RU2417094C2 - Method for producing strobile essence - Google Patents

Abstract

FIELD: medicine, pharmaceutics.

SUBSTANCE: invention refers to chemical-pharmaceutical industry, namely to a method for producing pine essence by vapour distillation of raw ground at temperature and essence separation from the distillate. Strobiles of low juniper pre-grounded to 2-3 mm, or of Korean pine pre-grounded to 1.5-2,5 cm are kept for 2 hours at temperature 70°C in a hermetically sealed distillation bowl. Vapour distillation is carried out at pressure 0.09-0.12 MPa and temperature 100-110°C for 6 hours.

EFFECT: prepared pine essence exhibits higher content of biologically active substances and extends a raw material base for producing thereof.

2 ex, 6 tbl, 1 dwg

Description

The invention relates to methods for extracting coniferous oil from plant materials and can be used in the pharmaceutical, medical, chemical industries, as well as in forestry and agriculture.

A method of producing fir oil is known in the literature [1].

Closest to the claimed invention in technical essence is a method for producing coniferous essential oil [2].

The disadvantages of this method compared with the claimed are: the duration of the process, the limited types of plant materials and the loss of valuable biologically active components: pinenes, fellandrenes, bornyl acetate and thujone. These substances are used for the synthesis of drugs or are part of the drugs [3, 4].

These components are part of many essential oils used in both official and traditional medicine [5].

The aim of the invention is the search for sources of plant materials containing biologically active substances (pinen, fellandren, bornyl acetate, thujone and others) and the development of technology for the production of coniferous essential oils with their high content, utilization of wood waste, expanding the raw material base for biologically active substances.

Essential oils containing biologically active components, in particular the above, it is possible to use both in its natural form and as a raw material substance for the creation of drugs.

Coniferous essential oils have antiseptic, anti-inflammatory, antispasmodic, sedative, analgesic, anti-ulcer and wound healing effects [6].

The identification of new sources of biologically active substances and increasing their yield is an important direction in a number of industries of production and consumption.

The goal is achieved by the fact that:

1. Plant materials are preliminarily kept in a hermetically sealed vat at a temperature of 70 ° C for 2 hours.

2. Distillation of essential oils with water vapor is carried out at a temperature of 100-110 ° C and a pressure of 0.09-0.12 MPa for 6 hours.

3. The raw materials used are the fruits (cones) of Siberian or Daurian juniper and the cones of Korean pine (Korean cedar).

An example of the method

1. Juniper fruits (cones), crushed to a size of 2-3 mm, are loaded into a distillation tank 1 of a batch plant and kept for 2 hours at a temperature of 70 ° C, and then water vapor is passed through them from a steam boiler 2 at a temperature of 100- 110 ° C and a pressure of 0.09-0.12 MPa for 6 hours. Water vapor extracts essential oils, which contain fellandren, bornyl acetate, thujone and other biologically active substances, and condenses in the refrigerator 3, from which their mixture is supplied with water and separated in oil separator 4 (Florentine). The oil enters the oil receptacle 5, and the Florentine water - into the tank 6. From one ton of crushed cones of Siberian juniper 25.5-29.8 kg of essential oil is obtained, from the cones of Daurian juniper - 19.8-21.5 kg.

2. Cones of Korean pine (Korean cedar), freed from nuts, waste of harvesting nuts, crushed to a size of 1.5-2.5 cm, loaded into a distillation vessel of a batch installation and kept in a hermetically sealed vessel for 2 hours at temperature 70 ° C, and then water vapor is passed through them from the steam boiler at a temperature of 100-110 ° C and a pressure of 0.09-0.12 MPa for 6 hours. Water vapor extracts essential oils, which contain pinen, phylladren, bornyl acetate, thujone and other biologically active substances, and condenses in the refrigerator, from which their mixture with water comes and is separated in an oil separator (Florentine).

From one ton of crushed cones of Korean pine (Korean cedar) get 7-10 kg of essential oil.

Essential oil containing biologically active substances can be successfully used in its natural form and as a raw material substance for the extraction of individual substances: fellandrenes, bornyl acetate and other components, and their subsequent use in medicine, as well as a biological additive in various new drugs based on plant materials (for example, in flavored products for therapeutic baths and aromatization of premises). Tables 1-6 provide data on the selection of the optimal parameters of the distillation process.

