RU2621024C2 - Method for producing and composition of melon seeds oil - Google Patents

Abstract

FIELD: food industry.

SUBSTANCE: melon seeds oil obtained by treating melon seeds collected in September by means of the method of supercritical fluid extraction by carbon dioxide. Wherein dried seeds of "Lada" sort of melon are used, crushed to particle size of1.0-2.0 mm, and the extraction is performed during 50 minutes at the pressure of 300 atmospheres, the temperature of 40°C and the carbon dioxide flow rate of 40 g/min.

EFFECT: invention provides obtaining melon seed oil comprising linoletic acid in a higher yield, with the simultaneous extraction of other 10 fatty acids.

3 cl, 1 dwg, 9 tbl, 27 ex

Description

The invention relates to the food industry and relates to a method for producing oil from melon seeds containing linoleic acid as a main component using supercritical fluid extraction.

The closest example to the claimed method for producing oil is a method for producing pumpkin oil by pressing with preliminary thermal treatment of crushed seeds at a temperature of 80-90 ° C and subsequent filtering of the oil [A.N. Shikov, V.G. Makarov, V.E. Ryzhenkov. Vegetable oils and oil extracts: technology, standardization, properties. M .: Russian doctor. 2004, S. 120-121].

The disadvantage of this method is that it does not allow to obtain oil with the extraction of other fatty acids (the number of extracted fatty acids is 6).

A known method of obtaining an extract from pumpkin seeds [RF patent No. 2051596], including the extraction of pumpkin seeds with vegetable oil in a ratio of 1: 2 in a water bath for 1.5 hours, followed by centrifugation and separation of the target product.

The disadvantage of this method is that it does not allow to obtain pure pumpkin seed oil.

A known method of producing oil from pumpkin seeds [RF patent No. 2197977], comprising the following steps: sterilization of seeds with hot air at a temperature of 100-120 ° C for 2.5-3.5 minutes, followed by lowering the temperature of the plant material to the environment and mechanical extraction of seeds at 60 ° C.

A known method of producing oil from pumpkin seeds [RF patent No. 2170027], which provides for the sorting and drying of seeds at first at 20-22 ° C, and then at 60-80 ° C and subsequent pressing.

A known method of producing oil from pumpkin seeds [RF patent No. 2064485], which consists in sorting the seeds, drying them at 50-60 ° C for 15-20 minutes and pressing at 70 ° C, followed by filtration at 40 ° C.

A known method of producing oil from pumpkin seeds [RF patent No.2018514], which includes grinding the seeds to wholemeal flour, heat treatment at a temperature not exceeding 60 ° C and pressing.

A known method of producing oil from pumpkin seeds [RF patent No. 2441664], which provides for the sorting of raw materials, grinding, steam treatment of seeds for 2-5 minutes and their cold pressing.

A known method of producing oil from pumpkin seeds [RF patent No. 2445111], which boils down to the following stages: seed disinfection, peeling and impurities, steaming and pressing seeds at first at 70-75 ° C, then at 20-25 ° C and oil filtration.

The disadvantage of these methods is that the heat treatment of seeds at the initial stage of the process can contribute to the destruction of some of the valuable substances that make up pumpkin oil.

A known method of producing oil from watermelon seeds [RF patent No. 2542758], based on the grinding of biological material and subsequent processing of it with supercritical carbon dioxide.

However, the above methods for producing oils cannot be analogues, since they are obtained from other plants.

We found that the grinding of vegetable raw materials of melon seeds of the Lada variety (Cucumis meld) dried at 30-35 ° C for 1.0-1.5 hours to a particle size of 1.0-2.0 mm leads to an increase the yield of oil during the extraction with carbon dioxide for 50 minutes (table 2), at a pressure of 300 atmospheres (table 4), a temperature of 40 ° C (table 5) and a flow rate of carbon dioxide of 40 g / min (table 6). At the same time, the extraction of other components increases simultaneously. With a longer extraction, the yield of valuable components, in particular linoleic acid and other fatty acids, decreases (table 3).

Reducing the amount of fatty acids is a disadvantage of the method of obtaining oil from melon seeds for a longer extraction.

