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KR101721747B1 - Purification and Conservation extension method of Zanthoxylum schinifolium oil - Google Patents

Purification and Conservation extension method of Zanthoxylum schinifolium oil Download PDF

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KR101721747B1
KR101721747B1 KR1020150018326A KR20150018326A KR101721747B1 KR 101721747 B1 KR101721747 B1 KR 101721747B1 KR 1020150018326 A KR1020150018326 A KR 1020150018326A KR 20150018326 A KR20150018326 A KR 20150018326A KR 101721747 B1 KR101721747 B1 KR 101721747B1
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colostrum
acidic
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KR20160097396A (en
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강승미
석주환
김종익
김황규
김학곤
최명석
서영롱
임현정
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경상남도
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23DEDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00Other edible oils or fats, e.g. shortenings, cooking oils
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23DEDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00Other edible oils or fats, e.g. shortenings, cooking oils
    • A23D9/02Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
    • A23D9/04Working-up
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23DEDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00Other edible oils or fats, e.g. shortenings, cooking oils
    • A23D9/06Preservation of finished products

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
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  • Fats And Perfumes (AREA)

Abstract

본 발명은 산초유의 불순물을 효과적으로 정제함과 동시에 산패를 방지하여 저장성을 증가시키는 방법에 관한 것이다. 산초유는 착유 후에 정치를 통해 불순물을 제거하지만 이 과정에서 산패가 일어나며, 육안적으로도 침전물 등이 관찰되어 효율적인 정제기술이 요구되고 있다. 또한 산초유는 산패가 급속히 진행되어 안전성에 문제가 발생할 수 있다. 본 발명은 효율적으로 산초유를 단시간에 정제함과 동시에 인체에 안전한 소제를 이용하여 산패를 방지하는 기술을 제공 한다.The present invention relates to a method for efficiently purifying impurities of sancho oil and preventing rancidity, thereby increasing storage stability. Acidic colostrum removes impurities through milking after milking, but rancidity takes place in this process, and sediment and the like are visually observed, and efficient purification technology is required. In addition, acidic colostrum may cause safety problems due to rapid rancidity. The present invention provides a technique for efficiently purifying acidic colostrum in a short time and preventing rancidity by using a safe agent for the human body.

Description

산초유 정제 및 저장성 연장 방법 {Purification and Conservation extension method of Zanthoxylum schinifolium oil}Purification and storage extension method of Zanthoxylum schinifolium oil < RTI ID = 0.0 >

본 발명은 산초유 정제 및 저장성 연장 방법에 관한 것으로, 보다 상세하게는 산초유의 보다 효율적인 정제와 더불어 인체에 안전한 소재를 활용한 산패의 문제점을 극복할 수 있는 산초유 정제 및 저장성 연장 방법에 관한 것이다.The present invention relates to an acidic colostrum refining agent and a preservative elongation method, and more particularly, to an acidic colostrum refining agent and a preservation extender method capable of overcoming the problem of rancidification using a safe material for human body, .

산초(Zanthoxylum schinifolium)는 운향과(Rutaceae)에 속하는 낙엽관목으로 예부터 민간요법에 이용되는 식물자원으로 널리 알려져 있다. 산초나무 열매에서 착유한 산초기름은 기관지, 천식, 위염, 지사제 등으로 이용되었으며, 최근 아토피 개선, 항염증 등의 과학적 효과가 널리 알려지고 있어 향후 산초나무는 유지 작물로 각광받을 것으로 기대되고 있다.
Zanthoxylum schinifolium is a deciduous shrub belonging to the genus Rutaceae and is widely known as a plant resource used for folk medicine since ancient times. In recent years, it has been widely used for bronchial, asthmatic, gastritis, and gastrointestinal tracts, and the scientific effects such as improvement of atopy and anti-inflammation are widely known.

