KR102112731B1 - Effective manufacture for deodorization of yuja seed oil utilizing natural gardenia jasminoides and Liquorice extract - Google Patents

Abstract

It relates to a method for removing odor from natural citron seed oil by low temperature aging using the natural plant extract of the present invention, the natural plant extract is selected from gardenia flower extract and licorice extract.
The oil and fat of oil obtained according to the method of the present invention does not generate odor due to acid waste, and thus has the advantage of using high-quality citron seed oil for flavoring, functional cosmetic raw materials, organic or eco-friendly materials.

Description

Efficient manufacture for deodorization of yuja seed oil utilizing natural gardenia jasminoides and Liquorice extract

The present invention relates to a method for efficiently removing odors from citron seed oil, and specifically, to a method for removing odor peculiar to citron seed oil by aging the citron seed oil with an extract of a plant.

Citrus junos Tanaka is Citrus junos Tanaka, and belongs to the genus Citrus genus. Origin China is rarely grown in citrons due to climate change, but it is a rare variety among citrus fruits unique to Korea and Japan worldwide. There is a limit to eating right.

Yuzu's scent is very unique and intense compared to other citrus scents, and it is popular with people without special dislikes due to its different flavor from lemon or grapefruit, and is used as a raw material for cosmetics, tea, and food. There is a tendency to manufacture citron seed oil and use it in cosmetic and fragrance treatment (aromatherapy) as a carrier oil.

Yuja seeds have a much higher content of various unsaturated fatty acids than seed oil of other natural plants, and they are used for atopic skin treatment according to traditional folk remedies. It becomes active, increases the production of hyaluronic acid, softens the skin (thickness of the skin layer and dermis layer due to fibroblast proliferation), whitening effect (whitening effect by lipid peroxidation and removal of old keratin), pores It has been reported to be effective in cleaning (the action of dissolving wastes), increasing skin moisturizing and elasticity (preventing skin from roughening), and blocking UV rays and hair care (J of Nutrition and Health, Vol. 47, No. 4,221-228) (2014), Food Science and Industry, Vol. 43, No. 4, 2-13 (2010), The J.of Skin Barrier Research, Vol. 17, No. 2, 36-49 (2015))

Yuja seed oil has a peculiar odor of natural seed oil. Especially, since it exhibits acidity by fatty acids contained in a small amount of oil, acidity occurs over time, so it can be used for cosmetic raw materials or aromatherapy due to the peculiar odor of yuja seed oil. There is a limit to use as a used carrier oil.

As a prior art related to the manufacture and utilization of natural citron seed oil, for example, in patent document 1, a cosmetic composition for alleviating skin irritation caused by a skin irritating raw material is effectively mixed with citron seed and mango seed Disclosed is a cosmetic composition containing oil in an amount of 0.01 to 10% by weight relative to the total weight of the composition, and after coarsely crushing citron seeds in Patent Document 2, 35 to 45 by adding viscozyme and pectinex Enzymatic treatment at 10 ° C. for 10-20 hours (A); After the enzyme treatment, the first wet crushing at 30 ~ 37 ℃, and the second wet crushing at 37 ~ 45 ℃ (B); And (C) after the wet pulverization to obtain a supernatant by centrifugation; It is a complex enzyme containing an agonist, and the pectinex discloses a method for producing citron seed oil with enhanced anti-atherosclerotic activity, characterized in that it is an enzyme having the activity of pectinase and hemicellulase. 1 to 60% by weight of citron seed ferment extract; 1 to 30% by weight of citron seed extract; 1 to 80% by weight of golden extract; And 1 to 60% by weight of a natural preservative containing octagonal fennel extract, but the prior arts are techniques related to the use or use of yuja seed oil and are independent of the technology to remove odor from yuja seed oil and No unique prior literature has been found regarding the technique of removing odors from oil.

Applicants of the present invention completed the present invention by removing the odor peculiar to citron seed generated by acid waste of citron seed oil using a plant extract.

