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ProEnvironment

ProEnvironment 11 (2018) 223 - 227

Original Article

Dyeing Potential of Linen Fabric with Flower Extracts

CRIŞAN Ioana, Roxana VIDICAN*, Adriana MOREA, Ştefania SIMEA

Faculty of Agriculture, University of Agricultural Sciences and Veterinary Medicine Cluj-Napoca, 3-5 Calea Mănăştur, 400372 Cluj-Napoca, Romania

Received 6 December 2018; received and revised form 11 December 2018; accepted 20 December 2018 Available online 30 December 2018

Abstract

Iris flowers have been used for pigments in Europe at least since Middle Ages. Natural coloring agents have many potential uses today and represent safer alternatives to synthetic ones which are common sensitizers posing concern especially for allergy-prone people. In this study, aqueous extract from flowers of Iris pallida and four Iris germanica were tested on natural linen fabric and resulting colors assessed with RHS chart. Most intense colors were obtained from Iris germanica ‘Black Dragon’, ranging from purple in case of simple flower extract to blue when alum was added. Red flowers produced also a shade from spectrum purple-blue because apparent red is determined by delphinidin with its associated co-pigments having high capacity to bound to fibers and carotenoids that wash off in absence of mordants. Large flowers with high pigment concentration of many current Iris germanica cultivars imply increased efficiency for obtaining valuable coloring agents, with significant potential for eco-friendly textiles.

Keywords: pigments, anthocyanins, tepals, textile, paper chromatography, flax fibers.

1. Introduction Because common sensitizers from textiles are disperse blue 106 and 124 [8], natural alternatives for Iris spp. present high potential for providing pigments from blue-purple spectrum could present coloring agents for textile, cosmetic and food high interest. Iris flowers have been used for their industry or serving as ink additive [6, 10, 17, 13]. pigments for many centuries in Europe. Medieval It is known today that use of natural pigments manuscripts mention the use of purple flowers from provides a safer alternative to synthetic ones which of Iris for obtaining both blue and green are responsible for allergies as well as for ecologic colors [7]. hazards following release into environment [16]. By the end of Middle Ages was perfected the Allergens from textiles used for clothing that method for obtaining iris green that was more stable may lead to contact dermatitis can be represented than green from Crocus used before. Thus, during either by dyes used to color the fabrics or by residues XIV century iris green became a main pigment used such as finishing substances that provide wrinkle- by manuscript illuminators [4]. It was obtained by resistance, shrink-proof or easy washing reaction of purple flower extract with an aluminum characteristics of final product, besides several other hydroxide base, and it is believed that Iris germanica possible additive traces. was the source of pigments. In connection with the Less often fibers themselves are responsible obtaining of this color is often mentioned the for allergies. “pezzette” method [7]. Some authors relate that medieval artists used a piece of cloth soaked in iris flower juice and placed in a shell with egg yolk for * Corresponding author. painting [18]. As further evidence comes the Tel: +40-264-596384 Fax: +40-264-593792 discovery of ‘iris juice’ mixed with rock alum in a e-mail: [email protected] group of fifteenth century Gospel books [7].