특허등록공보 등록번호 10-1056475호에는 본 발명에서 산초유는 산초나무의 종자를 건조한 후 230~250℃에서 5~10분간 볶은 후에 착유되거나, 산초나무의 종자를 건조한 후 10~20분간 찐 후에 착유된 것을 특징으로 하고, 아울러 본 발명의 아토피 피부 개선용 크림은 산초유를 포함하는 피부 컨디셔닝제 30.0~33.0중량%; 용제 43.0~44.0중량%; 계면활성제 9.0~9.2중량%; 유연제 7.8~8.0중량%; 팽화제 5.6~5.7중량%; 그리고 pH조절제와 천연방부제 0.1~4.6중량%; 의 비율로 혼합하여 제조되는 것을 특징으로 하는 산초유를 함유하는 아토피 피부 개선용 화장품 조성물이 공개되어 있다.
In Patent Registration No. 10-1056475, in the present invention, the colostrum of the present invention is obtained by drying the seeds of Sancho wood, roasting it at 230 to 250 ° C for 5 to 10 minutes and then milking, drying the seeds of the Sancho wood and drying it for 10 to 20 minutes The cream for atopic skin improvement of the present invention is characterized by comprising 30.0 to 33.0% by weight of a skin conditioning agent containing an acidic colostrum; 43.0 to 44.0% by weight of solvent; 9.0 to 9.2% by weight of a surfactant; 7.8 to 8.0 wt% softener; 5.6 to 5.7% by weight of flocculant; 0.1 to 4.6% by weight of a pH adjusting agent and a natural preservative; By weight of an acidic colostrum. The cosmetic composition for improving atopic skin contains an acidic colostrum.

또한, 공개특허공보 공개번호 10-2006-0083915호에는 하기 단계를 포함하는 구강위생용 조성물의 제조방법: Also, in Laid-open Patent Publication No. 10-2006-0083915, there is provided a method for producing an oral care composition comprising the steps of:

(A) 산초나무 (Zanthoxylum schinifolium)의 열매인 산초를 수세하는 단계;(A) washing the sancho, the fruit of Zanthoxylum schinifolium;

(B) 에탄올, 메탄올 및 이들과 물의 혼합물로 이루어진 군으로부터 선택된 용매 100 중량부 당 상기 단계 (A)의 산초 5 내지 25 중량부를 혼합하여 추출하는 단계;(B) mixing and extracting from 5 to 25 parts by weight of an acidic acid of the step (A) per 100 parts by weight of a solvent selected from the group consisting of ethanol, methanol and a mixture thereof with water;

(C) 상기 단계 (B)의 추출액을 여과하여 여액을 회수하는 단계;(C) filtering the extract of step (B) to recover the filtrate;

(D) 상기 단계 (C)의 여액으로부터 용매를 제거하여 산초 추출물을 회수하는 단계; 및(D) removing the solvent from the filtrate in the step (C) to recover an acnes extract; And

(E) 통상의 구강위생제품에 상기 단계 (D)의 산초 추출물 0.01 내지 5 중량%를 첨가하는 단계를 포함하는 산초 추출물을 함유하는 구강위생용 조성물 및 그 제조방법이 공개되어 있다.
(E) 0.01 to 5% by weight of a sancho extract of the step (D) in an ordinary oral hygiene product is added to an oral hygiene product and a preparation method thereof.

그러나 상기 종래의 식물유지는 가공, 조리 및 저장 중에 일어나는 변화로 그 이용성이 제한되고 있다. 일반적으로 식물성 유지는 착유방법, 저장기간에 따라 산화가 진행되고 이와 같은 변화는 유해물질을 발생시켜 식품위생에 엄청난 문제점을 야기할 수 있다. 산패 (rancidity)는 지방질 식품이 가공 및 저장 중에 화학적, 미생물학적인 각종 요인에 의해 냄새와 맛이 변화하고 영양적 가치가 손실되는 등의 품질이 저하되는 현상이다. 따라서 산초유는 민간에서 오래전부터 이용되어져 왔으나 정제법, 저장법 등이 과학적으로 구명이 되어 있지 않아 유통 및 이용에 문제를 야기할 수 있다.  However, the above conventional vegetable oils have been limited in their availability due to changes occurring during processing, cooking and storage. Generally, the vegetable oil is oxidized according to the milking method and the storage period, and such change may cause harmful substances, which may cause great problems in food hygiene. Rancidity is a phenomenon in which the quality of fatty foods is degraded during processing and storage due to various chemical and microbiological factors such as changes in smell and taste and loss of nutritional value. Therefore, it has been used in the civilization for a long time, but the refining method and the storage method are not scientifically known, which can cause problems in distribution and use.

