as well as total dietary fiber TDF content and its fractions (soluble SDF and insoluble IDF as indicated by the gravimetric enzymatic method) according to AACC 32-07. The gelatinization degree was assessed in duplicate by way of the enzymatic method, with the application of β-amylase (Taka-Diastase, Fluka BioChemica, Buchs, Switzerland) for starch hydrolysis, and jodometric measurements of reduced sugars expressed as a percentage of gelatinized starch (Wójtowicz & Mościcki, 2009).

2.3.2. Amino acids composition Amino acids were determined in dry pasta using the AAA 400 amino acid analyzer (INGOS, Czech Republic) via ion exchange chromatography, with post column ninhydrin-based detection being by means of using a sodium citrate buffer at pH 5.5, followed by applying the HPLC method (Konvalina et al., 2011). Ninhydrin amino acid derivatives were detected at 570 nm for primary amino acids and at 440 nm for secondary amino acids. The rate flow of lithium buffers was 0.2 mL/min and that of ninhydrin solution was 0.3 mL/min, the column temperature was kept at 40–70°C and the detector at 121°C. Analysis was performed twice. The content of tryptophan was not measured. The analytical procedure followed producer’s recommendations.

2.3.3. Phenolics content and antioxidant activity In determining phenolic acids and antioxidant potential in the dry pasta, extracts of the tested pasta were prepared through application of the ultrasound-assisted extraction method (USAE). Herein, 2 g 6

of the tested sample were quantitatively transferred to a glass flask with 40 mL of 100% methanol added. The flasks were then placed in an ultrasound bath equipped with a thermostat. The extraction was performed for 40 min at 60°C, with the ultrasound frequency of 33 kHz at 320 W. The extract was filtered through a paper filter, and then the solvent was evaporated. The residues were dissolved with methanol, refilled to 5 mL in volume with methanol and filtered with a 0.45 µm syringe filter (Kręcisz, Waksmundzka-Hajnos & Oniszczuk, 2017; Waksmundzka-Hajnos, Wianowska, Oniszczuk & Dawidowicz, 2008). Phenolic acids were analyzed in triplicate by means of high-performance liquid chromatography and electrospray ionization mass spectrometry (HPLC-ESI-MS/MS). Identified phenolic acids were quantified based on their peak areas and compared with a calibration curve obtained from corresponding standards by validating retention time and mass. MS detection was performed utilizing a 3200 QTRAP Mass spectrometer (AB Sciex, USA) equipped with an electrospray ionization source (ESI) and a mass analyzer (Applied Biosystems, Darmstadt, Germany) (Oniszczuk, Olech, Oniszczuk, Wojtunik-Kulesza, & Wójtowicz, 2017; Oniszczuk, Waksmundzka-Hajnos, SkalickaWoźniak & Głowniak 2013). The Multiple Reaction Mode (MRM) was used to monitor formation of multiple product ions from one precursor ion. Particular analytes were identified by comparing retention time and two intensive MRM transitions for every analyte (one MRM transition for 4hydroxybenzoic acid). The most intensive MRM transition was used for compound quantification. Detailed information about conditions and monitored MRM transitions (MRM pairs) are given in Supplementary Table 1. The antioxidant properties of the obtained extracts were examined in triplicate by way of applying the TLC-DPPH test. For the stationary phase, silica gel plates were used, while a mixture of acetonitrile, water, chloroform and formic acid was exploited for the mobile phase (30:2:5:2, v/v/v/v). Herein, a standard solution of 0.5 mg/mL rutin was prepared and it and 10 μL aliquots of 7

extracts were applied to plates using the automatic TLC applicator Desaga AS -30. After developing in a vertical chamber (DS-II, Chromdes, Lublin, Poland) and drying, the plates were sprayed with a 0.1% methanol solution of DPPH and scanned every 5 min. The images were processed using Sorbfil Videodensitometer TLC software (Sorbpolymer, Krasnodar, Russia). The intensity and size of spots were analyzed, and the areas under peaks were measured and compared with that of rutin (Oniszczuk, Oniszczuk, Wójtowicz, Wojtunik, Kwaśniewska & Waksmundzka-Hajnos, 2015). Assessment of antioxidant activity involved the evaluation of radical scavenging activity determined spectrophotometrically against that of a DPPH radical (1,1-diphenyl-2-picrylhydrazyl). In doing so, 2 mL of DPPH (0.1 mM) mixed with 1 mL of methanol was used as the reference sample. The analyzed extracts (1 mL) were mixed with 2 mL of prepared DPPH solution (0.1 mM), and each measurement against the DPPH radical (methanol extract of 0.4 mg/mL concentration) was repeated three times at 517 nm, at room temperature. The antioxidant activity was calculated as the % DPPH radical scavenging activity (% difference in absorbance of the reference sample and absorbance of the sample with tested extracts) in accordance with Oniszczuk et al. (2019).

2.4. Physical properties Minimal hydration time was evaluated every 0.5 min of hot water hydration according to the AACC (2000) method 66-50. The radial expansion index of the dry pasta was expressed as the ratio of pasta diameter to the diameter of the forming die. The water holding capacity (WHC) was calculated as the percentage of water (%) absorbed during pasta hydration in hot water (Wójtowicz & Mościcki, 2009). Cooking loss (CL) was determined as the amount of pasta components passing into the solution after hydration by the evaporation of water at a temperature of 110°C to constant weight (Sozer, Dalgıc & Kaya, 2007). The water absorption index (WAI) and water solubility index (WSI)

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were determined by the centrifuge method modified in-house to meet the needs of pasta products (Wójtowicz & Mościcki, 2014). All measures were in triplicate. Texture characteristics were determined via the universal testing machine Zwick-Roell (Ulm, Germany) with a 0.5 kN head. Dry pasta hardness was evaluated by means of applying a cutting test utilizing the Warner-Bratzler blade with 100 mm/min head speed. The texture profile (firmness and adhesiveness) was tested for cooked pasta after 5 minutes of hydration using a 5-blade Kramer cell, where 100 g of hydrated pasta was placed in a test chamber, and a double compression test was performed with the head speed of 100 mm/min (Bouasla et al., 2017). All texture tests were repeated five times.

