Optimization of extraction and dyeing conditions for traditional turmeric dye

Indian Journal of Traditional Knowledge Vol. 6(2), April 2007, pp. 270-278 Optimization of extraction and dyeing conditions for traditional turmeric dye Kiran Sachan & VP Kapoor* National Botanical Research Institute, Lucknow 226001, Uttar Pradesh Email: vpkapoor123@rediffmail.com Received 11 July 2005; revised 30 September 2005 Water soluble yellow dye was extracted from turmeric rhizomes (Curcuma longa L.), collected from Lucknow, Shillong and from local market, through aqueous/solvent extraction procedure using vacuum evaporator and spray drying of aqueous extract. Shillong sample was found to contain higher dye content (21.3-27.6%) followed by Lucknow sample (15.5-18.9%) and market sample (14.0-18.2%). Shillong sample was also been found to be rich in curcumin (6.6%) with compare to other samples (2.4-2.5%). Dyeing experiments were performed under different conditions of direct dyeing, pre-fixing treatment, mordanting treatment or/and simultaneous mordanting. 2% dyeing at 50-55 º C for 30-60 min was most appropriate to obtain good dyeing results. Numerous shades were obtained with good wash fastness properties. Emphasis has been laid to ensure ecofriendly dyeing profiles using soft or natural mordants and no salt of heavy metals were used. Keywords: Curcuma longa, Ecofriendly dye, Turmeric dye, Natural dye, Dyeing profile, Mordants IPC Int. Cl. 8 : D06P1/34, D06P1/36 Importance of natural dyes is more relevant world wide in the context of increasing environment consciousness. The non-toxic, biodegradable and ecofriendly properties make them exceedingly popular amongst nature loving and health awarded people. In spite of all, the present international consumption of natural dyes is around 10, 000 t, which is about 1% of the synthetic dye consumption. It is all due to the existing limitations and technical drawbacks of these dyes, which restrict their usage in textile dyeing. Some of these are colour yield, complexibility of dyeing process, limited shades, reproducible results, blending problems, and inadequate fastness properties. Lack of standardized profiles for extraction and textile dyeing are also major constraints. Indian craftsmen had monopoly on natural dyes before the advent of synthetic dyes but the craft of natural dyeing was very secretive amongst the particular communities. They did not disclose their trade secrets to any one except their family members. These techniques varied a lot depending upon the communities practicing in the different regions of India. They had no communication system and no documentation was made. In the era of synthetic dyes, natural dyeing became uncompetitive with regards to limited shades, less fastness properties and higher cost and thus neglected. It forced the *Corresponding author craftsmen to switch over to other professions thereby causing major set back to natural dyeing and the traditional knowledge became abdomened. Technical drawbacks and limitation of natural dyes can be solved through adequate scientific and R & D efforts 1. The amount of research efforts devoted to natural dyes is negligible 2. Most of the natural dyes are adjective in nature i.e. they require a suitable fixing agent under dyeing process. There is lot of possibilities to obtain numerous shades with good fastness properties by using suitable safe mordants. In view of above, adequate R & D efforts have been made at NBRI, Lucknow to tackle some of the impediments of natural dyes 3-8. Standardization of extraction and dyeing profiles of some of the prominent dyes has been developed under different conditions to achieve maximum yield and reproducible results. Incorporation of traditional knowledge with modern R & D expertise has been emphasized. The mordants used in past have been evaluated for their pre- and post- dyeing effects. The paper deals with standardization of extraction and dyeing profiles for traditionally known dye from the rhizomes of turmeric (Curcuma longa L.). Curcuma longa L, an important spice used as a cosmetic, and colouring agent has also been used in Indigenous System of Medicine 9-13. Turmeric is mainly valued for its principal colouring constituent curcumin, which imparts the yellow colour on textile fibers and food