산초유는 불포화지방산의 함량이 높아 유지의 산패가 일어나기 쉽고, 착유된 산초유는 색이 투명하지 못하고, 불순물 등이 다량 함유되어 있다. 이러한 불순물은 산초유의 저장 과정에서 산패요인을 작용할 수 있다. 일반적으로 유지의 정제는 탈검(degumming)과정과 탈산(neutralization)과정을 거친다. 탈검과정은 유지에 녹아 있는 인지질(lecithin)을 제거하는 방법이며, 탈산과정은 원유 중의 유리지방산을 알칼리 수용액(NaOH)으로 중화하여 제거하는 동시에 공존하는 인지질(lecithin), 점질물, 색소 등도 함께 제거한다. 이러한 과정은 보편적으로 행하여지고 있으나 유지종류에 따라 각기 다른 조건이 요구된다. 산초유는 민간에서 오랫동안 이용되어져 왔으나 정제법이 개발되어 있지 않다.The acidic colostrum has a high content of unsaturated fatty acids, so that the acidity of the oil is likely to occur, and the milked colostrum is not transparent in color and contains a large amount of impurities. These impurities may act as a rancid factor during the storage process of the acid plant. In general, the purification of the oil is subjected to a degumming process and a neutralization process. The deoxidation process removes the lecithin dissolved in the fat. In the deoxidation process, the free fatty acid in the crude oil is neutralized with an aqueous alkaline solution (NaOH), and the coexisting phospholipids (lecithin), viscous substance and pigment are also removed . This process is commonly performed, but different conditions are required depending on the type of maintenance. Acidic colostrum has long been used in the private sector, but no purification method has been developed.

또한 산초유는 민간에서 오랫동안 이용되어져 왔지만 산패에 민감한 특징을 가지고 있지만 이를 방지할 수 있는 방법이 개발되어 있지 않다. 유지 등의 저장성을 증대시키기 위해서는 항산화제 등이 제안되고 있으나 합성항산화제는 인체 안전성 등이 문제가 되고 있어, 인체 안전성이 보장되는 소재의 탐색이 요구되고 있다.In addition, acidic colostrum has long been used in the private sector, but it is susceptible to rancidity, but no method has been developed to prevent it. Antioxidants and the like have been proposed to increase the storage stability of oils and fats, but synthetic antioxidants have been problematic in terms of human safety and the like.

따라서 본 발명은 상기와 같은 문제점을 해결하고자 안출된 것으로서, 본 발명은 산초유를 탈검 탈산 처리하여 인지질과 유리지방산 등을 효율적으로 정제하고, 나아가 중탄산나트륨을 첨가하여 산패를 줄일 수 있는 방법을 제공하는데 그 목적이 있다.DISCLOSURE OF THE INVENTION Accordingly, the present invention has been made to solve the above-mentioned problems, and it is an object of the present invention to provide a method of deoxidizing acidic colostrum to efficiently purify phospholipids and free fatty acids, and further, to reduce rancidity by adding sodium bicarbonate It has its purpose.

본발명은 산초유 정제 및 저장성연장 방법에 관한 것으로, 인산을 혼합하여 산초유를 탈검하여 정제하고 저장성을 연장하게 되는 것을 특징으로 한다.The present invention relates to an acidic colostrum refining agent and a preservation extendable method, wherein the acidic colostrum is defatted by mixing phosphoric acid to purify and extend shelf life.

상술한 바에 따르면, 탈검과 탈산은 산초유의 상품성을 높여줄 수 있으며, 중탄산나트륨은 산초유의 산패를 방지해 줄 수 있다. 특히 탈검 및 탈산법과 중탄산나트륨 첨가는 산초유의 저장과 유통에 크게 도움을 줄 수 있을 것이다. 나아가 저장성이 향상된 산초유는 건강기능성 식품 제조, 기능성 음료, 의약품 소재로도 적의 이용될 수 있다. According to the above, the defection and deoxidation can increase the commerciality of the sancho oil, and the sodium bicarbonate can prevent the acidosis of the sancho oil. Especially, the addition of deoxidation and deoxidation and the addition of sodium bicarbonate can greatly contribute to the storage and distribution of the acidolide. Furthermore, the preserved acidic colostrum can be used as an ingredient of health functional foods, functional beverages, and pharmaceuticals.

