7* ; ; — = 159 Recent developments in the production of spices and their essential oils in Ceylon

R. O. B. Wijesekera and A. L. Jayawardena Section of Natural Products, CISIR, Colombo, Ceylon

Summary Sommaire

Ceylon's export of spices, which formed about one per L'exportation des epices de Ceylan qui constituait cent of the value of its total exports during the decade environ un pour cent de la valeur totale des exporta­ 1950 to 1960, has increased to about two to three per tion pendant les annees de 1950 a 1960 a augmente cent during 1965 to 1970. Prices have if anything a environ deux a trois pour cent de 1965 a 1970. Les trended downwards during this period, this is due to prix ont meme eu tendance a baisser pendant cette an increase in the volume of oil exported. periode, a cause de l'augmentation du volume de l'huile exportee. The earnings from spices will be expected to increase in the coming years, with the setting up of the On pense que le gain apporte par les epices augmentera proposed 'Spices Board' by the Government and the de beaucoup pendant les annees a venir grace a la implementation of a planned programme of develop­ proposition du Gouvernement de fonder la 'Spices ment for spices. The production of essential oils from Board' et la mise en oeuvre d'un programme de spices - except in the case of cinnamon - is of very developpement des epices. La production d'huiles recent origin. Ceylon has, now, several private essentielles a partir d'epices a l'cxception de la cannelle producers of cardamom, nutmeg, pepper, ginger and est d'origine tres recente. Ceylan possede maintenant turmeric oils and oil production is expected to increase de nombreux producteurs prives d'huiles de cardamome, with the attention now being given to the growing of muscade, poivre, gingembre et curcuma et on pense these spices. Improved distillation techniques and que la production de ces huiles va augmenter grace a methods of quality control of spice oils and oleoresins l'importance donnee a la culture de ces epices. De are being developed at CISIR, and attempts are being meilleures techniques de distillation et des methodes made to use modern instrumental methods such as de controle de qua lite des huiles d'epices et oleoresines GLC and IR spectroscopy for the purpose. Studies on sont en cours de developpement au CISIR et a cette the chemical constituents of oil from various sources is fin, 1'utilisation d'instruments modernes tels que la a prerequisite to the proper quality assessment of these chromatographic gaz liquide et la spectroscopic infra- oils. The Bureau of Ceylon Standards is formulating rouge sont en cours d'essais. L'etude des constituents standards for all essential oils and spices produced in chimiques d'huiles de diverses sources est une necessite this country. It is expected that, with these develop­ anterieure a 1'evaluation de la qualite propre a ces ments, Ceylon will be able to offer spices and spice huiles. Le Bureau des Standards de Ceylan est en products in the future that will be better and more train de formuler des etalons pour toutes les huiles reliable in quality. The efforts now being made to essentielles et epices produites dans le pays. On improve growing aspects, distillation techniques and espere qu'avec ces developpements, Ceylan sera capable assessments of quality in order to achieve this end, d'offrir dans le futur des epices et produits d'epices are discussed. de meilleure qualite et plus depcndables. On debat les efforts en cours orientes a aineliorer la croissance, les techniques de distillation et 1'evaluation de la qualite afin de venir a bout du probleme.

Proceedings of the International Conference on Spices Tropical Products Institute, London. 1972. Introduction chillies are imported into the country from India and the Middle East. Among these are the following: - The: demand for spices and spice products in the Coriander Coriandrum sativum. L. markets of the world, shows an increasing trend1. During the period 1964 to 1968 a 36 per cent increase in Cumin seed Cuminum cyminum. L. the world demand for spices was recorded. This is Fennel Foeniculum vulgare. Mill. largely due to the development of food industries The main exported spice is cinnamon bark, in Europe and the United States which are attempting (Cinnamomum zeylanicum) in the form of quills. to use spices to add glamour and variety to their In this spice, Ceylon holds a pre-eminent position, products. particularly in its exports to Europe and South In Ceylon spices form about 2 to 3 per cent of the total America. Ceylon produces nearly 60 per cent of the value of exports and as a consequence are referred to world's cinnamon, with the Seychelles next, with collectively as 'minor export crops'. The production about 35 percent. Apart from cinnamon, Ceylon also of spices in Ceylon has remained almost at the same exports the following spices to both the United States level over a long period of time (1949 to 1969), as and Europe. judged by the volume of spices exported over this Cloves Eugenia caryophyllus period2 (see Figure 1). During the post-war period, Cardamoms Elettaria cardamomum Maton Ceylon also spent more foreign exchange than she earned on exporting spices, on importing other spices, Nutmeg Myristica fragrans Houtt. particularly dry chillies, of which she is the largest Pepper Piper nigrum importer. Thus, Ceylon had a deficit balance of trade Though traditionally famed lor the quality of its in respect of spices. This situation has only been spices it is apparent that Ceylon has neglected this remedied recently by firstly the restriction of imports valuable range of export commodities for too long. of chillies, and secondly a campaign to step up In recent times she has lost a substantial share of the domestic production. Several other spices apart from export markets to other countries.