2.5. Pasting properties The pasting properties were determined using the Brabender Micro Visco-Amylo-Graph (Brabender GmbH & Co. KG, Duisburg, Germany). Suspensions of ground dry pasta (10% w/w dry mass basis) in distilled water were prepared by continuous stirring. The pasting properties of the suspensions were then assessed in accordance with Mitrus, Wójtowicz, Oniszczuk, Gondek and Mościcki (2017). The pasting temperature (PT), peak viscosity (PV) – the maximum viscosity during heating, hot paste viscosity (HPV) after a holding period at 93°C, cold paste viscosity (CPV) after cooling down to 50°C, breakdown (BD) and setback (SB) were recorded using Viscograph 4.11 software. The measurements were performed in duplicate.

2.6. Pasta color profile The color of the raw flour and the dry and hydrated pasta was evaluated using the Colour and Appearance Measurements Lovibond CAM-System 500 (The Tintometer Ltd., UK). The CIE-Lab scale was used for the evaluation of L* for luminosity, a* for (+)redness-(-)greenness and b* for 9

(+)yellowness-(-)blueness, following Bouasla et al. (2017) and Wójtowicz et al. (2017). The measurements were performed as 20 replications for each sample.

2.7. Microstructure observations The microstructure of dry pasta was observed using a scanning electron microscope (SEM) with various magnifications: x100 and x600 for surface and x125, x600 and x2000 for cross-sectional internal structure (Bouasla et al., 2016). Pasta samples of 3-5 mm long were mounted using silver tape and sprayed with gold in the vacuum sublimator K-550X (Emitech, RC, Ashford, England). Microstructure pictures were taken via the VEGA LMU microscope (Tescan, Warrendale, PA, U.S.A.) operating at the accelerating voltage of 10 kV.

2.8. Sensory analysis The sensory attributes were evaluated after hot water hydration (Martinez, Ribotta, León, & Añón, 2007). For the hydrated pasta, we evaluated the color, shape, appearance, taste, stickiness and overall quality as the mean of the results of three independent tests. A 15-member semi-trained panel (7 male and 8 females, age 23-40 years) assessed pasta products in a 9-point hedonic scale, where: 1 = extremely dislike, 5 = neither like nor dislike, and 9 = extremely like. Acceptability of pasta products was evaluated in relation to sensory preferences. The products were considered acceptable if their mean scores for an overall acceptability were above 5 (Bouasla et al., 2017).

2.9. Statistical analysis The results were reported as means of multiple measurements ± standard deviation. The analysis of variance (ANOVA) with the Duncan test at the confidence level of α=0.05 was carried out using Statistica 13.0 (Statsoft, Poland). 10

3. Results and discussion 3.1. Chemical proximate composition The flour types used for pasta processing were characterized by varied protein content, with the highest amount of protein (16.7%) reported in wholegrain spelt (WGS) flour (Table 1). The difference in protein content between spelt and common wheat was about 5%. Fat content in refined flours was lower (around 1.0%) than in wholegrain wheat and spelt flours because the fatty components, concentrated in the bran and germ, are removed during milling. Fiber amount was also almost twice as high for wholegrain flours because of the presence of kernel outside layers rich in fibrous components. Moreover, ash content, indicating the number of mineral components, was significantly higher for spelt flour pasta, which confirms the results presented by Kohajdová and Karovičová (2007). Bonafaccia et al. (2000) reported protein content from 15.9 to 17.1% and ash content of 1.76-1.85% and 12.9-13.8% of total dietary fiber for various spelt cultivars. In general, spelt may contain higher levels of protein, soluble dietary fiber and minerals (zinc, selenium, lithium, phosphorus, magnesium) depending on the genotype. Thus, spelt consumption is thought to have more positive nutritional consequences compared to common wheat (Escarnot, Jacquemin, Agneessens & Paquot, 2012). Table 1 presents the chemical composition of dry instant pasta made with various types of flour. Lower values of protein and fat content in the processed pasta compared to the raw materials may result from the formulation of protein-lipid and starch-lipid complexes that are characteristic of the extrusion-cooking process (Bouasla et al., 2016; Mercier et al., 1998; Mościcki, 2011). Herein, formation of starch–lipid complexes is reflected by processing conditions such as motor torque, die pressure, product temperature, specific mechanical energy (SME), water feed content, screw speed, or barrel temperature. De Pilli et al. (2012) found a considerable increase of oil loss (up to 40% of the basic level) after extrusion-cooking, while increased temperature had a significant effect on lower oil 11

amounts in rice starch and pistachio nut flour extrudates. The moisture content, in contrast, showed less significant effect. This phenomenon may be connected with lower extractability of lipids from complexes formed during extrusion processing. Lipid complexation with amylose is a very important reaction in extrusion-cooking that affects structure formation and the texture of the extruded products (Ilo et al., 2000). Helbron et al. (1983) found that DSC endothermic peaks of extrudates made of rice starch and oleic acid showed at 93–104°C, which is the characteristic melting temperature range of amylose and oleic acid complexes. In our study, similar temperatures were applied for the processing of wheat and spelt pasta, so similar behavior could have occurred. Extrusion-cooking treatment also denatures the enzymes that can promote oxidation, and lipids bound by starch are less susceptible to oxidation, so the extrusion-cooking process can minimize lipids oxidation, thus increasing the nutritional and sensory quality of food and feed (Singh, Gamlath & Wakeling, 2007). The highest protein content was reported in wholegrain pasta products, both made with wheat and with spelt flours. CW pasta exhibited the lowest fat and ash content. Kohajdová and Karovičová (2007) examined bread made from whole meal spelt flour, and revealed a protein content of 17.3% and an ash content of 2.21%. Dietary fiber is conventionally classified into two categories according to water solubility: IDF or insoluble dietary fiber (cellulose, part of hemicellulose and lignin) and SDF or soluble dietary fiber (pentosans, pectins, gums, mucilage) (Esposito, Arlotti, Bonifati, Napolitano, Vitale & Fogliano, 2005). The main physiological effect of insoluble fiber is the improvement of gut peristalsis, which is connected to the water holding capacity and viscosity. The tested pasta products showed significant variations in dietary fiber level. Pasta made with refined flours, both CW and SW, proved to have 3 to 4 times lower total dietary fiber level than did the wholegrain flours. There were no significant differences between WGW and WGS pasta, and the TDF values were 8.75 and 9.02%, respectively. This confirms the presence of fibrous compounds in the pericarp and aleurone layers which are removed during flour refinement. Escarnot et al. (2012) reported TDF white wheat flour 12