도 1은 압착산초유의 정치일수에 따른 산가변화 및 탁도의 변화를 의미한다.
도 2는 인산 처리에 따른 산초유의 인산함량을 나타낸 것이며,
도 3은 수산화나트륨 처리에 따른 산초유의 산가변화를 나타낸 것이며,
도 4는 수산화나트륨 처리에 따른 산초유의 불포화 지방산의 함량 변화를 나타낸 것이며,
도 5는 정제공정에 따른 산초유의 불포화 지방산 변화를 나타낸 것이며,
도 6은 탈검 및 탈산에 따른 색차, 폴리페놀함량, 항산화활성 변화를 나타낸 것이며,
도 7은 중탄산나트륨의 사용과 저장일수에 따른 산초유의 산가변화변화를 나타낸 것이다.
Fig. 1 shows changes in acid value and turbidity depending on the number of days of squeezed sancho oil.
FIG. 2 shows the content of phosphoric acid in the acidic acid according to the phosphoric acid treatment,
FIG. 3 shows the change of the acid value of the sancho oil by sodium hydroxide treatment,
Fig. 4 shows changes in the content of unsaturated fatty acids in the acidolide according to sodium hydroxide treatment,
FIG. 5 shows changes in unsaturated fatty acids of the oil of Sancho oil according to the purification process,
FIG. 6 shows changes in color difference, polyphenol content, and antioxidative activity caused by defection and deoxidation,
FIG. 7 shows changes in the acid value change of the acidic acid with use of sodium bicarbonate and storage days.

본 발명은 인산을 혼합하여 산초유를 탈검하여 정제하고 저장성을 연장하게 되는 산초유 정제 및 저장성 연장 방법에 있어서, 상기 산초유에는 인산과 함께 초산을 더 혼합하는 것으로, 산초유 99.4 ~ 99.9중량% , 인산 0.05 ~ 0.3중량%, 초산 0.05 ~ 0.3중량%의 혼합비로 혼합하고, 상기 인산을 혼합하여 탈검 정제된 산초유에 수산화나트륨(NaOH)을 더 혼합하여 추가로 불순물을 정제하고 저장성을 연장하되, 상기 수산화나트륨(NaOH)을 1~3N의 농도로 혼합하며, 상기 인산을 혼합하여 탈검 정제된 산초유에 중탄산나트륨을 더 추가하여 산패를 지연하는 것으로, 상기 중탄산나트륨은 전체중량의 0.5~2중량% 농도로 투입하고, 25±2℃ 온도 상태에서 암상태로 두면서 산초유의 산패를 방어하는 것을 특징으로 한다.The present invention relates to an acidic colostrum refining agent and a shelf life extension method for refining acidic colostrum by defatting acidic colostrum to improve its shelf life, wherein the acidic colostrum is further mixed with phosphoric acid and acetic acid, wherein 99.4 to 99.9% 0.05 to 0.3% by weight of phosphoric acid and 0.05 to 0.3% by weight of acetic acid, mixing the above-mentioned phosphoric acid and further adding sodium hydroxide (NaOH) to the defatted and purified acidic colostrum to further purify impurities, , Sodium hydroxide (NaOH) is mixed at a concentration of 1 to 3N, sodium phosphate bicarbonate is added to the defatted and purified acidic colostrum by mixing the phosphoric acid, and the sodium bicarbonate is added in an amount of 0.5 to 2 By weight, and the mixture is kept in a dark state at a temperature of 25 占 占 폚 to defend against acid rancidity.

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본발명을 첨부도면에 의해 상세히 설명하면 다음과 같다. 도 1은 압착산초유의 정치일수에 따른 산가변화 및 탁도의 변화를 의미한다. 도 2는 인산 처리에 따른 산초유의 인산함량을 나타낸 것이며, 도 3은 수산화나트륨 처리에 따른 산초유의 산가변화를 나타낸 것이며, 도 4는 수산화나트륨 처리에 따른 산초유의 불포화 지방산의 함량 변화를 나타낸 것이며, 도 5는 정제공정에 따른 산초유의 불포화 지방산 변화를 나타낸 것이며, 도 6은 탈검 및 탈산에 따른 색차, 폴리페놀함량, 항산화활성 변화를 나타낸 것이며, 도 7은 중탄산나트륨의 사용과 저장일수에 따른 산초유의 산가변화변화를 나타낸 것이다.
The present invention will be described in detail with reference to the accompanying drawings. Fig. 1 shows changes in acid value and turbidity depending on the number of days of squeezed sancho oil. FIG. 2 shows the phosphoric acid content of the acidophilic acid according to the phosphoric acid treatment, FIG. 3 shows the acid value change of the acidic acid with the sodium hydroxide treatment, FIG. 4 shows the content of the unsaturated fatty acid in the acidic acid according to the sodium hydroxide treatment, FIG. 5 shows changes in unsaturated fatty acids of the acidosis oil according to the purification process. FIG. 6 shows the change in color difference, polyphenol content and antioxidant activity due to the elimination and deoxidation. FIG. And the change in the acid value change.