KR 10-1425031 B KR 10-1492470 B KR 10-1532005 B

The problem to be solved in the present invention relates to a method for removing odor from natural citron seed oil, and more specifically, fatty acids contained in the natural citron seed oil are obscured over time, resulting in a characteristic odor of citron seed oil. How to efficiently remove odors from natural citron seed oil using plant extracts to solve the problem of limitations in using it as a carrier oil used in aromatherapy or cosmetic ingredients required by eco-friendly materials or organic materials It is intended to provide.

Method for removing odor from natural citron seed oil as a solution to the problem to be solved according to the present invention is a). First step process of mixing 10-15 parts by weight of gardenia flower extract or licorice extract with respect to 100 parts by weight of natural citron seed oil, and aging at 20 ° C under stirring for 1 to 5 days and b). It consists of a second step of separating the aged yuja seed oil mixed solution of the first step process to obtain the yuja seed oil with the odor removed from the supernatant.

One aspect of the method for removing odor from natural citron seed oil according to the present invention consists in obtaining from a compression method at a temperature condition of 40 to 70 ° C to prevent deterioration of natural citron seed oil.

Another aspect of the method for removing odor from natural citron seed oil according to the present invention is that it is more environmentally friendly by using natural plant extracts and has no odor caused by acid waste, thereby promoting blood circulation of the skin, softening of the skin, and skin whitening effect. It consists of using as raw materials for functional cosmetics and carrier oils used in aromatherapy.

The method of removing odor from natural citron seed oil of the present invention is effective in removing odor at the same time as being eco-friendly by using natural plant extracts.

In addition, the oil and fat obtained according to the method of the present invention does not generate odor caused by acid waste, and thus has the advantage of using high-quality citron seed oil for fragrance, functional cosmetic raw material, organic or eco-friendly material.

1 is a process diagram schematically showing the odor removal process of yuja seed oil using a plant extract according to the present invention
2 is a GC (Gas Chromatography) analysis chart of the raw material of natural citron seed oil

Hereinafter, the present invention will be described in more detail through specific details, examples (manufacturing examples) and test examples for carrying out the present invention, but the present invention is not limited by the following description.

1 is a process diagram schematically showing a process for removing odor of citron seed oil using a plant extract according to the present invention.

As shown in Figure 1, the method of removing odor of yuja seed oil using the plant extract according to the present invention a). First step process of mixing natural citron seed oil with gardenia flower extract or licorice extract and aging at low temperature, and b). It comprises a second step process of phase-separating the aged Yuja seed oil mixed solution of the first step process to obtain the Yuja seed oil from which the odor has been removed from the supernatant.

The natural citron seed oil selected in the first step process according to the present invention is extracted by compressing citron seed at a temperature of 40 to 70 ° C in a conventional manner, and the cold press is cooled at 49 ° C or less to prevent deterioration of the citron seed oil. It is preferred to extract the oil by compression.

The cold pressing method is a well-known method for extracting oil from the seeds of plants and is compressed at 49 ° C. or less, and in the present invention, it is extracted by cold pressing to extract the oil from natural citron seeds without deterioration. Cold presses to which cold presses are applied are widely commercially available.

The gardenia flower extract or licorice extract is composed of a method for conventional hot water extraction, for example, inserting a raw gardenia flower or licorice into a heavy water bath and bathing at 100 ° C. to remove solids, thereby obtaining a gardenia flower extract or a licorice extract.

The low-temperature aging process according to the present invention is a process for neutralizing fatty acids contained in citron seed oil, which causes odor by acid waste according to the passage of period of citron seed oil, and natural citron seed oil and gardenia flower extract or licorice extract The mixture is made of low-temperature maturing under stirring at 20 ° C for 1 to 5 days.

The mixing ratio of the mixture of the citron seed oil and the gardenia flower extract or licorice extract is preferably 10 to 15 parts by weight of the gardenia flower extract or the licorice extract with respect to 100 parts by weight of natural citron seed oil. The acid value is lowered, and there is no acid waste according to the passage of time, so there is no inherent odor of yuja seed oil.