values of 2.52%, while that for wholegrain wheat flour was from 12.5 to 15.4%. For spelt varieties, Bonafaccia et al., (2000) and Ranhotra et al. (1996) reported TDF amounts in the range from 2.65% for white flour and from 8.7 to 13.2% for wholegrain spelt. In the work of these authors and in our work, the ratio of soluble fiber to insoluble fractions (SDF/IDF) in the tested pasta was the lowest for WGS pasta, which may suggest the lowest ability of spelt to form soluble fractions of fiber in the proposed extrusion conditions during pasta processing. These products also revealed the lowest gelatinization degree (Table 1) because of the lower amount of total carbohydrates in raw materials and the highest amount of fiber in flour, which limited the processability of wholegrain spelt. Bonafaccia et al. (2000) uncovered a less amount of total starch, but also demonstrated that more resistant starch is formed in bread from wholegrain spelt and white spelt wheat, as compared to bread made from white wheat flour. The same authors showed TDF level in spaghetti made with durum wheat at the level of 2.7%, purified spelt flour at 2.3% and wholegrain spelt flour at 7.5%. A redistribution of the proportion of IDF to SDF seems to have occurred in all the extruded samples, with the effect being less distinct in wholegrain flour. For regular barley flour, an increase in both IDF and SDF contribute to increased TDF content (Vasanthan et al., 2002). At mild or moderate conditions, extrusion-cooking does not significantly change dietary fiber content, but makes some fiber components soluble. At more severe conditions, dietary fiber content tends to increase, mainly owing to rising SDF and enzyme-resistant starch fractions (Singh et al., 2007). The proposed extrusion-cooking conditions of pasta processing produced from 68 up to 91% of gelatinized starch. The highest degree of gelatinization was observed for CW pasta. Herein, more than 90% of starch was gelatinized, so the products are precooked during the processing, hence, a short preparation time without conventional cooking was reported. Similar results for the degree of gelatinization were reported by Wójtowicz & Mościcki (2009) for common wheat pasta processed by means of the extrusion-cooking technique under various conditions. For WGS products, the 13

gelatinization degree was the lowest because of the lower amount of total carbohydrates in the raw material and the highest amount of fiber, which limited the processability of wholegrain spelt. 3.2. Amino acids composition The evaluation of nutritive value of wheat protein in the tested pasta was expressed by the proportion of essential amino acids present in the test material (Table 2). The proportion of protein in grain dry matter was evaluated first. As regards food quality, not only is a high proportion of nutritional components important, but so too is their nutritive quality (WHO, 2015). Wheat proteins are known to contain less of some amino acids that are considered essential for diet, especially lysine, but they are rich in glutamine and proline, i.e. functional amino acids important in dough formation. In the presented study, lysine content was the lowest for SW pasta (2.5 mg/g of protein) and the highest for WGS pasta (about 4 mg/g of protein). The differences between CW and WGW pasta were much lower. The total sulphur amino acids level was the lowest for CW pasta (2.3 mg/g of proteins), while slightly higher values, but insignificant differences, were observed for WGW and refined SW pasta. The highest total sulphur amino acids level at 2.93 mg/g of protein was reported in WGS flour pasta. Methionine aids the production of sulphur, which is needed for normal metabolism and is also essential for the synthesis of haemoglobin and the glutathione that counters free radical damage. In this study (Table 2), methionine content was the highest in WGS pasta (1.98 mg/g of proteins) and the lowest in CW pasta (1.58 mg/g of proteins). Leucine is one of three essential amino acids that increase muscle mass and regulate blood sugar, supply the body with energy and have an impact on brain functions (Wu, 2010). In precooked extruded pasta, a higher leucine level was measured in WGW and WGS pasta than in CW and SW pasta. Isoleucine is important for the regulation of blood sugar, so precooked pasta made with wholegrain flours can be recommended as a better source of isoleucine than pasta made with refined wheat and spelt flours. The total content of sulphur amino acids (TSAA) was the lowest for CW flour (2.32 mg/g of protein). Somewhat higher but 14

insignificantly different values were observed for WGW and SW pasta, while the highest TSAA (2.93 mg/g of proteins) was found in WGS pasta. The quantity of lysine varied from 1.96 to 3.96 g/100 g protein in eight cultivars of spelt studied by Ranhotra et al. (1996). Table 2 presents the results of amino acid composition analysis with the selection of total essential (TEAA) and non-essential (TNEAA) amino acids. Essential amino acids, also called ‘limiting amino acids’, cannot be bodily produced and must be taken in with food. TEAA are important neurotransmitters and facilitate the communication of the brain with the nerve cells in the body (Wu, 2010). In this study, TEAA ranged from 31.4 to 33.0% of total amino acids. Insignificant differences were reported for CW and SW, with the values of 34.37 and 35.83 mg/g of protein, respectively, but the amount of TEAA compared to total amino acids was the lowest for WGW and WGS flour, with the level of 31.9 and 31.4% of total amino acids, respectively. Escarnot et al. (2012) reported similar TEAA in wheat and spelt, herein ranging from 34 to 40% of total amino acids. The highest level of TEAA in the precooked pasta was reported for WGS – at 42.86 mg/g of protein. Matuz, Bartok, Morocz-Salamon & Bona (2000) observed that whole-meal and spelt flour had a higher content of most amino acids than some recently developed common wheat varieties. As regards the total proportion of amino acids in grain dry matter, some emmer wheat landraces are considered more prospective. This is due to high crude protein content in the grain. Herein, the nutritive value of protein is the same, but the proportion of essential amino acids is higher (by 16-26%). Total nonessential amino acids (TNEAA) in precooked pasta varied significantly depending on the flour type used in the experiments (Table 2). The highest value of TNEAA was measured for WGS pasta – 86.97 mg/g of protein, next to the highest level of arginine (6.30 mg/g), aspartic acid (6.92 mg/g), glycine and alanine (both 5.40 mg/g). Glutamic acid and proline content were also the highest, yet some insignificant differences were observed compared with the results of WGW and SW pasta. The level of serine was the highest in pasta processed from WGW flour, while somewhat lower values 15

were obtained for WGS pasta (6.44 and 6.39 mg/g of protein, respectively). The lowest values of arginine, aspartic acid and glycine were noted for SW pasta. Glutamic acid was found to be the predominant TNEAA, with the values ranging from 33.37 mg/ g of proteins for CW pasta, and to 39.80 mg/g of proteins for WGS pasta. In wheat and spelt pasta, a high amount of proline (13.5616.76 g/g of proteins), aspartic acid (4.98-6.92 g/g of proteins) and serine (5.52-6.44 g/g of proteins) was also reported. The highest amount of non-essential amino acids was measured in WGS pasta, followed by WGW products; significantly lower values were observed for CW and SW precooked pasta. In a previous study, Abdel-Aal & Hucl (2002) and Marconi, Carcea, Schiavone & Cubadda (2002) reported the applicability of spelt flour to produce a pasta with a high nutritional value. Accordingly, mild extrusion conditions (high moisture content, low residence time, low temperature) favor a higher retention of amino acids, high protein and starch digestibility, increased soluble dietary fiber, decreased lipid oxidation, higher retention of vitamins and a higher absorption of minerals (Singh et al., 2007).