The problem solved by the invention is the production of oil from melon seeds, including linoleic acid, with a higher oil yield and simultaneous extraction of 10 other components besides linoleic acid (drawing). The problem is solved with the help of oil from plant materials, representing melon seeds, including linoleic acid. The oil was obtained by supercritical fluid extraction with carbon dioxide, dried at 30-35 ° C for 1.0-1.5 hours, seeds of Lada melon, crushed to particles with a size of 1.0-2.0 mm, followed by extraction for 50 minutes, at a pressure of 300 atmospheres, a temperature of 40 ° C and a flow rate of carbon dioxide of 40 g / min. Melon seeds collected in September are preferably used, since the oil yield from the seeds during this period is maximum (Table 7). Grinding raw melon seeds to a particle size of 1.0-2.0 mm leads to an increase in the yield of oil from melon seeds. Along with linoleic acid, other valuable fatty acids are also extracted, which under other extraction conditions are not extracted in such quantities. Grinding the feed to a particle size of less than 1.0 mm (0.7 mm) led to a decrease in the oil yield from 62.63% to 62.25% (table 2, example 9). Raw materials, crushed to a particle size of 1.0-2.0 mm, followed by extraction for 50 minutes, at a pressure of 300 atmospheres, a temperature of 40 ° C and a carbon dioxide flow rate of 40 g / min, allows to obtain oil from melon seeds with a higher content and the number of active components, without violating their structure. With a longer extraction time, more than 50 minutes (table 3, example 14), or higher pressure, more than 300 atmospheres (table 4, example 17), or higher temperature, more than 40 ° C (table 5, example 20), or at a higher flow rate of carbon dioxide, more than 40 g / min (table 6, example 24), undesirable processes can occur, which leads to a decrease in the yield of linoleic acid and a number of other fatty acids (table 3, example 14).

When grinding raw materials to particles with a size of 10 mm, a high oil yield is not achieved (table 2, the oil yield is 15.5%). When the degree of grinding of raw materials of 0.7 mm decreases the amount of linoleic acid from 62.54% (table 2, example 7) to 62.25% (table 2, example 9).

The following shows the content of the components in the resulting oil according to the claimed method.

The difference of the present invention from previously known methods for producing oils is that as a raw material, seeds of Lada melon dried at 30-35 ° C for 1.0-1.5 hours are collected in September and crushed to particle size 1.0-2.0 mm followed by extraction with carbon dioxide for 50 minutes, at a pressure of 300 atmospheres, a temperature of 40 ° C and a carbon dioxide flow rate of 40 g / min. The technical result of the proposed solution is to obtain oil from melon seeds, including linoleic acid, with a higher yield with the simultaneous extraction of 10 other fatty acids (table 8). The ratio of unsaturated and saturated acids of oil from melon seeds is shown in table 9.

A method of obtaining oil from melon seeds is as follows.

Dried at 30-35 ° C for 1.0-1.5 hours and crushed to a particle size of 1.0-2.0 mm melon seeds of the Lada variety, preferably collected in September, weighing 65 g are poured into a separator of 200 ml supercritical extractor brand SFE-500 M1 (company THAR). Plant materials are treated in supercritical carbon dioxide for 50 minutes, a pressure of 300 atmospheres, at a temperature of 40 ° C and a carbon dioxide flow rate of 40 g / min, followed by separation of the oil.

The chemical composition of the obtained oil samples from melon seeds was studied by chromatography-mass spectrometry on an Agilent instrument with a library of 40 thousand chemical compounds, the quantitative determination of oil components was carried out by gas-liquid chromatography on a Shimadzu QP 2010 chromatograph with a mass-selective detector after the conversion of fatty acids to the corresponding ones methyl esters when treated with diazomethane. The diazomethane ether solution was obtained from N-nitroso-N-methylurea by a known method [G. Becker, G. Domshke, E. Fanghenel. Organikum: in 2 volumes T. T. 2. M .: 1979. S. 248]. The NIST 02 mass spectra library was used for identification. Chromatography was performed on an MDN-1 column (methyl silicone, solid bound) 30 m, diameter 0.25 mm. Chromatography mode: injector - 180 ° C; detector - 200 ° C; interface - 210 ° C; carrier gas - helium 1 ml / min. when dividing the stream 20: 1; thermostat 60 ° C - 1 min, 2 degrees / min - up to 70 ° C, 5 degrees / min - up to 90 ° C, 10 degrees / min - up to 180 ° C, 20 degrees / min - up to 280 ° C, then the isotherm - 1 min. The content of oil components from melon seeds is given in mass. %