The second step process according to the present invention consists of obtaining the citron seed oil from which the odor has been removed from the supernatant by phase-separation, that is, liquid-liquid separation, of the matured citron seed oil mixture of the first step process.

In the following, the present invention will be described in detail through <Examples>, <Comparative Examples>, and <Test Examples>.

In general, the composition of saturated and unsaturated fatty acids of natural citron seed oil is generally 22.6% of Palmitic Acid (16: 0), 3.8% of Stearic Acid (18: 0), 34.6% of Oleic Acid (18: 1), and Linoleic Acid (18 : 2) 37% and Linolenic Acid (18: 3) 2.1%.

Sample pretreatment methods for analyzing the content of saturated and unsaturated fatty acids in natural citron seed oil in <Example>, <Test Example> and <Comparative Example> of the present invention are as follows [Table 1] GC (Gas Chromatography) analysis conditions Are shown in [Table 2] below.

The compositional content of each component was calculated as the peak area percent of GC (Gas Chromatography) analysis from the standard content calibration curve.

order  Contents One Weigh 25 mg of sample. 2 After adding 1.5 ml of 0.5N Methanolic NaOH, heat it in a heating block at 100 ℃ for 5 minutes. 3 Cool the heated sample in a water bath at 30 ~ 40 ℃ 4 After adding and mixing 2 ml of 14% BF3-Methanol, heat again in a heating block at 100 ℃ for 2 minutes. 5 The heated sample is cooled again in a 30-40 ° C. water bath. 6 Add 2 ml of iso-octane and 1 ml of saturated brine, vortex and leave for 3 minutes. 7 When the layer separation is completed, the upper layer is recovered, and 1 g of sodium-sulfate is added to dehydrate it.

Instrument Agilent GC system 7890B Column Agilent HP-INNOWAX (30m × 0.2㎜, 0.25㎛) Injector 260 ℃ Injection volume 1 μl Split ratio 50: 1 Oven Temperature (℃) Rate (℃ / min) Hold (min) Total (min) One 100 2 2 2 140 4 0 12 3 250 3 20 68.67 Column flow 1ml / min (Constant flow mode) Carrier gas N ₂ H ₂ flow 30ml / min Air flow 300ml / min Detector FID, 260 ℃

And the analysis method and calculation formula of acid value measurement for analyzing the quantitative measure of the cause of acid lung occurrence of citron seed oil selectively used in the present invention are shown in [Table 3] below.

order Contents 0.5 g of sample is precisely weighed and placed in an Erlenmeyer flask. Ethanol: Ether = 1: 2 Add 100 ml of mixed solution to completely dissolve the sample. Add 1 ml of 1% phenolphthalein solution as an indicator. Titrate with 0.1N ethanolic potassium hydroxide solution until the pale red color persists for 30 seconds. formula

S: Sample collection amount (g),
a: Consumption of 0.1N ethanolic potassium hydroxide solution to the sample (ml)
b: Consumption of 0.1N ethanolic potassium hydroxide solution for blank test (ml)
f: Titer of 0.1N ethanolic potassium hydroxide solution

<Example 1>

 <Raw material preparation process>

 100 kg of dried citron seeds are put into a cold press machine (model name: COLD PRESS low-temperature milking machine, manufacturer: National ENG) and chopped juice at a process temperature of 70 ℃, discharge rate of 30 kg / hr and high vacuum to obtain 30 kg of citron seed oil. Did.

In addition, 1 kg of domestic licorice and 9 liters of water were placed in a water bath and extracted at a temperature of 100 ° C for 8 hours to prepare a licorice extract.

a). First stage process (low temperature aging process)

 10 parts by weight of natural licorice extract was mixed with 100 parts by weight of the domestic natural citron seed oil prepared above, put in a low-temperature stirring and aging bath, and aged at a temperature of 20 ° C. for 1 day with low temperature stirring to obtain a aging solution.

b). Second stage process (Yuja seed oil acquisition process)

The aged liquid obtained above was placed in a liquid-liquid separator and left for 2 hours, and then natural citron seed oil was obtained from the supernatant.