3.3. Phenolic compounds and antioxidant activity of pasta Phenolic compounds detected in pasta products also showed the better nutritional characteristics of wholegrain products compared to CW and SW pasta. The highest amount of protocatechuic acid, vanilic acid, trans-coumaric acid, trans and cis-ferulic acid was measured in WGS pasta. Still, WGW products also showed a significant amount of phenolic acids (Table 2). SW precooked pasta evidenced the lowest quantity of phenolic compounds, as compared to the other tested pasta products. Yet, significant differences were seen between the tested samples in all identified phenolic acids. Syringic acid was detected only in wholegrain products. For SW pasta, the levels of protocatechuic acid and trans- and cis-coumaric acids were below the quantification limit of the HPLC method because these phenolic components are mainly located in the outer layer of seeds, and this layer is 16

removed during the processing for white flour. Gawlik-Dziki, Świeca & Dziki (2012) found the amount of total phenolics ranged from 506.6 to 1257.4 μg/g in six varieties of spelt, and prevailing phenolic acids were ferulic and sinapinic acids. In whole-wheat spaghetti, Hirawan, Ser, Arntfield, & Beta (2010) found significantly higher levels of total phenolic content, especially ferulic acid, than in regular wheat spaghetti. Additionally, they reported that total phenolics content remained at 48–78% of the original content in both regular and whole-wheat spaghetti after cooking. Exemplary LC-MSMRM chromatograms and the mass spectra of analyzed phenolic acids (obtained in negative ion mode) are presented in Supplementary Figures 1-7. The radical scavenging activity of precooked pasta against DPPH measured with the spectrophotometric method is presented in Figure 1A. WGS precooked pasta showed the highest radical scavenging activity in the spectrophotometric analysis against DPPH. The activity was around 55% after 30 minutes of testing. WGW pasta also demonstrated a high ability for radicals scavenging (around 40%). The shorter time of activity, the better antioxidant activity of pasta, so, wholegrain products demonstrated superiority, in that greater antioxidant potential was indicated just after 5 minutes of tests and because, as indicated, they are a good source of active components. Precooked pasta made with CW and SW flours, in contrast, have some, but limited, activity. In the TLC-DPPH test, the free radical activity is proportional to the intensity of radical color changes. Antioxidant potentials were calculated as the total of the areas under peaks. As a reference point, the surface area of the standard solution of rutin was taken and assigned an activity of 1.0 (Supplementary Figure 8). The antioxidant activity of precooked pasta products is shown in Figure 1B. The results of the radical scavenging activity and antioxidant activity using spectrophotometry and thin layer chromatography for the tested extracts were very similar. WGS pasta showed the greatest activity in the chromatographic method, having a value of 0.73, against 1.0 set for rutin, while a lower activity, ranging from 0.30 to 0.45, was observed for CW and WGW pasta products. Phenolic compounds are 17

found in grains to be bonded, most often by ester and glycosidic bonds, with the polysaccharide cell wall of the seed bran, thus forming so-called “antioxidant cellular fiber” (Acosta-Estrada, GutiérrezUribe & Serna-Saldívar, 2014). Given this, it seems obvious that the highest antioxidant properties, both in the TLC-DPPH test and in the spectrophotometric method, were seen in the two wholegrain pastas. Moreover, the outer layers of spelt wheat abound in polyphenolic compounds as opposed to the bran of ordinary wheat (Gawlik-Dziki et al., 2012). This translates into the test wholegrain pasta holding higher antioxidant properties, hence, WGS having higher DPPH free radical scavenging activity when compared to WGW pasta. Therefore, there should be the minimum processing of grain before and during the manufacture of the product so as to achieve maximum health benefits. The results obtained in the discussed tests using DPPH correspond very well with the results of the chromatographic analysis performed for phenolic acids. The main antioxidants of grains are phenolic acid derivatives. Flavonoids and polyphenols other than phenolic acids occur in grain in very small quantities. Gull et al. (2018) found that the content of phenolic acids and the antioxidant activity of produced pasta based on 64% composite flour containing durum semolina and carrot pomace and 20% of finger millet was significantly higher in the control semolina pasta. Moreover, Gawlik-Dziki et al. (2012) observed a high antioxidant potential in all tested spelt varieties.

3.4. Physical properties of precooked pasta The physical characteristics and texture profile of pasta are presented in Table 3. Low expansion ER of precooked products is needed because of its short preparation time. In the products we tested, the expansion of precooked pasta did not exceed 1.5 and was lower for pasta processed with wholegrain flours. In the case of instant noodles, hot water hydration is needed, and cooking is not required. A small diameter (smaller cross-section) is, hence, preferred as it promises a shorter hydration time (Wang, Bhirud, Sosulski, & Tyler, 1999; Wójtowicz & Mościcki, 2009). In our study, the minimum 18