Example 1

1,4735-1,5015. Относительная плотность изменялась в пределах d₄ ²⁰ 0,9153-0,9420. Выход и состав основных компонентов масла приведены в таблице 1.An exact weighed portion of the raw material (65 g) of melon seeds dried at 30-35 ° C for 1.0-1.5 hours and crushed to a particle size of 10 mm is placed in a separator with a volume of 200 ml of a SFE-500 M1 supercritical extractor (THAR company ) and carry out extraction in a medium of supercritical carbon dioxide for 20 minutes, a pressure of 300 atmospheres, at a temperature of 40 ° C and a flow rate of carbon dioxide of 40 g / min. The pressure is released to atmospheric pressure, and the oil is collected in the receiver, it is a yellow liquid, the refractive index changed to insignificant limits and is equal to

1.4735-1.5015. The relative density varied within d ₄ ²⁰ 0.9153-0.9420. The output and composition of the main components of the oil are shown in table 1.

Example 2

Similar to example 1, only the extraction of oil in a supercritical extractor is carried out for 30 minutes (yield and composition are shown in table 1).

Example 3

Similar to example 1, only the extraction of oil in a supercritical extractor is carried out for 40 minutes (yield and composition are shown in table 1).

Example 4

Similar to example 1, only the extraction of oil in a supercritical extractor is carried out for 50 minutes (yield and composition are shown in table 1).

Example 5

Raw materials (melon seeds), crushed to particles with a size of 10 mm. Oil extraction in a supercritical extractor was carried out for 50 minutes, while observing the technological parameters of the extractor, indicated in example 1 (yield and composition are shown in table 2).

Example 6

An accurate sample of raw materials (65 g) of melon seeds, crushed to particles of 7 mm in size, is placed in a supercritical extractor. The extraction is carried out for 50 minutes, subject to the technological parameters of the extractor, indicated in example 1 (yield and composition are shown in table 2).

Example 7

Similar to example 5, only a sample of raw materials (65 g) of melon seeds is crushed to particles 2 mm in size (yield and composition are shown in table 2).

Example 8

Similar to example 5, only a sample of raw materials (65 g) of melon seeds is crushed to particles 1 mm in size (yield and composition are shown in table 2).

Example 9

Similar to example 5, only a sample of raw materials (65 g) of melon seeds is crushed to particles with a size of 0.7 mm (yield and composition are shown in table 2).

Example 10

Similar to example 5, only a sample of raw material (65 g) of melon seeds is crushed to particles 1 mm in size. Oil extraction in a supercritical extractor was carried out for 20 minutes (yield and composition are shown in table 3).

Example 11

Similar to example 10, only the extraction of oil in a supercritical extractor was carried out for 30 minutes (yield and composition are shown in table 3).

Example 12

Similar to example 10, only the extraction of oil in a supercritical extractor was carried out for 40 minutes (yield and composition are shown in table 3).

Example 13

Similar to example 10, only the extraction of oil in a supercritical extractor was carried out for 50 minutes, subject to the technological parameters of the extractor, indicated in example 1 (yield and composition are shown in table 3).

Example 14

Similar to example 10, only the extraction of oil in a supercritical extractor was carried out for 60 minutes, subject to the technological parameters of the extractor, indicated in example 1 (yield and composition are shown in table 3).

Example 15

Similar to example 13, only the extraction was carried out at a pressure of 200 atmospheres, while observing the technological parameters of the extractor, indicated in example 1 (yield and composition are shown in table 4).

Example 16

Similar to example 13, only the extraction was carried out at a pressure of 300 atmospheres while observing the technological parameters of the extractor, indicated in example 1 (yield and composition are shown in table 4).