<Examples 2 to 5>

 Natural citron seed oil was obtained in the same manner as in <Example 1> except that the aging time was changed to 2 days, 3 days, 4 days, and 5 days, respectively, and then aged at a low temperature.

<Test Example 1>

To test the properties of the licorice extract and the obtained product according to the ripening time, the acid value and components of natural citron seed oil obtained in <Example 1 to Example 5> were analyzed and the results were shown in [Table 4]. It is represented by.

division Aging time <Examples 1 to 5> Raw material 1 day 2 days 3 days 4 days 5 days Mountain 1.92 1.34 0.75 0.1 0.02 0.01 Configuration
ingredient Palmitic Acid (16: 0) 22.7% 22.6% 22.7% 22.7% 22.6% 22.7% Stearic Acid (18: 0) 3.8% 3.8% 3.7% 3.8% 3.8% 3.7%  Oleic Acid (18: 1) 34.6% 34.4% 34.4% 34.5% 34.6% 34.6% Linoleic Acid (18: 2) 37.1% 37.2% 37.1% 37.1% 37% 37.1% Linolenic Acid (18: 3) 2.2% 2.1% 2.2% 2.1% 2.2% 2.2%

As shown in [Table 5], the acid value of citron seed oil continues to decrease as the aging time elapses, based on the raw material (raw citron seed oil), and is significantly reduced to 0.02 or less from day 4 and included in citron seed oil. It can be seen that free fatty acids have been neutralized, and the proportions of the constituents of citron seed oil are almost unchanged within the error range over time of aging. The ratio of saturated fatty acids to unsaturated fatty acids is 26.5%: 73.9%, indicating that the ratio of unsaturated fatty acids is remarkably high.

<Example 6>

<Raw material preparation process>

 1 kg of domestic gardenia flower and 9 liters of water were placed in a water bath and extracted at a temperature of 100 ° C. for 8 hours to prepare a gardenia flower extract.

a). First stage process (low temperature aging process)

 10 parts by weight of the natural gardenia flower extract was mixed with 100 parts by weight of the domestic natural citron seed oil prepared above, put in a low-temperature stirring and aging bath, and aged at a temperature of 20 ° C. for 1 day with low temperature stirring to obtain a aging solution.

 b). Second stage process (Yuja seed oil acquisition process)

 The aged liquid obtained above was placed in a liquid-liquid separator and left for 2 hours, and then natural citron seed oil was obtained from the supernatant.

<Examples 7 to 10>

Natural citron seed oil was obtained by the same method as in <Example 1> except that the aging time was changed to 2 days, 3 days, 4 days, and 5 days, respectively, and then aged at a low temperature.

<Test Example 2>

 To test the properties of the extract from gardenia flower extract and the ripening time, the acid value and components of natural citron seed oil obtained in <Example 6 to Example 10> were analyzed and the results were shown in [Table 5]. ].

division Aging time <Examples 6 to 10> Raw material 1 day 2 days 3 days 4 days 5 days Mountain 1.92 1.71 0.25 0.34 0.11 0.05 Configuration
ingredient Palmitic Acid (16: 0) 22.7% 22.5% 22.7% 22.6% 22.6% 22.6% Stearic Acid (18: 0) 3.8% 3.9% 3.7% 3.7% 3.8% 3.7%  Oleic Acid (18: 1) 34.6% 34.7% 34.4% 34.6% 34.6% 34.6% Linoleic Acid (18: 2) 37.1% 37.1% 37.1% 37.2% 37% 37.1% Linolenic Acid (18: 3) 2.2% 2.2% 2.3% 2.2% 2.2% 2.1%

As shown in [Table 5], the acid value of citron seed oil continues to decrease as the aging time elapses, based on the raw material (raw citron seed oil), and is significantly reduced to 0.11 or less from day 4 and included in citron seed oil. It can be seen that the fatty acids (Free acids) are neutralized, and the proportions of the constituents of citron seed oil are almost unchanged within the error range as in <Test Example 1>. Able to know.

