RU2550076C2 - Method for production and composition of pumpkin seed oil - Google Patents

Abstract

FIELD: food industry.

SUBSTANCE: invention relates to fat-and-oil industry. Pumpkin seed oil is produced by way of treatment of pumpkin seeds by way of supercritical fluid extraction. Pumpkin seeds are harvested in October; large variety pumpkin seeds are dried at a temperature of 30-35°C during 1.0-1.5 hours and milled into particles sized 1.0-2.0 mm. Extraction is performed during 50 minutes under a pressure of 300 atm at a temperature of 40°C at the rate of carbon dioxide flow equal to 40 g/min. The produced oil includes the base component represented by linoleic acid in an amount of 29.28 wt % and additionally - palmitic acid in an amount of 23.08 wt % and stearic acid in an amount of 7.12 wt %.

EFFECT: invention allows to increase the yield of oil rich in linoleic acid with simultaneous isolation of other biologically active components.

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Description

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

A known method of producing pumpkin seed 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 disadvantages of these methods are that 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.

We found that the grinding of coarse vegetable pumpkin seeds 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 in oil yield when conducting extraction for 50 minutes (table 2), at a pressure of 300 atmospheres (table 4), a temperature of 40 ° C (table 5) and a carbon dioxide flow rate 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 components, decreases (table 3).

Reducing the amount of valuable compounds is a disadvantage of the method of obtaining oil from pumpkin seeds for a longer extraction.

The problem solved by the invention is the production of oil from pumpkin seeds, including linoleic acid, with a higher oil yield and simultaneous extraction of 13 other components besides linoleic acid (drawing). The problem is solved using oil from plant materials, representing pumpkin seeds, including linoleic acid. The oil was obtained by supercritical fluid extraction of dried pumpkin seeds of a large variety, dried at 30-35 ° C for 1.0-1.5 hours, 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. It is preferable to use pumpkin seeds collected in October, since the yield of oil from the seeds during this period is maximum (table 7). Grinding raw pumpkin seeds to a particle size of 1.0-2.0 mm leads to an increase in the yield of oil from pumpkin seeds. Along with linoleic acid, other valuable biologically active components are also extracted, which under other extraction conditions are not extracted in such quantities. Grinding the raw material to a particle size of less than 1.0 mm (0.7 mm) led to a decrease in the oil yield from 22.5% to 19.7% (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 flow rate of carbon dioxide of 40 g / min, allows you to get oil from pumpkin seeds with a higher content and amount 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 components (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 14.6%). When the degree of grinding of raw materials 0.7 mm, the amount of linoleic acid decreases from 28.1% (table 2, example 7) to 21.6% (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 the previously known is that as a raw material used dried at 30-35 ° C for 1.0-1.5 hours, seeds of large pumpkin varieties, collected in October and 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 carbon dioxide flow rate of 40 g / min. The technical result of the proposed solution is to obtain oil from pumpkin seeds, including linoleic acid, with a higher yield with the simultaneous extraction of 13 other biologically active components (table 8). The ratio of unsaturated and saturated acids of oil from pumpkin seeds is shown in table 9.

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

Coarse pumpkin seeds dried at 30-35 ° C for 1.0-1.5 hours and crushed to particle size 1.0-2.0 mm, preferably collected in October, weighing 65 g are poured into a 200 ml supercritical separator extractor brand SFE-500 M1 (company THAR). Plant materials are treated in supercritical 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, followed by separation of the oil.

The chemical composition of the obtained oil samples from pumpkin 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.2. M., 1979. P.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 with a division of 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 the components of the oil from pumpkin seeds is given in wt.%.

Example 1

1,4515-1,4935. Относительная плотность изменялась в пределах $$d_4^{20}$$

0,9033-0,9560. Выход и состав основных компонентов масла приведены в таблице 1.An accurate weighed portion of the raw material (65 g) of pumpkin 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 supercritical extractor brand SFE-500 M1 (company THAR) and carry out extraction in supercritical carbon dioxide for 20 minutes at a pressure of 300 atmospheres, a temperature of 40 ° C and a carbon dioxide flow rate of 40 g / min. The pressure is released to atmospheric pressure, and the oil is collected in the receiver, it is a yellowish-red liquid, the refractive index changed to insignificant limits and is equal to $${\eta }_D^{\mathrm{twenty}}$$

1.4515-1.4935. The relative density varied within $$d_{\mathrm{four}}^{\mathrm{twenty}}$$

0.9033-0.9560. 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 (pumpkin seeds) are 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 pumpkin 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 pumpkin 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 pumpkin 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 pumpkin 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 materials (65 g) of pumpkin 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 pumpkin seeds was made in the month of September (the oil yield is shown in table 7).