time (OCT) needed to prepare extruded pasta for consumption was measured without cooking. Hot water hydration time to achieve the ready-to-eat form varied from 5 minutes for precooked pasta from purified wheat flour, up to 7 minutes to get the right consistency both of WGW and WGS pasta. Still, the products had a proper shape even after 10 to 12 minutes of prolonged rehydration. A longer hydration time disrupted the structure of mainly wholegrain pasta. There were no significant differences between the pasta samples. Similar observations were made for a variety of extruded precooked pasta (Bouasla et al., 2016, 2017; Wójtowicz & Mościcki, 2014). The absorption and retention capacity of hot water during the hydration of instant pasta products is the parameter indicating the necessary amount of liquid required for the full hydration and for proper consistency of products prepared for consumption. Insufficient amount of water relative to pasta weight can affect its hardness, and bring about low hydration and a floury taste. The values of water holding capacity (WHC) in the tested products were highly correlated with protein content in the raw materials used in the study. The WHC of pasta hydrated in hot water ranged from 120.58 to 243.55% and was higher for wholegrain pastas. These values are in accordance with Martinez et al. (2007), who determined a water absorption of 256-267% for commercial semolina pasta; Wang et al. (1999), who measured water absorption from 147 to 174% in extruded pasta with pea flour; Bouasla et al. (2016) who reported water absorption after hydration of 200 to 360% in precooked pasta, depending on raw materials formulation, enrichment and extrusion parameters. Cooking loss (CL) is a commonly used predictor of overall spaghetti cooking performance by both consumers and the industry. In our study, the number of components passing into the solution after 5 minutes of hydration did not exceed 9%, which indicates good binding of starch and protein components in the pasta. The results, however, showed CL values that ranged from 7.25 and 8.42% for CW and SW pasta, respectively, due to a high degree of starch gelatinization in pasta. The significant increase in CL observed for WGW and WGS pasta could be due to a disruption of the 19

protein-starch matrix and the uneven distribution of water within the pasta matrix due to the competitive hydration tendency of fiber. A higher number of components leached from pasta into hot water is typical of pasta products made with wholegrain flours. The maximum number of components leached from starch during the cooking of noodles should not, however, exceed 10% (Kruger et al., 1996). The application of extrusion-cooking conditions in the given range may result in the initial formation of the matrix and the ability of pasta to keep gelatinized starch and other components together, which limits the amount of components loss during hot water hydration. According to the literature, the quality of pasta with the losses of <12% can be considered acceptable (Chillo, Laverse, Falcone, Protopapa & Del Nobile, 2008; Martinez et al., 2007; Sozer et al., 2007; Wang et al., 1999). Important features of intensity of extrusion-cooking treatment are the WAI and WSI indices. These are often used to determine internal changes occurring in the material, especially starch transformation (Mercier et al., 1998). The results of the WAI and WSI are reported in Table 3. Extrusion-cooking provides the thermal conditions necessary to trigger starch gelatinization for all precooked pasta, as well as allowing major degradation leading to high water solubility. The higher solubility of products obtained by extrusion-cooking can be explained by the action of shear forces that disrupt the molecular network of the starch-protein matrix (Mercier et al., 1998). In our study, the WSI was low due to a high degree of starch gelatinization, good pasting characteristics and compact and dense internal structure - as confirmed by microstructure images (Figure 2). Oikonomou and Krokida (2012) showed that experimental WAI values ranged from 0.3 to 12.8 g/g, whereas WSI values varied from 2.7 to 73.2% for the extruded food products. They concluded that the WAI and WSI increase when the extrusion variables rise in several types of raw materials, but the results were strongly affected by the processing conditions and the raw materials used.

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3.5. Texture characteristics of precooked pasta Texture properties of food products play an important role in quality and consumer acceptability. WGW pasta had the lowest hardness value (6.71 N) in a cutting test, as well as a low expansion index and a lower gelatinization when compared with CW products (Table 3). In contrast, the hardness of both SW and WGS pasta was higher than observed in common wheat products due to higher protein content in the raw materials. The hardness of precooked pasta was also found strongly linked to the processing conditions, such as initial dough moisture content and screw speed during extrusion (Wójtowicz & Mościcki, 2009), in addition to the composition of raw materials (Bouasla et al., 2016, 2017; Wójtowicz & Mościcki, 2014). Firmness of hydrated precooked pasta after 5 minutes of hydration differs depending on the raw material used (Table 3). The lowest firmness was seen in WGW pasta, which exhibited the lowest expansion and the lowest hardness of dry products. Somewhat improved texture was observed in pasta made with WGS flour, while firmer texture was noted for SW pasta, probably due to a higher protein content and stronger starch-protein matrix formation during the extrusion-cooking process. Adhesiveness of WGW pasta was also much higher than in other tested products and corresponded to the low firmness of hydrated products (Table 3). Low adhesiveness was observed for CW and SW pasta due to the low amount of fiber in the composition. Low adhesiveness is very important for pasta texture, so these products proved superior in quality. Firmer consistency of pasta made with refined flours limited product adhesiveness compared to wholegrain products. A higher amount of bran lowered the total starch content and made the transformation of starch into a homogenous starch-protein matrix more difficult. Additionally, the decrease in firmness shows association with the reduced starch gelatinization in the tested pasta. Extra fiber appears to interfere with the structure of pasta, possibly disrupting the continuity of the protein-starch matrix, thus lowering the resulting pasta’s firmness compared to the control. This is in accordance with the results of Edwards, Biliarderis & Dexter (1995). They reported that the 21

strengthening of pasta with pea fiber altered its structure and resulted in a moderate reduction in firmness and an increase in cooking losses. The inclusion of soluble non-starch polysaccharides also raised the temperature of gelatinization, as confirmed in our tests, too.

3.6. Pasting properties of precooked pasta PT values observed for extrusion-cooked pasta (54-70°C) were in a typical range known for extruded products. The lowest PT and onset of gelatinization were recorded for WGW pasta products (Table 3). Indeed, almost all components were already gelatinized. Stuknytė et al. (2014) reported the pasting temperature of 64.5°C for uncooked and 67.8°C for cooked durum wheat spaghetti. Starchlipid and starch-protein complexes, along with other wholegrain flour components, assure the integrity of starch granules during heating, and, therefore, higher pasting temperatures were recorded for CW, SW and WGS pasta products. Edwards et al. (1995) suggested that inclusion of soluble nonstarch polysaccharides leads to an increase in gelatinization temperature. This is partly due to the soluble fiber competing with starch for water absorption, thus limiting starch swelling and gelatinization. In our work, however, pasting curves showed a characteristic peak during the heating stage (Supplementary Figure 9), which indicates that not all starch was gelatinized during pasta extrusion-cooking. Maximum viscosity (MV) during heating, high BD and SB was reported for pasta made with CW flour, which can be attributed to the pasta products holding high carbohydrate content and high water absorption. The BD value is the difference between the PV and HPV and shows the degree of starch disintegration during cooking. The pasta processed with CW and WGW flour exhibited the top BD values, which may indicate lower cooking stability than spelt pasta. SB is the difference between CPV and PV and indicates the retrogradational tendency of amylose. Our work saw that the lowest SB value was recorded for WGW pasta. We believe that changes in the rheological properties are behind the diverse handling properties of the dough during processing. 22

Marconi et al. (2002) reported that Triticum spelta L. wheat has rheological and technological properties similar to those of durum wheat. Hence, it can, therefore, be used to make pasta with good nutritional and sensory properties.