Table 1 The output and composition of the main components from the cones of Siberian juniper Name of components, wt.% Distillation temperature, ° С 95 one hundred 110 120 α-pinene 1.9 17.4 13,4 2.0 β-pinene 2,4 17.8 17,2 5.7 Tuyon 1,5 11.6 11.2 6.8 Bornyl acetate 1.8 16,2 16,0 1,0 % oil yield from abs. dry matter 1,0 2.98 1,0 0.5

table 2 The output of essential oil from cones of Korean pine, freed from nuts, and the composition of the main components Name of components, wt.% Distillation temperature, ° С 95 one hundred 110 120 α-pinene 2.2 22.7 22.0 18.0 β-pinene 2.6 23.8 21.3 20.3 Sum of (α + β) fellandrenes 1,5 16,4 16,0 6.2 Bornyl acetate 9,4 28.6 20.6 15.8 Oil yield from abs. dry matter 0.1 1,2 0.3 0.1

Table 3 The results of the effect of grinding juniper fruits (cones) on the yield of essential oil Essential Oil Yield Unfinished cones Size of grinding cones, mm 5,0 3.0 2.0 1,5 % of abs. dry raw materials 1,2 1,5 2.95 3.00 1.8

Table 4 The results of the effect of chopping Korean pine cones on the yield of essential oil Essential Oil Yield Unfinished cones Size of crushing cones, cm 5,0 2.5 1,5 1,0 % of abs. dry matter 0.2 0.80 1.25 1.42 0.6

Table 5 The composition of the main components of the essential oil (cones) of Siberian juniper during grinding Name of components, wt.% Unfinished cones Size of grinding cones, mm 5,0 3.0 2.0 1,5 α-pinene 2.2 2,8 17.0 14.8 2,8 β-pinene 2.6 3.2 18.2 17.4 3,7 Tuyon 1.7 2.0 12,4 12.0 2,4 Bornyl acetate 1.4 2.2 17.6 15.8 1.8

Table 6 The composition of the main components of the essential oil of Korean pine cones when chopping Name of components, wt.% Unfinished cones Size of crushing cones, cm 5,0 2.5 1,5 1,0 α-pinene 8.0 14.2 21.8 22.0 16.8 β-pinene 6.2 13.1 24.6 21.9 17.3 Sum of (α + β) fellandrenes 2.2 3.8 17.6 16,4 4.6 Bornyl acetate 5.8 9.6 28.8 22.4 12,4

As can be seen from tables 1 and 2, the optimal temperatures of the distillation process are temperatures of 100-110 ° C, since they allow you to get essential oils with the highest yield and maximum content of the main components of the oil.

The lower (95 ° C) and upper (120 ° C) temperature limits do not allow to achieve the highest yield and content of components of essential oils.

Tables 3 and 4 show that the grinding of raw materials has an important effect on the yield of oils. So, for juniper cones, it is advisable to chop to sizes of 2-3 mm, and for pine cones of Korean - to sizes of 1.5-2.5 cm.

The effect of grinding raw materials on the composition of the main components of the oils are given in tables 5 and 6.

As follows from these tables, when grinding Siberian juniper cones to a size of 2-3 mm, the maximum content of dominant components is achieved. For Korean pine cones, an increase in the main components occurs when grinding to sizes of 1.5-2.5 cm.

Thus, the method is carried out as follows in a batch installation shown in the drawing.

Juniper cones (fruits), crushed to a size of 2-3 mm, or Korean pine cones, crushed to a size of 1.5-2.5 cm, are loaded into a distillation vessel 1 of a batch plant of the West Siberian type, for example, PPU-1 type, at a temperature of 70 ° C for 2 hours and water vapor is passed from the boiler-steam generator 2 at a temperature of 100-110 ° C and a pressure of 0.09-0.12 MPa for 6 hours. Passing steam extracts essential oils from the feedstock and condenses in the refrigerator 3, from which a mixture of them with running water enters and is separated in Florentine (oil separator) 4. Coniferous oil with biologically active substances accumulates in the oil receiver 5, and the running water in the tank 6.

Information sources

1. Kalinin A.M. Production of fir oil / A.M. Kalinin, G.V. Nikiforov. M .: Forest industry, 1979. - 104 p.

2. AS of the USSR 1723109 A1, СВВ 9/02, А61К 31/37. The method of obtaining coniferous essential oil [text] / Yu.G. Tagiltsev, R. D. Kolesnikova (USSR) - No. 4856529/13; declared 06/04/1990; publ. 03/30/1992, Bull. No. 12 - 6 p., 1 ill.

3. Nikitin V.M. Chemistry of terpenes and resin acids / V.M. Nikitin. - M .: Science. - 1952. - 348 p.

4. Register of medicines of Russia: Sat. / Ed. Yu.F. Krylova. - M.: Genfarmkhim. 1993 .-- 989 p.

5. Tagiltsev Yu.G. Far Eastern plants - our doctor / Yu.G. Tagiltsev, R.D. Kolesnikova, A.A. Nechaev. - Khabarovsk: Dalpress - 2004 .-- 520 s.

6. Coniferous healers / Yu.G. Tagiltsev [et al.] - Khabarovsk: KhKTSPZ publishing house, 2004. - 52 p.

Claims (1)

A method of producing coniferous essential oil by steam distillation of crushed raw materials at a temperature followed by separation of the essential oil from the distillate, characterized in that Siberian juniper cones pre-crushed to sizes 2-3 mm or Korean pine cones crushed to sizes 1.5-2.5 cm incubated for 2 hours at a temperature of 70 ° C in a hermetically closed distillation tank, and steam distillation is carried out at a pressure of 0.09-0.12 MPa and a temperature of 100-110 ° C for 6 hours

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