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Also, archaeological excavations in Gdansk more and delphinidin another one. As hydroxyl region revealed evidence from XII-XIII centuries groups are added the peak of absorbance spectrum graves, of Iris pseudacorus used for dyeing in yellow changes. Thus, delphinidin-based anthocyanins tend [12]. Several natural fibers can be dyed using blue- to be purple, violet or dark-blue while cyanidin-based violet Iris flowers [6]. Recent studies have re- anthocyanins tend to be blue, magenta or sometimes affirmed this potential with good results on cotton by red, while pelargonidin-based anthocyanins are using Iris sibirica [10], species previously mentioned almost always red or orange [15]. for potential at coloring silk [17]. The purpose of this study was to test the As coloring agents in cosmetic industry of potential of Iris germanica and Iris pallida flowers to current importance are the flowers of Iris dye natural -based fabrics. Besides being widely pseudacorus. Also, from of this species, a cultivated ornamental plants, Iris pallida and Iris coloring agent either brown or black-gray when iron- germanica have medicinal value as well [5] and based mordants are involved in the process, is could maximize profits for growers if flowers are recognized as effective in textile industry or at ink sold for pigment extraction. preparation [13]. The bluish pigment extracted from However, in case of taxa cultivated for orris, Iris flowers is widely known for the tint it gives to only Iris pallida might be suitable because Iris some beverages [20]. germanica var. florentina has very low concentration It is currently known that color of plants is of pigments in flowers. determined by the production, interaction and breakdown of three classes of substances: porphyrins 2. Material and Method (chlorophyll), carotenoids (carotene, lycopene and xanthophyll) and flavonoids (flavone, flavonol, Dyes were obtained from flowers of Iris anthocyanin) [1]. pallida Lam. and from four Iris germanica L. The most common and widely distributed type cultivars: ‘Black Dragon’, ‘Blue Rhythm’, ‘Sultan’s of floral pigments are the anthocyanins, with three Palace’ and ‘Lime Fizz’. Flowers were collected in major classes: pigments based on pelargonidin, full bloom (Fig. 1) and had lower tepal hairs as well cyanidin and delphinidin. These differ in the number as the stamens removed, then were stored in freezer of hydroxyl groups on beta ring of the molecule: (-18°C). Chromatograms on filter paper were pelargonidin having the fewest, cyanidin having one obtained using ethanol 98% as solvent.

Figure 1. Obtaining Iris flower dyes for testing on natural linen fabric (Original)

Steps followed for coloring the fabric were: acetic acid) for one hour, and after that were I. Obtaining the dyes washed with tap water - frozen tepals from each flower color were turned - a few pieces of linen were prepared by soaking into a paste using mortar and pestle (Fig. 1) in water with a few ammonium alum chips in - crushed tepals from each color were added in order to be used with black flower extract ratio of 25 grams to 100 ml water III. Dyeing - mixture of water and primary extract was heated - linen fabric pieces were introduced into dye in for 5-10 minutes separate recipients, covered with a plastic lid and - obtained dye was poured through a sieve. left for 1 day II. Preparation of fabric for coloring - linen fabric pieces were washed and dried - natural linen fabric pieces of 10 × 10 cm (Fig. 1), IV. Assessing colors obtained were placed in a solution of 20% vinegar (of 9% - color of each linen fabric piece was compared

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with RHS color chart to establish the intensity was obtained for Iris germanica ‘Black Dragon’, and shade obtained before and after drying. followed by Iris germanica ‘Sultan’s Palace’ (Fig. 2). Images of final colors obtained on linen fabric The fresh dye from red flowers of ‘Sultan’s Palace’ were taken using Canon scanner and fibers were had a purple color, but after linen was washed at the observed under Bresser microscope. end of dyeing, the yellowish tint washed away revealing a purple-blue color. This happened because 3. Results and Discussion red flowers of this are actually caused by a combination of carotenoids and blue-type The black, red, purple and blue flowers of Iris anthocyanin. germanica and Iris pallida lead to the obtaining of This was proven through chromatography on different colors from purple-blue spectrum. Color filter paper, when the carotenoids migrated fast intensity obtained can be directly linked to towards the solvent front, resulting clear separation anthocyanin concentration. Thus, darkest shade of the two main components of the primary flower following linen treatment with simple water extract extract.