Example 17

Similar to example 13, only the extraction was carried out at a pressure of 400 atmospheres while observing the technological parameters of the extractor, indicated in example 1 (yield and composition are shown in table 4).

Example 18

Similar to example 13, only the extraction was carried out at a temperature of 32 ° C, subject to the technological parameters of the extractor, indicated in example 1 (yield and composition are shown in table 5).

Example 19

Similar to example 18, only the extraction was carried out at a temperature of 40 ° C, subject to the technological parameters of the extractor, indicated in example 1 (yield and composition are shown in table 5).

Example 20

Similar to example 18, only the extraction was carried out at a temperature of 45 ° C while observing the technological parameters of the extractor specified in example 1 (yield and composition are shown in table 5).

Example 21

Similar to example 19, only the extraction was carried out at a flow rate of carbon dioxide of 20 g / min, subject to the technological parameters of the extractor, indicated in example 1 (yield and composition are shown in table 6).

Example 22

Similar to example 21, only the extraction was carried out at a flow rate of carbon dioxide of 30 g / min, subject to the technological parameters of the extractor specified in example 1 (yield and composition are shown in table 6).

Example 23

Similar to example 21, only the extraction was carried out at a flow rate of carbon dioxide of 40 g / min, subject to the technological parameters of the extractor specified in example 1 (yield and composition are shown in table 6).

Example 24

Similar to example 21, only the extraction was carried out at a flow rate of carbon dioxide of 50 g / min, subject to the technological parameters of the extractor specified in example 1 (yield and composition are shown in table 6).

Example 25

Similar to example 13, only the collection of raw melon seeds was carried out in the month of August (the oil yield is shown in table 7).

Example 26

Similar to example 13, only the collection of raw melon seeds was carried out in the month of September (the oil yield is shown in table 7).

Example 27

Similar to example 13, only the collection of raw melon seeds was made in the month of October (the oil yield is shown in table 7).

Thus, in the process of searching for the optimum degree of grinding of raw materials from seeds of Lada melon, collected mainly in September, containing linoleic acid, it was found that it is optimal to use the particles with a size of 1.0–2.0 mm, followed by extraction carbon dioxide for 50 minutes, at a pressure of 300 atmospheres, a temperature of 40 ° C and a flow rate of carbon dioxide of 40 g / min, since under these technological conditions a higher oil yield is combined with a higher content of l Entrance acid and other fatty acids (Table 2).

Applications

Table 1 The output of oil from raw materials of melon seeds, crushed to a particle size of 10 mm and the content of linoleic acid, oleic acid and palmitic acid, depending on the duration of extraction Example No. Duration of extraction, minutes The yield of oil (in% of dry raw materials) The amount of the main components of the oil (wt.% Of whole oil) linoleic acid oleic acid palmitic acid one twenty 15.4 58.3 16.8 7.7 2 thirty 16.5 60.1 17.5 8.2 3 40 17.1 60.7 18.1 8.6 four fifty 17.5 61.2 18.8 9.1

table 2 The output of oil from the raw materials of melon seeds and the content of linoleic acid, oleic acid and palmitic acid in it, depending on the degree of grinding (extraction time 50 minutes) Example No. The degree of grinding, mm The yield of oil (in% of dry raw materials) The amount of the main components of the oil (wt.% Of whole oil) linoleic acid oleic acid palmitic acid 5 10 15,5 61.35 18.06 8.93 6 7 16.7 61.76 18.58 9.12 7 2 18.2 62.54 19.21 9.83 8 one 18.3 62.63 19.34 9.91 9 0.7 17.1 62.25 19.03 9.87

Table 3 The output of oil from raw materials of melon seeds, crushed to a particle size of 1 mm, and the content of linoleic acid, oleic acid and palmitic acid, depending on the duration of extraction Example No. Duration of extraction, minutes The yield of oil (in% of dry raw materials) The amount of the main components of the oil (wt.% Of whole oil) linoleic acid oleic acid palmitic acid 10 twenty 15.7 59.78 16.76 8.11 eleven thirty 16.9 61.46 17.25 8.74 12 40 17,2 62.15 18.54 9.35 13 fifty 18.3 62.63 19.34 9.91 fourteen 60 17.5 62.34 19.02 9.15