Example 26

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

Example 27

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

Thus, in the process of searching for the optimal degree of fineness of raw materials from seeds of pumpkin seeds of a large variety, collected mainly in October, containing linoleic acid, it was found that the optimal use of particles with a size of 1.0–2.0 mm followed by extraction during 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 linoleic acid and rugih biologically active components (Table 2).

Applications

Table 1 The output of oil from raw materials of pumpkin seeds, crushed to a particle size of 10 mm, and the content of linoleic acid, palmitic acid and oleic 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 palmitic acid oleic acid one twenty 12.6 17.3 14.5 14.5 2 thirty 18.2 20.5 12.8 11.3 3 40 20.3 23.8 18.1 12.1 four fifty 22.5 29.28 23.08 15.43

table 2 The output of oil from raw materials of pumpkin seeds and the content of linoleic acid, palmitic acid and oleic 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 palmitic acid oleic acid 5 10 14.6 14.5 10.1 6.3 6 7 15.8 20.3 16,4 9.5 7 2 21.6 28.1 21.5 13.1 8 one 22.5 29.28 23.08 15.43 9 0.7 19.7 21.6 19,4 11,2

Table 3 The output of oil from raw materials of pumpkin seeds, crushed to a particle size of 1 mm, and the content of linoleic acid, palmitic acid and oleic 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 palmitic acid oleic acid 10 twenty 10.8 11.6 8.9 7.7 eleven thirty 17.5 18.2 14.6 9,4 12 40 18.3 25.5 20.1 13,2 13 fifty 22.5 29.28 23.08 15.43 fourteen 60 19.1 27.3 21.5 11.7

Table 4 The output of oil from raw materials of pumpkin seeds, crushed to a particle size of 1 mm, with an extraction time of 50 minutes and the content of linoleic acid, palmitic acid and oleic 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 palmitic acid oleic acid fifteen 200 18.1 22.8 12,4 8.1 16 300 22.5 29.28 23.08 15.43 17 400 20.3 25.6 20.1 11.8

Table 5 The output of oil from raw materials of pumpkin seeds, crushed to a particle size of 1 mm, with an extraction time of 50 minutes and the content of linoleic acid, palmitic acid and oleic 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 palmitic acid oleic acid eighteen 32 15.4 25.6 11,4 14.6 19 40 22.5 29.28 23.08 15.43 twenty 45 17.1 22.5 19.1 10.8

Table 6 The output of oil from raw pumpkin seeds, crushed to a particle size of 1 mm, with an extraction time of 50 minutes and the content of linoleic acid, palmitic acid and oleic 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 palmitic acid oleic acid 21 twenty 10.3 12.1 9.8 6.2 22 thirty 16.7 20.9 16.5 9.7 23 40 22.5 29.28 23.08 15.43 24 fifty 20,2 25.5 15.3 12.3

Table 7 The output of oil from raw pumpkin seeds, crushed to a particle size of 1 mm, with 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 September 19.2 26 October 22.5 27 November 20.7

Table 8 The quantitative composition of oil from pumpkin seeds according to gas chromatography Peak number Exit time, min Content% Identified connection one 5.78 0.42 Myristic acid 2 6.65 0.23 Pentadecyl acid 3 7.35 0.36 Palmitoleic acid four 7.58 23.08 Palmitic acid 5 8.67 0.24 15-methyl palmitic acid 6 9.51 29.28 Linoleic acid 7 9.62 15.43 Oleic acid 8 9.69 1.49 cis-6-octadecenoic acid 9 10.07 7.12 Stearic acid 10 10.53 5.48 9,12-octadecadien-1-ol eleven 12.95 0.33 Arachidonic acid 12 15.27 0.41 Cyclopentantrydecanoic acid 13 15.83 1,11 Genecosanoic acid fourteen 16.31 15.02 Squalene

Table 9 The ratio of unsaturated and saturated acids of pumpkin seed oil Unsaturated acids Saturated Acids Palmitoleic acid Myristic acid Linoleic acid Pentadecyl acid Oleic acid Palmitic acid cis-6-octadecenoic acid 15-methyl palmitic acid Stearic acid Arachidonic acid Cyclopentantrydecanoic acid Genecosanoic acid 1.41 one

Claims (1)

Pumpkin seed oil obtained by treating pumpkin seeds collected in October using supercritical fluid extraction, using coarse pumpkin seeds dried at 30-35 ° C for 1.0-1.5 hours, crushed to particles of size 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, including linoleic acid in the amount of 29.28 wt.% And additionally palmitic acid 23.08 wt.%, stearic acid 7.12 wt.%.

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