Figure 2. Final linen colors obtained using dyes from Iris spp. flowers: a) control, b) Iris germanica ‘Lime Fizz’, c) Iris germanica ‘Blue Rhythm’, d) Iris pallida, e) Iris germanica ‘Sultan’s Palace’, f) Iris germanica ‘Black Dragon’; Colors from ‘Black Dragon’: simple extract, extract + ammonium alum (Original)

Iris germanica ‘Blue Rhythm’ presents Although extract was intense in color, after washing flowers that when observed seem more into the blue the treated linen, carotenoid pigments washed away spectrum than flowers of Iris pallida which seem to because they bounded less effectively to fibers (Fig. have a soft purple-violet hue. However, after drying 2), revealing the need of fixing agents. The colors the linen dyed with Iris pallida flower extract seemed observed immediately after treatment of dyed linen more into the blue spectrum than linen color resulted were slightly different from final color after drying from dying with Iris germanica ‘Blue Rhythm’. the fabric. At first most of them seemed in the purple Yellow dye color of Iris germanica ‘Lime Fizz’ lead spectrum but after drying some slightly changed and to the obtaining of a very light-yellow linen. presented a bluish tone (Tab. 1).

Table 1. Assessment for dyed linen based on RHS color chart Source of dyes Flower color Linen color Final linen color before drying after drying Iris germanica ‘Black Dragon’ + ammonium alum black 95B 96A Iris germanica ‘Black Dragon’ black N82A 83B Iris germanica ‘Sultan’s Palace’ red N82B 85A Iris pallida violet N82D 84D Iris germanica ‘Blue Rhythm’ blue N82C 85C Iris germanica ‘Lime Fizz’ yellow 3C 3D

The flowers of Iris germanica ‘Black Dragon’ previously in ammonium alum solution as well as appear black due to high anthocyanin concentration. addition of small quantity of alum into the dye, the Simple water extract of flowers produced a purple color shifted to blue (Fig. 2). Higher quantities of shade on linen while in the case of linen soaked alum would shift the spectrum to green.