SACHAN & KAPOOR: OPTIMIZATION OF TRADITIONAL TURMERIC DYE 271 items. Rhizome, the main source of curcumin also contains various ingredients like protein, fat, fibers, carbohydrates, essential oil, etc. Curcumin possesses various bioactive properties and is used in modern system of medicine 14. It is well recognized for its antiinflammatory, hepatoprotective, anticancer, metabolic disorders, antimicrobial, antiviral and antioxidant activities. Methodology Curcuma longa L. rhizome collected from Banthra Research Station of the Institute, Lucknow, Shillong (Meghalaya), and local market were observed for effect of habitat on the dye and curcumin yield (Figs 1 and 2). Different methodologies were adopted for extracting the dye from the different samples: Powdered raw material (100 gm) was soaked in water (800 ml) and kept overnight. The resulted coloured solution was subjected to warming at 90 C with continuous stirring for 5 hrs. The extracted solution was filtered followed by centrifugation at 6000 rpm to remove suspended impurities. The resulting centrifuged solution was concentrated under reduced pressure using Buchi Rotavapor at 50-60ºC. The material was kept in oven at 45ºC for 12 hrs. Market and Shillong samples were also subjected to aqueous extraction of dye using above mention conditions. The centrifuged solution obtained through aqueous extraction of Lucknow sample was subjected to spray drying. The following conditions yielded best result: Compressor air pressure 0.05 bar Air flow 32 m 3 /hr Pump flow 10-12 ml/h Inlet temperature 180 C Exhaust temperature 90 C Powdered raw material (100 gm) soaked in ethyl alcohol (600 ml) and solution was continuously vigorously stirred for 3 hrs and kept over night. The resulting solution was filtered and was concentrated under reduced pressure at 60ºC to obtained residual mass. The concentrated paste was dried in oven at 45 º C for 12 hrs and kept in a desiccator for further use. Market and Shillong samples were also subjected to extraction of yellow dye following above procedure. All turmeric samples were subjected to the estimation of curcumin content 15. λ max values of turmeric dye and curcumin for their 0.1% solutions in ethanol were determined on Cintra 20 UV visible spectrophotometer according to standard procedure. Heavy metal analysis of all the three samples was carried out using Varian Spectra A 250 Plus Atomic Absorption Spectrophotometer. Following fabrics were undertaken for dyeing purpose: 8 4 cm strips of silk (weight: 45 g/m 2 ); 8 4 cm strips of pure cotton (weight: 113 g/m 2 ); and 25 cm bolls pure wool (weight: 25 g/ boll). Myrabalan fruit (100 gm) powder with 1 L distilled water was heated at 90ºC with continuous stirring for 3 hrs and finally filtered. 10% myrabalan extract, thus prepared, was used for fixing pretreatment and mordanting. Silk & cotton strips and wool bolls were washed with 2 gm/ml soap solution for about 15-30 min, followed by washing with running tap water. The washed samples were dried under shade and were treated with 10% myrabalan extract for 15 minutes with continuous stirring and dried under shade. Alum, ferrous sulphate, copper sulphate, stannic chloride and eucalyptus bark dye extract were used for premordanting. The mordants were dissolved in water to obtained 5% concentrated solution. Pretreated

272 INDIAN J TRADITIONAL KNOWLEDGE, VOL 6, No. 2, APRIL 2007 myrabalan samples were dipped in mordant solution for 5 min with time to time stirring. The samples were dried under shade before immersing into the dye bath. Lactic and acetic acid (5 ml each) were added in dye solution at the start of dyeing in dye bath. A dye bath having 2% dye solution, maintained at 50-55 C was used for dyeing applications. The pretreated or/and pre-mordanted samples were immersed in the dye bath solution. The dyeing was done for 30 and 60 min for achieving light and dark shades. The dyed samples were taken out, squeezed gently and dried in shade. The dried dyed samples were washed with plain water followed by washing with 2 gm/ml mild soap solution and rinsing in running water. The samples were dried in shade and analyzed for their wash colourfastness. The dyed samples were tested for their wash colourfastness by washing with plain water 16. The samples were then subjected to observation of different stages of successive washing i.e. single wash, double wash, triple wash and hot wash (40-45 C). If the water became clean in successive washing stages, the dye was fast to the material. If the samples resulted into the lost of colour in washing stages, the dye was not fast on the material. Finally, the samples were dried under shade. A wide range of colours/shades was obtained on silk/cotton fibers and wool bolls using different mordants and experimental conditions. Prominent dyed samples have been presented as shade charts. Results and discussion Turmeric is one of the oldest natural colouring agents used throughout the world from ancient times 17-18. The rhizomes of the perennial turmeric are the source of colour. It is cultivated in almost all the parts of India. Curcumin is the prime principal constituent of yellow dye, along with other constituents like monodesmethoxycurcumin and bisdesmethoxycurcumin, which also contributes fewer amounts of pigment and flavour. Under experimental trials, different methodologies have been adopted for the extraction of colour. It was obtained through aqueous/solvent and spray drying techniques. The different trials were made to examine the technical feasibility of process at lab scale with reference its yield and quality. It was observed that yield of the colouring matter varied a lot depend upon the extraction procedure and habitat of the samples (Table 1). The results show that maximum yield was obtained in solvent extraction process followed by aqueous extraction and spray drying 19. Under spray drying, the yield was low but physical appearance and purity of the dye was superior with others. The colouring matter was a bright yellow amorphous powder, easily dispersible in water, ethanol and isopropyl alcohol. It has been classified as CI Natural Yellow 3 and considered as direct dye The curcumin is the main colouring constituent of the turmeric and according to some reports, its content varies from 2-8 % depending upon particular variety and habitat 20. The procedure for the extraction of pure curcumin is altogether different depending upon the type of application e.g. general or therapeutic purpose. Three samples were analyzed for their curcumin content and results are presented (Table 2). The Shillong sample has been found to be very rich in curcumin with compare to other samples. The λ max values 21-22 as determined through spectroscopic estimation were 426 nm for extracted dye and 420 nm for curcumin. As regards to the presence of heavy metals in three turmeric samples, their contents were found in safe limits, For example, the range was Cd, 0.02-0.04; Cu, 0.11-0.31; Cr, 0.38; Pb, 0.49-0.81; Ni, 0.06-0.34 and Mn 0.07-1.99 ppm. The results are presented in Table 3. These results clearly reveal that the extracted dyes are quit safe for eco-textile dyeing in accordance with the specified safe limits 23-26 under national and international standards. Under the present studies, all dyeing experiments have been made with natural fabrics e.g. 100% pure cotton, pure silk and pure wool. The fabrics were well washed with soap and in running water, so that all lose fibers and stains of dust or grease, if any, may be Turmeric Table 1 Yield of dyes in different samples Aqueous extraction % Solvent extraction (Ethanol) % Spray drying of aqueous extract % Lucknow sample 17.5 18.9 15.5 Market Sample 16.5 18.2 14.0 Shillong Sample 25.5 27.6 21.3 Table 2 Yield of curcumin in different samples Turmeric Curcumin % Lucknow Sample 2.5 Market Sample 2.4 Shillong sample 6.6