본 발명의 1견지에 의하면, 산초유에 포함되어 있는 다양한 불순물 들을 효율적으로 정제하는 방법이 제공된다.
According to one aspect of the present invention, a method for efficiently purifying various impurities contained in an acidic colostrum is provided.

또한, 본 발명의 2견지에 의하면, Further, according to two aspects of the present invention,

식품 등에 널리 사용되는 중탄산나트륨의 처리는 산패를 방지할 수 있는 방법이 제공된다.
The treatment of sodium bicarbonate, which is widely used in foods and the like, provides a method of preventing rancidity.

이하, 본 발명에 대하여 구체적으로 설명한다.
Hereinafter, the present invention will be described in detail.

우선, 산초유를 착유하고 나서 불순물을 제거하기 위해 실온에 정치하는데 이 과정에서 발생하는 산초유의 산패도와 탁도의 변화를 측정하였다. 이후 탈검 탈산법으로 산초유를 효과적으로 정제하는 조건을 조사하였다.First, after milking the colostrum, it was allowed to stand at room temperature to remove impurities, and the changes in the acidity and turbidity of the acidophilus caused by the process were measured. The conditions for effectively purifying the acidic colostrum by deacidification were investigated.

탈검은 0.05-0.3중량%의 인산을 산초유와 적정 비율로 혼합하고, 정제효율을 조사하였다.        0.05-0.3% by weight of phosphoric acid was mixed with the acidic colostrum in a proper ratio and the purification efficiency was investigated.

또한, 1-3N 농도의 수산화나트륨을 이용하여 불순물을 효과적으로 제거하는 적정농도를 조사하였다. 탈검 및 탈산 공정을 통하여 정제효율과 더불어 포화 및 불포화지방산, 폴리페놀, 항산화활성과 색차를 조사하였다.       In addition, an appropriate concentration for effectively removing impurities was examined using sodium hydroxide of 1-3 N concentration. The effect of purification and unsaturated fatty acid, polyphenol, antioxidant activity and color difference were investigated through the deionization and deoxidation process.

마지막으로 산패를 지연 또는 방어하기 위한 적정소재로 중탄산나트륨을 0.5, 1.0, 2 중량% 농도로 투입하고 산패지연 여부를 조사한다.Finally, sodium bicarbonate is added at 0.5, 1.0, and 2 wt% concentration as a suitable material to retard or prevent rancidity, and the rancidity is investigated.

그 결과 인산을 이용한 탈검공정, 수산화나트륨을 이용한 탈산공정은 산초유를 보다 효율적으로 정제할 수 있음을 확인하였다. 또한 산패가 급속히 진행되어 저장 등의 문제점이 있는 산초유의 산패방지에 중탄산나트륨이 매우 효과가 있음을 입증하였다.
As a result, it was confirmed that deoxidation process using phosphoric acid and deoxidation process using sodium hydroxide can purify acid colostrum more efficiently. In addition, it proved that sodium bicarbonate is very effective for prevention of sickness rancidity, which causes problems such as storage and so on.

이하, 실시 예를 통하여 본 발명의 정제방법 및 소재가 산초유의 불순물 정제 및 산패를 강력하게 억제하는 방법을 구체적으로 설명한다. 이는 본 발명의 실시 예일 뿐, 본 발명을 이에 한정하려는 것은 아니다.
Hereinafter, the purification method and the material of the present invention will be described in detail by way of examples, with reference to the method of strongly suppressing impurity purification and acid corrosion of the acid pickling oil. It is to be understood that the present invention is not limited thereto.

[실시예 1] 산초유의 정치에 따른 산가 및 탁도 측정 시험 [Example 1] Test of acid value and turbidity according to the politics of Sancho

본 발명에 사용된 산초유는 경남 하동 A농장에서 생산된 산초종자를 착유하여 사용하였다. The acidic colostrum used in the present invention was obtained by milking onion seeds produced in Hadong A farm in Gyeongnam Province.

전통방법으로 산초유는 채유 후 실온에 정치하여 불술물을 침전시킨다. In the traditional method, the colostrum is left at room temperature after oil extraction to precipitate the fluoride.