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Similar with results of this study, previous First, current cultivars can present very high authors [10] identified as well slight changes in the concentration of pigments in their tepals while fresh color shade of cotton fabric dyed with Iris flowers are large. Both these aspects imply increased sibirica flower extract compared to final color, but in efficiency for obtaining pigments. their case, assessment was conducted at different Secondly, their cultivation is not difficult, and time intervals compared to this study when shade was can be achieved with little to no pesticide application, assessed before and after drying the fabric. In leading to the obtaining of safe coloring agents. addition, they identified in some cases differences in Simple reaction of anthocyanin flower extracts color related to soaking time. with alum can lead to color shift from purple shades According to previous researches, Iris to blue shades and even green, extending their germanica flower color was found to be determined potential use. by two distinct biochemical pathways: biosynthesis of anthocyanins and carotenoids. In cyanic Iris flowers the main pigments are of delphinidin-type References responsible for colors from spectrum blue and violet while in a-cyanic flowers carotenoid pigments [1] Alkema J., S. Seager, 1982, The chemical pigments of determine the occurrence of orange and yellow plants, Chem Supplement 59(3): 183-186. colors. True red is naturally missing due to deficiency in synthesis of pelargonidin and cyanidin-type [2] Asen S., N. Stewart, K. H. Norris, D. R. Massie, 1970, anthocyanins and lack of ability to accumulate A stable blue non-metallic co-pigment complex of delphanin and C-glycosylflavones in Prof. Blaauw Iris, lycopene in larger quantities. There were efforts Phytochemistry 9(3), 619-627. made for obtaining red flowers for Iris germanica by genetic transformation [11]. Exception within the [3] Ashtakala S. S., D. F. Forward, 1971, Pigmentation in genus is species Iris ensata which presents cyanidin iris hybrids: occurrence of flavonoid pigments in six and peonidin in some cultivated varieties [19] as well cultivars of Iris germanica, Canadian Journal of Botany as cyanidin in botanic species [9]. 49(11), 1975-1979. An important aspect related to pigmentation of Iris flowers is the presence of co-pigments. A study [4] Ball P., 2001, Bright Earth: art and the invention of involving several Iris germanica cultivars with color color, The University of Chicago Press, 101. similar to the ones used in present study (red, purple, [5] Crişan I., M. Cantor, 2016, New perspectives on blue, yellow) showed the common presence of medicinal properties and uses of Iris sp., Hop and delphanin and other flavonoid compounds with major Medicinal Plants 24(1-2), 24-36. co-pigment mangiferin occurring uniformly. The study suggested the existence of an in vivo pigment [6] Diamond D., 1990, The complete book of flowers, complex besides co-pigmentation [3]. North Atlantic Books, 119. The same major cyanic pigment (delphanin) was identified also in flowers of Iris hollandica ‘Prof. [7] Eastaugh N., V. Walsh, T. Chaplin, R. Siddall, 2004, Blaauw’ and associated with co-pigments: swertisin, Pigment compendium: a dictionary of historical pigments, vixetin, iso-orientin and swertiajaponin [2]. Elsevier, Oxford, 198. Similarly, Iris sibirica presents delphinidin as well as [8] Edwin K. J., 2001, Allergic contact dermatitis to textile malvidin [9], while delphinidin is also one of the dyes, Dermatology Online Journal 7(1), 9. most important flower pigments in Iris ensata [19]. Following results of this study it is evident that [9] Kaššák P., 2013, Screening of presence of the chosen Iris flowers can be used as coloring agents. As anthocyanin colorants in the Limniris group Irises, previous authors also concluded [14], further Preliminay communication - Vegetable Growing, researches should concentrate on identifying best Ornamental, Aromatic and Medicinal Plants, 48th natural mordants or fixing compounds to achieve Croatian & 8th International Symposium on Agriculture, long lasting colors of natural dyed fabrics, in order to Dubrovnik, http://sa.agr.hr/pdf/2013/sa2013_p0409.pdf. meet practical challenges for their larger scale application. [10] Kaššák P., M. Kuli, 2014, Dyeing potential of the Iris sibirica flowers, European Scientific Journal, Special Edition, 2, 372-380. 4. Conclusions [11] Lim T. K., 2016, Edible medicinal and non-medicinal Iris germanica flowers can provide an plants: volume 11 modified stems, roots and bulbs, important source of pigments for textile industry Springer International Publishing AG Switzerland, 3, 27- besides other possible uses for two main reasons. 40.

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[12] Macchia A., F. Prestileo, S. Cagno (eds.), 2016, Research 34, 384-399. YOCOCU 2014: Professionals’ experiences in cultural heritage conservation in America, Europe and Asia, [17] Stanišić M., M. Raspor, S. Ninković, S. Milošević, D. Cambridge Scholars Publishing, 107. Ćalić, B. Bohanec, M. Trifunović, M. Petrić, A. Subotić, S. Jevremović, 2015, Clonal fidelity of Iris sibirica plants [13] Pippen L., 2015, Laurie Pippen’s all natural colorants regenerated by somatic embryogenesis and organogenesis for cosmetic, culinary, and textile dyeing, Eiram in leaf-base culture - RAPD and flow cytometer analyses, Publishing, 86. South African Journal of Botany 96, 42-52.

[14] Prabhu K. H., A. K. Bhute, 2012, Plant based natural [18] Thompson D.V., 1956, The materials and techniques dyes and mordants: a review, J. Nat. Prod. Plant. of medieval painting, Dover Publications New York. Resources, 2(6), 649-664. [19] Yabuya T., M. Nakamura, A. Yamasaki, 1993, P- [15] Rausher D. M., 2008, Evolutionary transitions in coumaroyl glycosides of cyanidin and peonidin in the floral color, International Journal of Plant Scieces 169(1): flowers of Japanese garden iris, Iris ensata Thunb., 7–21. Euphytica 74(1), 47-50.

[16] Samanta A. K., A. Priti, 2009, Application of natural [20] ***, http://www.magellanbluegin.com. dyes on textiles, Indian Journal of Fibre & Textile

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