Fiijure 1 Since exports from Ceylon, 1949 to 1969

1,000 CWT Million Rs.

140 - - 70

60

100

10

1 1 1 o ' ' 1 ' " 1 1 1 1 1 1 1 I n 1949 1951 1953 19bb 1957 1959 1961 196J 1965 1967 1969 Agricultural aspects improving market. Cardamom has also benefitted under the agricultural diversification scheme. During the last five years Ceylon has had to pay con­ Present trends in the development of the cultivation of siderable attention to the spice crops. An agricultural spices could be summarized as foliows:- diversification project has been set up with FAO/ (1) New planting programmes to be undertaken UNDP assistance, and this has resulted in substantial during 1972 to 1976 to increase the acreage under increases in the local production of these crops. A cultivation. subsidy scheme is in operation for some of these (2) A comprehensive scheme of subsidies to be crops, and the scheme currenUy operates for uneconomic tea and rubber plantations to encourage brought into operation. replanting into spice crops. The Ministry of Plantation (3) Agricultural research, particularly with respect to Industries is presently working on a more compre­ fertilizer response to be sponsored by the hensive scheme of subsidies which will encompass all Department of Minor Export Crops and to be spice crops grown in Ceylon. One of the crops carried out in collaboration with the Central receiving immediate attention is chillies which are an Agricultural Research Institute at Gannoruwa important item in the local diet. Chillies are eaten as and the Dry Zone Research Station at Maha green chillies, as well as in the dry form, in curries Illuppalama, and the proposed Research Institute and sambols. The restriction on imports of chillies on Minor Export Crops. has greatly encouraged the domestic production of chillies and the present five year plan envisages self- sufficiency in this commodity by 19763. The present production of 125,000 cwt of dry chillies is to be stepped up to 600,000 cwt by 1976. Several problems Research and quality assessment of spice products have been encountered in the production of chillies in Ceylon, and the occurrence of 'leaf curl* is one of Until very recent times, Ceylon exported only whole them. The leaf curl complex4 is caused by mites, spices except in the case of cinnamon leaf oil which thrips, viruses and possibly deficiency diseases. Effec­ was produced in south Ceylon using very primitive tive remedies against mites and thrips are available but equipment. During the last few years a handful of there is no solution as yet for the control and preven­ private entrepreneurs have successfully processed and tion of the virus diseases. Some results have been marketed various types of spice oils and oleoresins, achieved in breeding for resistance to these viruses and such as cardamom oil, ginger oil, pepper oil, clove strains resistant to viral attack for a long time are now leaf and bud oils, and nutmeg oil. These products available5. The second problem in the island-wide produced with considerable care and thorough applica­ propagation of chillies is that of preserving the seed so tion of basic scientific 'know-how' have been most that a high percentage of germination is retained for acceptable to the sophisticated markets of Europe, the some time. Collaborative work by the CISIR and the USA and Canada. Dry Zone Research Station at Maha Illuppalama has given encouraging results6 in retaining a high percentage There is a tremendous interest at the moment in the of viability in the seeds. production of spice oils and oleoresins, and plenty of room for work directed towards the improvement in the techniques currently used. The increased attention Microbial deterioration of dried chillies during storage being paid to the cultivation of these spices has been gives rise to several problems like mould growth, loss initiated by the promising market potential of spice of flavour and stack burning. Investigations at the oils and oleoresins and has enhanced the need for CISIR7 established the optimum conditions for storage research on spice oils and oleoresins produced in of chillies, as a maximum moisture content of 15 per Ceylon. The CISIR mindful of this has launched into cent under an atmosphere of 65 per cent relative humidity a programme of research covering the chemistry, for short term period and for storage for indefinite periods exceeding one year, a maximum moisture analytical methods, and technology of essential oils content of 12V4 per cent under a storage atmosphere and spices. Suitable methods for the quality control of 60 per cent or less relative humidity. of these products are needed if Ceylon is to retain the markets it intends to secure. Both the CISIR and the Bureau of Ceylon Standards are now working towards Cardamom production in Ceylon has recently received this end. a substantial boost, due to favourable prices obtained for the spice and its oil in the world markets. It is The CISlR's programme of research on spices is now estimated3 that Ceylon has about 12,000 acres designed to develop better methods of processing of under cardamom cultivation: Cardamom grows very spice oils and oleoresins, in order to furnish the well in the central regions of Ceylon. A substantial markets with quality products; to investigate the part of the cardamom plantations are in 50 acre chemical constituents of these spices and to develop holdings or more and the larger holdings are advanta­ modern methods of quality control and assessment geous in the implementation of the proposed develop­ based on the latest instrumental techniques. On a ment programmes. Ceylon's exports in this commodity long term basis it is hoped that methods