본 발명에서는 이 과정에서 산가 및 탁도변화를 알아보기 위해 압착 착유한 산초유를 25℃에서 7일간 정치해두고 산가 및 탁도를 측정하였다.In the present invention, in order to investigate changes in acid value and turbidity in the process, compressed colostrum oil was allowed to stand at 25 DEG C for 7 days and acid value and turbidity were measured.

본 발명에서 산초유의 산가측정은 AOAC (1984)의 방법으로 행하였다. 100 ml 삼각플라스크에 에테르:에탄올 (2:1, v/v) 혼합물 20 ml와 1% 페놀프탈레인 17 μl를 넣고 0.1 N KOH를 이용하여 적정하여 공실험의 KOH의 적정량을 구하였다. 그 다음 전자저울 위에 100 ml의 삼각플라스크를 올려 놓고 영점을 맞춘 후 측정할 산초유 시료 1g을 첨가하고, 에테르:에탄올 (2:1, v/v) 혼합물을 20 ml 첨가하여 시료를 완전히 용해시킨 다음 0.1 N KOH를 이용하여 적정하여 실험군의 적정량을 구하였다. KOH의 역가는 안식향산 0.2∼0.3 g을 이용하여 표정하여 구하였다 (식 1). 적정시 종말점은 선홍색이 1분간 유지되는 KOH 적정량으로 하였고, KOH 적정량을 이용하여 산초유의 산가를 조사하였다 (식 2).
In the present invention, the measurement of the acid value of the sancho oil was carried out by the method of AOAC (1984). 20 ml of a mixture of ether: ethanol (2: 1, v / v) and 17 μl of 1% phenolphthalein were added to a 100 ml Erlenmeyer flask and titrated with 0.1 N KOH to determine the amount of KOH in the experiment. Then, a 100 ml Erlenmeyer flask was placed on the electronic balance, zero point was added, and 1 g of an acidic colostrum sample to be measured was added. 20 ml of an ether: ethanol (2: 1, v / v) mixture was added to completely dissolve the sample Next, titration was performed using 0.1 N KOH to determine the appropriate amount of the experimental group. The backwash of KOH was calculated by using 0.2-0.3 g of benzoic acid (Equation 1). When the titration was proper, the amount of KOH was maintained at the end point for 1 minute, and the acid value of the acid was measured using the KOH titration amount (Equation 2).

Figure 112015012734928-pat00001

Figure 112015012734928-pat00001

그 결과 산초유는 침전물을 가라앉히기 위해서 상온에서 정치하는 일수가 증가할수록 산초유의 산가는 증가하는 경향을 보였고, 탁도는 반대로 감소하는 것으로 나타났다(도 1). As a result, the acidity of acidified colostrum showed a tendency to increase with increasing number of days of incubation at room temperature in order to sediment the precipitate, and the turbidity decreased inversely (Fig. 1).

산초유의 산패를 방지하기 위해 저온에서 정치시킨다 할지라도 산초유의 점도가 증가함으로 불순물을 제거하는데 어려움이 있었다. 따라서 산초유를 효율적으로 정제할 수 있는 방법의 개발이 필요한 것으로 조사되었다.
Even if it is allowed to stand at a low temperature in order to prevent the acid corrosion of the acidic acid, it is difficult to remove the impurities because the viscosity of the acidic acid oil is increased. Therefore, it is necessary to develop a method to efficiently purify acidic colostrum.

[실시예 2] 탈검 및 탈산공정에 따른 산초유의 정제 시험 [Example 2] Purification test of Sansho oil according to defection and deoxidation process

A. 산초유의 탈검 시험A. Test for pickling of the pickles

100g의 산초유를 정량한 다음 인산과 초산 각각 0.05-0.3중량%까지 0.05중량%의 간격으로 10 ml 투입한 다음 아래의 탈검효과 검정방법에 따라 그 효율을 측정하였다. 상기 초산은 인산과 병행하여 사용하는 것으로, 유지내 불순물, 특히 단백질 및 인지질의 제거효과가 크다.100 g of colostrum was quantified, and then 10 ml of 0.05% by weight of 0.05-0.3% by weight of phosphoric acid and acetic acid was added at intervals of 10% by weight, and the efficiency was measured according to the following method. The acetic acid is used in parallel with phosphoric acid and has a large effect of removing impurities in the fat, especially protein and phospholipid.