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SACHAN & KAPOOR: OPTIMIZATION OF TRADITIONAL TURMERIC DYE 277 Table 3 Heavy metal contents on different samples (ppm) Cd Cu Fe Zn Pb Cr Ni Mn 1. Lucknow Sample (Aqueous) 0.04 0.31 Nil 0.81 0.81 0.38 0.34 1.49 2. Market Sample (Ethanol) 0.02 0.11 5.33 1.53 0.47 Nil 0.31 0.28 3. Shillong Sample (Aqueous) 0.02 0.11 1.07 0.47 0.59 Nil 0.06 0.07 removed. Proper washing of the fabric facilitates the fixation of dye in uniform manner. Numerous dyeing experiments have been performed in view to obtain large number of shades with good fixation properties. Pre-fixation, premordanting, simultaneous mordanting, dye bath concentration, dyeing duration are some of the important aspects which enable uniform and smoothing colour effects to the fabrics. In present context of eco-friendly dyeing, natural mordants and safe mordant i.e. safe chemical salts were used. No salts of heavy metals like Ni, Cr, Pb, Co, Mn etc. were used. No doubt, the use of heavy metal salts could provides unlimited fast shades but there is no sense to use these in contest of environmental and health hazard considerations. Under dyeing experiments, natural mordants viz myrabalon extract, eucalyptus bark extract and safe chemicals viz aluminium sulphate, ferrous sulphate, copper sulphate, stannous chloride, acetic acid and lactic acid were used. Dyeing was performed directly with dye solution, mordanting with myrobolan or eucalyptus bark dye extract, pretreatment with myrobalan extract followed by mordanting with a mordant, or pretreatment with myrobalan extract followed by simultaneous dyeing with mordant and dye. Under experiments, wide range of shades has been developed using different mordants through varying experimental conditions. The observation of dyeing trials under various conditions conclude that 2% dyebath maintained at 50-55 C is the optimize condition and 30 minutes dyeing is sufficient time to obtained good results. However, the dyeing duration may be extended up to 60 min to get darker shades. It was also observed that 10% myrabalan, 1% eucalyptus dye and 5% mordant conditions were most appropriate for pre-fixation and mordanting treatment. The description of the shades along with experimental trials and dyeing conditions is summarized in shade colour charts (Figs 3-6). Conclusion Standard profiles have been developed for the extraction of yellow dye from turmeric rhizomes using aqueous, solvent and spray drying methodologies. Maximum yield was obtained through solvent extraction but purest dye was obtained through spray drying. The dyeing experiments reveal that the dye is quit suitable for dyeing cotton, wool and silk at 2% concentration. A variety of shades bright yellow, golden glow, ivory, sunset yellow, buff, light khaki, golden yellow, cream, smoke brown, pineapple, olive green, lemon, etc. were obtained with good washing properties through varying experimental conditions using different mordants. There is lot of scope to use the turmeric dye for obtaining numerous colour shades using safe mordants under eco-friendly textile dyeing. Acknowledgement Authors are thankful to Dr P Pushpangadan for his keen interest in the work and to CSIR for financial support by providing Emeritus Scientist Position (VPK) and SRF (KS) under an Emeritus Scientist Project. References 1 Kapoor V P, Dye Yielding Plants - Extraction and Applications, In: Advances in Ornamental Horticulture, (Poiter Publisher, Jaipur), 2005. 2 Gulrajani M L, Present status of natural dyes, Convention on Natural Dyes, Indian Institute of Technology, Delhi, December 9-10 th, 1999. 3 Kapoor V P, Studies on Indian Vegetable dyes, Final project report, National Botanical Research Institute, Lucknow, 1999. 4 Penfold A R, The Eucalypts, (JL Willis Interscience Publishers, NewYork), 1961. 5 Kapoor V P & Puspangadan P, Natural dyes-based herbal Gulal, Natural Product Radiance, 1 (2), (2002), 8-14. 6 Kapoor V P, Sachan K & Chandra S, Eco-dyeing processing with some traditional natural dyes, 89 th Indian Science Congress, Lucknow University, Lucknow, 3-7 January 2002. 7 Kapoor V P, Role of Natural Colours in Food Industry, Proc Dev Food Processing Industries in UP (Department and Food Processing UP, Lucknow), (2002).

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