3.7. Color of pasta products The assessment of color as a method of testing the visual characteristics of food products is mostly done by means of the CIE-Lab color scale. This helps to appraise brightness and color balance. Results showed similar L* values for dry and hydrated pasta made with CW and SW flour, while pasta made with wholegrain flours had a darker color, both in dry and hydrated products (Table 4). Therein, dry WGW pasta showed higher values of the red component a*, which was associated with the presence of dark-colored bran fractions in the wholegrain flour. Wholegrain pasta also showed a slight red tint and a higher yellowness than that made with purified flours. Still, after hydration, it was much brighter and lost its characteristic color, the redness being less intensive, but the differences were negligible. When measuring the observed intensity of dry pasta yellow hue (b*), hydration reduced the value of the discriminant by about 30%, resulting in a lower intensity of the yellow color in hydrated pasta. The differences between pasta samples made from CW and SW flour before and after hot water hydration were insignificant, so these products have a similar color profile. For common wheat flour pasta-like products, Wójtowicz & Mościcki (2011) reported that the L* values reached 83.8 for dry and 87.8 for hydrated pasta. The addition of wheat bran lowered the L* values for both dry (from 71.6 to 56.1) and hydrated (from 81.3 to 68.9) pasta products. Chillo et al. (2008) saw similar tendencies. The decrease in yellowness of cooked pasta could be related to the degradation and dissolution of carotenoid pigment by hot water, as already observed in legumes or shrimp-fortified pasta (Bouasla et al., 2017; Desai, Brennan, & Brennan, 2018). Marconi et al. (1999) tested the suitability of spelt as purified and wholegrain flours for the processing of spaghetti by way 23

of the conventional pressing method for 1.7 mm diameter pasta. They found that color values varied in the range of 79.9-83.1 for lightness, 0.4-1.9 for a* and 15.5-18.1 for b* color parameter depending on the variety of spelt.

3.8. Microstructure of pasta products Microscopic pictures taken with a scanning microscope showed in detail, the external and internal structure of the tested pasta (Figure 2). In this regard, CW and SW pasta had a highly compacted and homogenous internal structure where starch granules appear to be entrapped within a protein-starch matrix (Figure 2A and 2C, respectively). The surface of strands in such kinds of pasta was also aligned, smooth and indiscrete. This may explain not only the appearance (different from other types of pasta), but also the reduced cooking losses and the significantly altered textural characteristics. The most compact and dense structure was observed for CW pasta (Figure 2A). This confirms it having the highest degree of starch gelatinization (Table 1). Of note, Stuknytė et al. (2014) reported the presence of a partly gelatinized structure if low-temperature drying was applied in durum pasta. When analyzing the microscopic pictures of wholegrain pasta products, a rough and uneven structure of the surface is clearly visible both in WGW and WGS pasta (Figure 2B and 2D, respectively). The internal composition of wholegrain products was less compacted, with visible particles of bran (Figure 2B, magnification x600 and 2000) and aleurone layer components, with untreated starch granules embedded in the fibrous structure of the external parts of the spelt caryopsis (Figure 2D, magnification x600 and 2000). Additionally, some empty spaces are seen in these products, especially next to ungelatinized particles (Figure 2D, magnification x600 and 2000). This can explain the low WAI of WGS pasta. Moreover, the high number of ungelatinized particles in wholegrain flour pasta may be the reason for its heightened ability to absorb and keep water, as demonstrated by the WHC results. Wójtowicz & Mościcki (2011) observed a similar microscopic structure in extruded 24

pasta enriched with wheat bran. In addition, Bouasla et al. (2016) reported the presence of untreated particles of yellow pea added to rice-based precooked pasta. However, during the extrusion-cooking of rice pasta enriched with legume flours, Bouasla et al. (2017) found a compact and homogenous starch-protein matrix which stabilized the uniform (integral) structure of pasta and minimized cooking loss obtained during hydration in hot water.

3.9. Sensory evaluation of precooked pasta products The sensory properties of precooked pasta are presented in Table 4. The sensory characteristics of pasta, such as color, shape, and appearance as rated by consumers often solely influence the purchasing decision. Instant noodles should have a good visual quality, but also an appropriate texture and taste after reconstitution (Kruger et al., 1996). Higher notes for shape, appearance and taste, in addition to low stickiness, were registered for CW and SW pasta. In addition, items made of WGS flour revealed significantly higher hydrated pasta organoleptic properties than did WGW pasta products. Using CW flour for pasta production can have multiple health and production benefits; however, lower sensory attributes and cooking quality of such products results in a preference for durum semolina. The application of the extrusion-cooking process, therefore, affords a great opportunity to use common wheat as a raw material for producing instant pasta with acceptable quality without (Wójtowicz & Mościcki, 2009) or with various additives (Wójtowicz & Mościcki, 2011, 2014), as well as for the processing of gluten-free pasta products (Bouasla et al., 2016, 2017).

4. Conclusions Application of the extrusion-cooking technique resulted in creating pasta products with good nutritional and sensory profiles, especially when wholegrain wheat and wholegrain spelt were used as raw materials. Wholegrain wheat and wholegrain spelt precooked pasta were characterized by a 25

higher protein, ash and fiber content than did refined flour pasta. Extrusion-cooking in the presented conditions allowed producing precooked pasta with a short preparation time and attractive texture after hot water hydration. Physiochemical properties, however, varied depending on the flour type. Microstructure analyses confirmed less compact starch-protein matrix with visible bran particles inside wholegrain wheat and spelt pasta products. Over all, wholegrain flours, especially spelt, may successfully be used to create nutritionally valuable precooked pasta products of acceptable quality with high dietary fiber content and high biologically active compound content, e.g. especially with regard to the essential amino acids and phenolic acids.