5N 황산, 0.01M potassium antimonyl tatarate, 4% ammonium molybdate, 1M ascorbic Acid를 각각 제조하여 혼합시약을 제조하였다. 혼합시약은 50 ml of 5N sulfuric acid, 5 ml potassium antimonyl tartarate. 15 ml ammonium molybdate. 30 ml ascorbic acid을 혼합하여 총 100 ml을 제작한 다음 산초유를 5 ml 정량하여 혼합시약을 0.8 ml 투입하여 혼합하였다. 그 다음 30분간 정치하고, 2 ml의 95% 에탄올을 투입하여 vertexing 한 후 880 nm 자외선분광계에서 흡광도를 측정하였다. 인산의 standard 검량선은 KH2PO4를 이용하여 혼합시약 0.8 ml을 넣고 30분간 정치 후 2 ml의 95% 에탄올을 혼합하여 vertexing한 다음 880 nm에서 흡광도를 측정하여 총 인산의 함량을 구하였다. 이때 유효인산의 standard curve는 y=0.007x+0.0119, R2=0.9989이었다. 5N sulfuric acid, 0.01M potassium antimonyl tatarate, 4% ammonium molybdate and 1M ascorbic acid were prepared, respectively. 50 ml of 5N sulfuric acid, 5 ml of potassium antimonyl tartrate. 15 ml of ammonium molybdate. 30 ml of ascorbic acid was added to make 100 ml of total ascorbic acid, then 5 ml of colostrum was mixed with 0.8 ml of mixed reagent. Then, the mixture was allowed to stand for 30 minutes, and 2 ml of 95% ethanol was added thereto for vertexing, and the absorbance was measured by an 880 nm ultraviolet spectrometer. The standard calibration curve of phosphoric acid was prepared by adding 0.8 ml of the mixed reagent with KH 2 PO 4 and incubating for 30 minutes. Then, 2 ml of 95% ethanol was mixed and the total phosphoric acid content was determined by measuring the absorbance at 880 nm. The standard curve for effective phosphoric acid was y = 0.007x + 0.0119 and R 2 = 0.9989.

그 결과, 산초유의 탈검공정에 있어서 인산을 사용하였을 때 인산의 농도가 0.15중량%까지는 농도의존적으로 탈검효율이 증가하였으나, 0.2중량% 처리구에서는 그 효율이 감소하는 것으로 나타났다(도 1). 또한 0.2중량% 농도 이상의 인산을 사용하였을 때 산초유의 탈검 효율은 0.2중량% 처리구보다 감소하였으나, 그 이상의 농도에서는 탈검 효율은 좋아지지 않았다. 탈검효율이 가장 높은 인산의 농도는 0.15중량%로 사용하였을 때 나타났으며, 그 효율은 약 72.5%였다.
As a result, when the phosphoric acid was used in the deoxidation process of the acid pickling, the efficiency of the deodorization was increased in a concentration dependent manner up to the concentration of 0.15 wt%, but the efficiency decreased in the treatment of 0.2 wt% (FIG. In addition, when phosphoric acid concentration of 0.2 wt% or more was used, the efficiency of delicacy of the soybean paste was lower than that of 0.2 wt% treatment. The highest concentration of phosphoric acid was found to be 0.15 wt%, and the efficiency was about 72.5%.

B. 산초유의 탈산 시험B. Deoxidation test of Sancho oil

100g의 산초유를 정량한 다음 수산화나트륨(NaOH)을 1-3N의 농도로 하여 수율 및 산가에 효율적인 수산화나트륨 농도를 구명하였다. 이때 처리해주는 수산화나트륨의 농도는 0.2-1%이었다. 수산화나트륨을 투입한 산초유는 80℃의 수욕조에서 10분간 반응시킨 후 유리막대를 이용하여 저어가며 30분간 더 반응시킨 다음 정제 과정에 따른 변화를 측정하였다. 100 g of colostrum was quantitatively determined, and sodium hydroxide (NaOH) was added at a concentration of 1-3 N to determine the concentration of sodium hydroxide effective for yield and acid value. At this time, the concentration of sodium hydroxide to be treated was 0.2-1%. The acidic colostrum containing sodium hydroxide was reacted in a water bath of 80 ℃ for 10 minutes, then stirred with a glass rod for 30 minutes, and then the change was measured by the purification process.