<Comparative Example 1>

 For the comparative test for the present invention, citron in the same manner as in <Example 1> to <Example 5>, except that 10 parts by weight of the extract of the hawthorn extract with hot water extract of hut trees against 100 parts by weight of citron seed oil Each oil was obtained.

In order to test the properties of the obtained product according to the aging time, the acid value and components of natural citron seed oil obtained in <Comparative Example 1> were analyzed and the results are shown in [Table 6] below.

division Aging time <Examples 6 to 10> Raw material 1 day 2 days 3 days 4 days 5 days Mountain 1.92 1.85 1.72 1.65 1.55 1.52 Configuration
ingredient Palmitic Acid (16: 0) 22.7% 22.7% 22.7% 22.6% 22.6% 22.6% Stearic Acid (18: 0) 3.8% 3.8% 3.9% 3.8% 3.9% 3.7%  Oleic Acid (18: 1) 34.6% 34.4% 34.5% 34.5% 34.5% 34.6% Linoleic Acid (18: 2) 37.1% 37.2% 37.1% 37.2% 37.1% 37.1% Linolenic Acid (18: 3) 2.2% 2.2% 2.2% 2.1% 2.1% 2.1%

As shown in [Table 6], it can be seen that the acid value of the obtained product obtained using the extract of oleum tree is significantly higher than the acid value shown in <Test Example 1> and <Experimental Example 2>, so that it differs from the acid waste of citron seed oil. It can be predicted that the odor removal effect is significantly lower than that of the present invention.

<Test Example 3>

<Example 5>, <Example 10> and for comparison of the stability evaluation and sensory evaluation of the natural citron seed oil obtained in <Example 1> to <Example 10> and <Comparative Example 1> of the present invention In <Comparative Example 1>, samples obtained by harvesting 30 ml of each citron oil obtained by low temperature aging for 5 days were placed in a thermostat, and the acid value was measured at 60 ° C for 12 weeks at intervals of 2 weeks to perform stability testing. Sensory evaluation (appearance, odor) was evaluated for each sample after 12 weeks. The results are shown in [Table 7] below.

division Stability test (acid value change) Sensory evaluation results 0 weeks 1 week 4 weeks 6 weeks 8 weeks 10 weeks 12 weeks Example 5 0.01 0.01 0.01 0.01 0.01 0.01 0.01 Appearance: Light yellow, transparent (no change)
Odor: Odorless Example 10 0.05 0.05 0.04 0.04 0.03 0.03 0.03 Appearance: Light yellow, transparent (no change)
Odor: Odorless, slight gardenia Comparative Example 1 1.52 1.19 0.67 0.35 0.27 0.15 0.12 Appearance: White (residue occurs)
Odor: Odor occurs

As shown in [Table 8] above, the natural citron seed oil obtained according to the present invention is not only low in acid value, but also has no change even after elapse, and it is also possible to confirm that the characteristics of the tube and odor are excellent. The natural citron seed oil thus obtained can be predicted to provide high quality citron seed oil as a raw material for fragrance, functional cosmetics, organic or eco-friendly materials.

Claims (5)

a). A mixture of 10 to 15 parts by weight of a gardenia flower extract or licorice extract with respect to 100 parts by weight of natural citron seed oil extracted by squeezing the natural citron seed at 40 to 49 ° C by cold pressing is stirred at 20 ° C for 1 to 5 days 3 A first step process to obtain a neutralized ripening solution with a reduced acid value by neutralizing the fatty acids contained in citron seed oil with a gardenia flower extract or licorice extract by low temperature aging for 5 days,
b). A second step process of phase-separating the neutralized ripening liquid of the first step process to remove fatty acids contained in citron seed oil neutralized with a gardenia flower extract or licorice extract, which is a lower layer liquid, and obtaining citron seed oil from the supernatant Efficient odor removal method of yuja seed oil, characterized in that it comprises a. delete delete delete delete

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