Table 4 The output of oil from raw materials of melon seeds, crushed to a particle size of 1 mm, an extraction time of 50 minutes and the content of linoleic acid, oleic acid and palmitic acid, depending on the pressure Example No. Pressure, atmospheres The yield of oil (in% of dry raw materials) The amount of the main components of the oil (wt.% Of whole oil) linoleic acid oleic acid palmitic acid fifteen 200 16.5 58.03 18.65 8.86 16 300 18.3 62.63 19.34 9.91 17 400 17,2 61.14 18.67 9.05

Table 5 The output of oil from raw materials of melon seeds, crushed to a particle size of 1 mm, an extraction time of 50 minutes and the content of linoleic acid, oleic acid and palmitic acid, depending on temperature Example No. Temperature ° C The yield of oil (in% of dry raw materials) The amount of the main components of the oil (wt.% Of whole oil) linoleic acid oleic acid palmitic acid eighteen 32 16.9 60.85 18.16 8.72 19 40 18.3 62.63 19.34 9.91 twenty 45 17.8 61.09 18.92 9.35

Table 6 The oil yield from the raw material of melon seeds, crushed to a particle size of 1 mm, an extraction time of 50 minutes and the content of linoleic acid, oleic acid and palmitic acid, depending on the flow rate of carbon dioxide Example No. Carbon dioxide flow rate, g / min The yield of oil (in% of dry raw materials) The amount of the main components of the oil (wt.% Of whole oil) linoleic acid oleic acid palmitic acid 21 twenty 15,2 58.28 17.06 8.65 22 thirty 17.6 61.35 18.54 9.27 23 40 18.3 62.63 19.34 9.91 24 fifty 17.8 61.23 19.02 9.54

Table 7 The output of oil from raw materials of melon seeds, crushed to a particle size of 1 mm, an extraction time of 50 minutes depending on the time of collection Example No. Month The yield of oil (in% of dry raw materials) 25 August 15.6 26 September 18.3 27 October 17,2

Table 8 The quantitative composition of oil from melon seeds according to gas chromatography Peak number Exit time, min Content% Identified connection one 4.48 0.11 Dodecanoic acid 2 5.54 0.06 Tetradecanoic acid 3 6.48 0,03 Pentadecanoic acid four 7.24 0.16 Palmitooleic acid 5 7.42 9.91 Palmitic acid 6 8.48 0.09 Margaric acid 7 9.32 62.63 Linoleic acid 8 9.54 19.34 Oleic acid 9 9.57 0.92 6-octadecenoic acid 10 10.18 5.74 Stearic acid eleven 12.27 1.01 7,10,13-eicosatrienic acid

Table 9 The ratio of unsaturated and saturated acids of melon seed oil Unsaturated acids Saturated Acids Palmitoleic acid Dodecanoic acid Linoleic acid Tetradecanoic acid Oleic acid Pentadecanoic acid 6-octadecenoic acid Palmitic acid 7,10,13-eicosatrienic acid Margaric acid Stearic acid 5.27 one

Claims (3)

1. Oil from melon seeds obtained by treating melon seeds collected in September by supercritical fluid extraction with carbon dioxide, using Lada seeds melon seeds dried at 30-35 ° C for 1.0-1.5 hours, crushed to particles with a size of 1.0-2.0 mm, and the extraction is carried out for 50 minutes at a pressure of 300 atmospheres, a temperature of 40 ° C and a flow rate of carbon dioxide of 40 g / min. 2. The oil according to claim 1, comprising as the main component linoleic acid in an amount of 62.63 wt.% And additionally oleic acid 19.34 wt.%, Palmitic acid 9.91 wt.%. 3. The method of producing oil from melon seeds according to claim 1, characterized in that the melon seeds collected in September and dried at 30-35 ° C for 1.0-1.5 hours are ground to a particle size of 1.0- 2.0 mm and carry out supercritical fluid extraction for 50 minutes at a pressure of 300 atmospheres, a temperature of 40 ° C and a flow rate of carbon dioxide of 40 g / min, followed by separation of the oil.

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