for producing doubled between 1965 to 1970 due to new plantings, isolates and aromatic chemicals of industrial value increased prices, attention to harvesting methods, from the spices will also be developed and new sources maintenance and processing in the face of a rapidly of valuable aromatic chemicals discovered. The design and construction of suitable stills for the trade in Ceylon fears that the bark oil may be ••%» production of spices is handicapped by the non­ adulterated with leaf oil and consequently is reluctant availability of material for fabrication. Stainless steel, to guarantee oils purchased by them at source. GLC aluminium, galvanized iron, etc have to be imported techniques can readily be used to detect any such and thus the initial outlay becomes very expensive. adulteration. They also could be used to detect any, The CISIR is presently working on the design for three adulteration of genuine Ceylon cinnamon bark oil with sizes of stills: cassia (Cinnamomum cassia) a common adulterant,'as Type A - To handle bulky material up to a charge the GLC profiles of the three oils have very significant volume of 2,000 kg, eg for grasses like differences (see Figure 3). lemon grass and for cinnamon leaf; Type B - To handle charges up to 1,000 kg. To be used for cinnamon bark, ginger, nutmeg, Pepper oleoresins etc. Oleoresins are also being produced now in Ceylon and Type C - To hand the 'fine spices' like clove, are finding good markets in Europe. Oleoresins are cardamom and pepper. difficult to standardize since they involve not only Some valuable improvements in the design of type A the volatile oil but very often other constituents which stills have already been effected by the employment of are responsible for desired features such as pungency. some new ideas to suit the local environment. The oleoresins of pepper and red chillies are two typical examples. Methods available for quality control The assessment of quality in spice oils and spice of pepper are often vitiated by additives. For example, oleoresins demands the use of modern techniques in the estimation of total nitrogen as an index for analytical chemistry such as gas liquid chromatography, piperine content is invalidated by the addition of thin layer chromatography, and infra-red spectroscopy. adulterants containing nitrogen9. A method for It is also necessary that prior to developing methods quality assessment of pepper oleoresin has been pro­ of quality assessment, a thorough study of the chemical posed10. It is based on: constituents of the essential oils be made. Such a study would involve the utilization of all the above (i) Estimation of the residual solvent by means of 11 techniques and more. The CISIR's Natural Products existing GLC methods Section has undertaken this assignment and some (ii) Determination of the piperine content by a typical examples of the work done are described here. rapid quantitative TLC method. (iii) The use of two-dimensional TLC to detect any foreign additives (see Figure 4). Cardamom oil. (oil of Elettaria cardamomum Maton) (iv) Estimation of the amount of p'-caryophyliene Figure 2(v) by GLC. Cardamom oil of very good quality is now distilled in Ceylon. Detailed GLC studies8 on the essential oils The determination of the residual solvent is carried from various types of cardamom grown in Ceylon out using one of the existing GLC methods. The thin revealed that there were recognizable differences layer chromatographic method for the determination of between the oils from them. The giant wild cardamom piperine10 depends on the separation of piperine as a (Elettaria ensal (Gaertn.) Abeywick) endemic to single spot and its visualization with a colour reagent, Ceylon gave an oil that bore little resemblence to the followed by use of the spot-area method"'13 for oil from the commercial cardamom. The two com­ quantitative estimation. pounds 1, 8-cineole Figure 2(i) and a-terpinyl The estimation of the amount of p'-caryophyliene in acetate Figure 2(ii), which together form the major the oleoresin itself can serve as a measure of the part of commercial cardamom oil are present only in essential oil content in the oleoresin, as in the Ceylon trace quantities in the wild variety. The cineole/a- variety the p'-caryophyliene content varies very little terpinyl acetate ratio in cardamom oil is a fairly good from sample to sample. index of the purity and authenticity of the oil. The ratio is usually around 0.7 to 1.4 (SD = ± 0.4). When Several other methods for the quality control of the distillation has been carried out for less than the various spice oils and oleoresins are in the process of optimum duration, the ratio oversteps this range as the being worked out and doubtless would serve to full amount of the higher boiling a-terpinyl acetate improve the quality of exported spice products. has not come completely over in the distillation. The Ceylon is most keen to see that only the best possible presence of the monoterpene hydrocarbons in the products free of adulteration are exported from the »sual amounts, is indicative of the freshness of the country. naterial distilled. iinnamon oil. (oil of Cinnamomum zeylanicum) Proposals regarding the organization of the spice industry tbth cinnamon leaf and bark oil are distilled in Ciylon. These oils are now offered to the market in The current five year plan of the Government3 ttrms of their content of eugenol Figure 2(iii) and envisages a considerable increase in the exports of ciinamaldehyde Figure 2(iv). The amount of eugenol several minor export crops which includes all the huhe Ceylon leaf oil is around 70 to 80 per cent. The spices now cultivated in Ceylon and many others