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Figure captions

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Figure 1. Antioxidant properties of precooked pasta from various types of flours: A) radical scavenging activity, B) antioxidant activity of precooked pasta against rutin (thin layer chromatography). Figure 2. Microstructure of dry precooked pasta: A) CW, B) WGW, C) SW, D) WGS, with various magnifications (x100 for surface, x125, 600, 2000 for cross-section). Supplementary figure 1. Extracted LC-MS-MRM chromatograms of phenolic acids detected in negative ion mode in WGW pasta. MRM transition are given in brackets: 1 - protocatechuic (m/z 152.9 > 107.8); 2 – 4-hydroxy-benzoic (m/z 136.9 > 93); 3 – vanillic acid (m/z 166.8 > 107.9); 4 syringic (m/z 196.9 > 122.8); 5 - trans-p-coumaric (m/z 162.8 > 119); 6 - cis-p-coumaric (m/z 162.8 > 119); 7 – trans-ferulic (m/z 192.8 > 133.9); 7 – cis-ferulic (m/z 192.8 > 133.9). The isomers were distinguished based on their retention times after careful comparison with the isomers found in standards. Supplementary figure 2. Mass spectrum of protocatechuic acid obtained in negative ion mode. Supplementary figure 3. Mass spectrum of 4-hydroxybenzoic acid obtained in negative ion mode. Supplementary figure 4. Mass spectrum of vanillic acid obtained in negative ion mode. Supplementary figure 5. Mass spectrum of syringic acid obtained in negative ion mode. Supplementary figure 6. Mass spectrum of p-coumaric acid obtained in negative ion mode. Supplementary figure 7. Mass spectrum of ferulic acid obtained in negative ion mode. Supplementary figure 8. Results of TLC- DPPH test Mobile phase: acetonitrile, water, chloroform, formic acid (30:2:5:2, v/v/v/v): a) scan after 10 minutes, b) scan after 30 minutes. Supplementary figure 9. Pasting curve registered for various pasta types.

32

33

34

Table 1. The chemical composition of raw materials and dry pasta. Raw materials (producers’ data)

Flour type

Prote in (%)

CW

12.2a

F at ( %) 0.9a

Dry pasta

Carbohydrate

Fibe

Protei

s

r

n

(%)

(%)

(%)

70.9a

1.3a

11.35a

Fat

Ash

IDF

SDF

TDF

(%)

(%)

(%)

(%)

(%)

0.12a

0.85a

1.25a

0.44a

1.69a

±

±

±

±

±

0.01

0.05

0.02

0.02

0.06

14.34b

0.53

1.39a

c

b

b

6.05c

2.70c

8.75c

±

±

±

±

±

0.02

0.03

0.03

0.06

0.07

± 0.06

WG

13.7ab

W

2.1 b

65.5bc

4.0c

± 0.42

SW

14.8b

1.0a

67.8b

1.5a

13.23b

± 0.13

WGS

16.7c

1.9 b

63.9c

2.7b

15.52c

± 0.11

0.48 b

1.52b

2.08 b

1.13b

3.21 b

±

±

±

±

±

0.01

0.02

0.05

0.09

0.02

7.96

1.06a

d

b

0.52 b

1.71b

9.02c

±

±

±

±

±

0.02

0.02

0.12

0.03

0.03

SDF/ID F Index (-)

0.352b

0.445bc

35

90.73a

80.59 b

± 1.17

0.543c

80.47 b

± 0.77

0.133a

insoluble dietary fiber, SDF – soluble dietary fiber, TDF – total dietary fiber, GD – gelatinization degree different letters in columns indicate significant differences in means at α≤0.05

(%)

± 0.33

mean±SD, CW – common wheat, WGW – wholegrain wheat, SW – white spelt, WGS – wholegrain spelt, IDF –

a-c

GD

67.96c

± 0.95

Table 2. Amino acids and phenolic acids composition of dry precooked pasta from different flour types. Flour type Composition CW

WGW

SW

WGS

Amino acids (mg/g*) Isoleucine

3.44 ± 0.03

3.98 ± 0.02

3.78 ± 0.02

4.27 ± 0.05

Leucine

7.42 ± 0.03

8.62 ± 0.03

8.18 ± 0.08

9.20 ± 0.10

Lysine

2.87 ± 0.03

3.17 ± 0.03

2.52 ± 0.02

3.89 ± 0.04

Cystine

0.74 ± 0.03

0.89 ± 0.02

0.91 ± 0.05

0.95 ± 0.02

Methionine

1.58 ± 0.08

1.80 ± 0.04

1.72 ± 0.03

1.98 ± 0.02

Total sulphur amino acids

2.32a ± 0.11

2.69ab ± 0.06

2.63ab ± 0.04

2.93b ± 0.04

Tyrosine

2.75 ± 0.04

2.81 ± 0.03

2.59 ± 0.09

3.41 ± 0.02

Phenylalanine

5.25 ± 0.03

6.28 ± 0.03

5.81 ± 0.10

6.50 ± 0.15

Total aromatic amino acids

8.00a ± 0.01

9.09ab ± 0.04

8.40a ± 0.15

9.91b ± 0.04

Threonine

3.26 ± 0.04

3.64 ± 0.05

3.00 ± 0.17

3.77 ± 0.06

Valine

4.53 ± 0.04

5.02 ± 0.03

4.78 ± 0.09

5.74 ± 0.05

Histidine

2.53 ± 0.03

2.89 ± 0.02

2.54 ± 0.05

3.15 ± 0.04

36

Total essential amino acids

34.37a ± 0.28

39.10b ± 0.19

35.83a ± 0.32

42.86c ± 0.22

Arginine

4.80 ± 0.15

5.40 ± 0.25

4.39 ± 0.04

6.30 ± 0.20

Aspartic acid

5.40 ± 0.2

5.98 ± 0.05

4.98 ± 0.02

6.92 ± 0.03

Glutamic acid

33.37 ± 0.06

39.61 ± 0.12

38.57 ± 0.45

39.80 ± 0.25

Serine

5.52 ± 0.03

6.44 ± 0.20

5.66 ± 0.06

6.39 ± 0.09

Proline

13.56 ± 0.05

16.36 ± 0.09

16.46 ± 0.05

16.76 ± 0.06

Glycine

4.39 ± 0.04

4.95 ± 0.05

4.08 ± 0.05

5.40 ± 0.10

Alanine

3.27 ± 0.03

4.75 ± 0.06

3.97 ± 0.02

5.40 ± 0.15

Total non-essential amino acids

70.31a ± 0.46

83.49ab ± 0.81

78.11ab ± 0.64

86.97b ± 0.87

Total amino acids

104.68a ± 0.74

122.59b ± 0.99

113.94ab ± 0.96

129.83c ± 1.09

Phenolic acids (ng/g) protocatechuic

134.6a ± 0.78

221.7b ± 1.12

BQL

845.7c ± 1.55

4-OH-benzoic

208.5b ± 1.09

237.3bc ± 2.23

131.7a ± 0.89

284.4c ± 2.15

vanillic

798.8b ± 2.08

1867.6c ± 3.98

305.9a ± 0.96

2273.9d ± 4.86

siringic

BQL

99.6a ± 0.76

BQL

289.3b ± 0.44

trans–p-coumaric

41.6a ± 0.06

82.1b ± 1.24

BQL

107.5c ± 0.48

cis-p-coumaric

61.6a ± 0.66

97.3c ± 0.69

BQL

88.1b ± 1.12

trans-ferulic

204.3b ± 1.84

520.2c ± 0.89

55.1a ± 0.16

842.0d ± 3.86

37

cis-ferulic

1205.6b ± 6.84

3189.5c ± 9.77

441.1a ± 2.46

4279.6d ± 8.04

mean±SD, CW – common wheat, WGW – wholegrain wheat, SW – white spelt, WGS – wholegrain spelt, BQL – below quantification level *at

a-d

93% dry matter

different letters in rows show significant differences at α≤0.05

38

Table 3. Physical properties of precooked pasta made with various flour types.

H

Flour

ER

OCT

WHC

CL

WAI

WSI

Hardness

Firmness

Adhesiveness

PT

MV

type

(-)

(min)

(%)

(%)

(g/g)

(%)

(N)

(N)

(mJ)

(°C)

(mPas)

CW

1.45c

5.0a

191.03b

7.25a

5.96c

4.21a

15.62bc

112.2bc

188.72a

63.6b

316c

20

± 0.02

± 0.28

± 4.96

± 0.19

± 0.03

± 0.37

± 1.41

± 5.11

± 7.55

± 0.33

± 3.26

±

1.19a

6.0a

222.60bc

11.91c

3.44a

6.71c

6.71a

87.8a

285.95c

54.7a

201a

10

± 0.12

± 0.45

± 2.86

± 0.99

± 0.87

± 0.84

± 0.12

± 6.49

± 11.47

± 0.41

± 1.63

±

1.49c

7.0b

120.58a

8.42ab

4.12b

4.67ab

17.50c

130.6c

169.27a

68.8c

197a

14

± 0.03

± 0.39

± 8.23

± 0.35

± 0.03

± 0.64

± 0.67

± 8.04

± 7.94

± 0.70

± 2.05

±

1.38bc

6.5ab

243.55c

9.46b

3.07a

5.28b

13.45b

105.8b

235.83b

70.4c

228b

15

± 0.02

± 0.50

± 1.75

± 0.16

± 0.02

±0.07

± 0.81

± 4.60

± 6.17

± 0.43

± 2.16

±

WGW

SW

WGS

mean±SD, CW – common wheat, WGW – wholegrain wheat, SW – white spelt, WGS – wholegrain spelt, ER -= expansion ratio, OTC – optimal cooking time, WHC – water holding capacity, CL – cooking loss, WAI – water absorption index, WSI – water solubility index, PT - pasting temperature, MV - maximum viscosity, HPV - hot paste viscosity, CPV - cold paste viscosity, BD – breakdown, SB - setback a-c

different letters in columns show significant differences at α≤0.05

39

(m

Table 4. Color profile of dry, hydrated pasta and sensory characteristics of precooked hydrated pasta.

Color of raw flour

Color of dry pasta

Color of hydrated pasta

Flour type

CW

Appearanc

Tast

Stickines

r

e

e

e

s

7.5a

7.5a

7.5a

7.5a

7.5a

±

±

±

0.82

0.58

0.49

5.5b

5.5b

±

±

±

1.89

1.09

0.81

7.5a

6.0ab

±

±

±

0.83

0.49

0.79

6.0ab

6.0ab

±

±

±

0.85

0.73

0.51

b*

L*

a*

b*

L*

a*

b*

92.2

-

10.1

86.7

-

11.9

90.9

-

10.5

c

1.4a

a

c

2.3b

a

c

1.5a

a

±

±

±

±

0.34

0.60

0.99

1.18

24.6

64.5

31.1

76.5

b

b

c

b

±

±

±

±

1.29

1.42

1.20

1.43

WG

78.3

W

b

± 1.30

± 0.6 7

2.1b

± 0.4 6

± 0.4 7

2.7c

± 0.3 3

± 0.4 1

2.3b

± 0.4 3

27.8 b

91.1

-

11.7

84.2

-

16.3

87.7

-

12.2

c

1.1a

a

c

4.1a

b

c

1.1a

a

±

±

±

±

0.39

0.63

0.29

0.98

27.6

54.8

29.7

67.4

b

a

c

a

±

±

±

±

1.14

1.08

0.80

1.14

± 0.68

WGS

Shap

a*

0.55

SW

Colo

L*

±

72.4 a

± 1.65

± 0.2 7

4.0c

± 0.8 5

Sensory profile of hydrated pasta

± 0.5 1

5.2d

± 0.3 5

± 0.2 8

3.2c

± 0.1 4

30.4 c

±0.67

4.0b

± 0.86

7.5a

± 0.67

6.0ab

± 0.86

± 0.81

5.0b

± 1.03

8.0a

± 0.69

7.5a

± 0.57

± 0.74

3.0c

± 0.65

7.5a

± 0.58

5.0b

± 0.97

mean±SD, CW – common wheat, WGW – wholegrain wheat, SW – white spelt, WGS – wholegrain spelt, L* luminosity, a* (+)redness, (-)greenness, b* (+)yellowness, (-) blueness.

40

a-c

different letters in columns show significant differences at α≤0.05

41

Highlights: New types of precooked wheat and spelt pasta products have been developed Extrusion-cooking apply for treatment of wheat and spelt pasta allows to achieve instant products Wholegrain pasta showed better nutritional composition and greater antioxidant potential Pasta showed high gelatinization degree, compact structure and attractive quality.

42