164 Figure 3 Comparison of the GLC profiles for oil from cinnamon leaf and bark and cassia.

Operating parameters

Instrument Varian 1740

Column LAC 2R 446 : 15per cent on Chromosorb - W 3 metres x 3 mm

Temperatures Injectors 200°C

Detectors 245°C

Column Initial 6CTC Column Final 190°C

Programmed at 2u/min Linear

Detector Dual flame ionisation

Range 16 x 10'10amp f.s.d.

Carrier gas Argon — 27.5 ml/min

Recorder Varian G - 1000 (2mV range)

100

CINNAMON 90 80 70 60 50 \ 40 V I 1 • ""^ 30 1 20 i i nII .. a 111I L^v i\ j\ AAJ 10 0 190" 60"

100 90 1 Cassia 80 70 I 60 l 50 L / 40 u 30 / 20 10 0 190° 60" Figure 4 Thin layer chromatograms of pepper essential oil and pepper oleoresin

la) Pepper essential oil (CISIR sample)

Benzene / Et Ac 10 : 1

Spray Vanillin / H2S04 Heat 100°C

Brown , > BrQwn

Violet

' Hexane / Acetone 7:3

lb) Pepper oleoresin (CISIR sample)

Benzene / Ct Ac 10 : 1 dK Violet

Spray Vanillin / H2S04

Red uv —I— \ /~\

Red uv \J \J Vi0iet

Red uv fW 1/

-Green — Blue uv

Violet -4— J f j a Brown ^

Yellow

Hexane / Acetunu 7:3 166 Table I

Ceylon: present production and acreages of spice crops and proposed increased acreages

Spice Acreage present proposed increase Production World Production

1. Cinnamon 36,000 4,000 3,000 tons 5,000 tons 2. Pepper 1,600 tons 3. Cardamom 9,500» 6,000 4. *C'loves 1,500 4,000 5. •Nutmeg 2,500 2,000 6. Lemon grass 200 5,000 - - •Does not take into account an estimated 2,500 acres already planted during 1968 to 1970.

which have shown promise of cultivation possibilities. fully realized that in the not too distant future, the The present acreage is to be extended by new planta­ once renowned 'Spices of Ceylon', may adequately aid tions, see Table 1, and existing plantations are to be her in her dire financial situation. rehabilitated and replanted when necessary. It is hoped that the proposed Research Station on the minor export crops will enhance the agronomic aspects Acknowledgements of the spices while the CISlR's efforts in respect of then chemistry and technology will help develop the The authors are grateful to Miss C. L. M. Nethsingha, industry further. Chief Librarian CISIR, for critical comments and much help in the preparation of this paper; to The Ministry of Plantation Industry is also finalizing Mr S. F. Laurentius, Chief Research Officer, of the plans for assisting the cultivators of spices with CISIR and Dr M. A. V. Devanathan, Head of the incentives for fertilizer use. Purchasing boards are to Physical Chemistry Division, for valuable discussions be set up for certain crops which have been adversely on the subject matter of this paper; to Dr E. Jayanetti, affected by price instability and the export promo­ Director, Minor Export Crops, Ministry of Plantation tional effort is to be strengthened. Industries, and Dr Ravindra A. H. Weerakoon, Director In order to co-ordinate activity in the matter of CISIR, for their interest in this work; and to Messrs Ceylon's spice industry, a 'Spice Board' is to be set K. Ratnasingham, S. Ponnasamy, A. T. Jayalath and up soon and it will be responsible for the development Mrs Shirani Wijayanayaka for help in various ways in anil promotional programmes. It has now been the preparation of this manuscript.