그 결과, 수산화나트륨을 이용한 산초유의 탈산효과는 수산화나트륨 농도와 투입량에 비례하여 증가하였다 (도 3). 가장 탈산이 효율적으로 이루어지는 농도와 그 양은 2N, 1%로 약 50%의 정제 효율을 보였다. 이것은 1N의 NaOH 1%를 사용했을 때의 탈산효과와 비교하여 매우 큰차이가 나고1N NaOH보다 낮은 농도 및 투입량에선 탈산의 효과가 없는 것으로 나타나기 때문이다. 또한 3N의 NaOH 1%를 사용했을 때는 2N NaOH, 1%를 투입하였을 때보다 탈산효과의 차이가 크게 나지 않는다는 결과에 기인한 것이다. (도 3). 수산화나트륨의 투입량에 비례하여 고형물의 양도 증가하였다. 탈산효과가 가장 높았던 2N 수산화나트륨을 1%을 사용하였을 때 그 발생량은 약 15 ml로 나타났다.As a result, the deoxidation effect of the hydrogen peroxide using sodium hydroxide was increased in proportion to the sodium hydroxide concentration and the amount of the input (FIG. 3). The most effective concentration of deoxidation was 2N, 1%, and about 50% purification efficiency. This is because there is a big difference compared with the deoxidation effect when 1N NaOH 1% is used and it shows that deoxidation is not effective at lower concentrations and doses than 1N NaOH. In addition, when 1N NaOH 3N was used, the difference in deoxidation effect was not significantly different from when 2N NaOH and 1% were added. (Fig. 3). The amount of solids increased in proportion to the amount of sodium hydroxide added. When 1% of 2N sodium hydroxide, which had the highest deoxidation effect, was used, the yield was about 15 ml.

한편, 탈산처리에 따라서 불포화지방산, 포화지방산의 함량 차이를 보였다 (도 4). 불포화지방산인 oleic acid(18:1), linoleic acid(18:2), linolenic acid(18:3)의 함량은 수산화나트륨 농도가 10 ppm일 때 가장 큰 감소율을 보였다 (도 4). 그 비율은 각각 52.5중량%, 59.4중량%, 56.8중량%로 palmitic acid(14:1)와 palmitoleic acid(16:1)와 비교하여 약 10중량%이상 감소하였다. 하지만 수산화나트륨 농도가 10 ppm이상에서는 다른 불포화 지방산의 함량이 감소하는 것과 달리 oleic acid(18:1)의 함량은 타 수산화나트륨 처리군에 비하여 증가하는 경향을 보였다.
On the other hand, the contents of unsaturated fatty acids and saturated fatty acids were different according to the deoxidation treatment (FIG. 4). The contents of unsaturated fatty acids such as oleic acid (18: 1), linoleic acid (18: 2) and linolenic acid (18: 3) showed the largest reduction rate at 10 ppm sodium hydroxide concentration (Fig. The proportions were 52.5 wt%, 59.4 wt% and 56.8 wt%, respectively, and decreased by about 10 wt% or more compared with palmitic acid (14: 1) and palmitoleic acid (16: 1). However, the content of oleic acid (18: 1) tended to be higher than that of the sodium hydroxide treatment, while the content of other unsaturated fatty acids was decreased at a sodium hydroxide concentration of more than 10 ppm.

C. 정제 산초유의 색도, 폴리페놀함량, 항산화활성 변화시험C. Test for change in color, polyphenol content and antioxidant activity of purified pepper powder

탈검 및 탈산 처리된 산초유는 색도, 산가, 폴리페놀함량, 항산화활성, 지방산함량을 분석하였다(도 6). The acidity, acid value, polyphenol content, antioxidant activity, and fatty acid content of the deacidified and deoxidized acidic colostrum were analyzed (Fig. 6).

그 결과 색차는 탈검 및 탈산 과정을 거치면서 원유에 비해 급격히 낮아지는 것으로 나타났다. 이는 탈검 및 탈산공정을 통해 정제가 진행된 것을 의마한다. 폴리페놀 함량은 탈검 및 탈산공정을 통해 급격히 감소하였다. 그러나 항산화활성은 크게 변하지 않았다.As a result, the color difference was drastically lowered than that of crude oil through the defection and deoxidation process. This suggests that the purification has proceeded through the de-oxidation and de-oxidation processes. The content of polyphenols decreased sharply through deionization and deoxidation process. However, antioxidant activity did not change significantly.

이상과 같은 탈검 및 탈산 과정을 통해 산초유는 불포화지방산, 항산화 활성 등에 큰 손실을 주지 않으면서도 시각적으로도 좋은 산초유를 효율적으로 정제할 수 있다.
Through the above-described defection and deoxidation process, the acidic colostrum can efficiently purify the viscous acidic colostrum without giving great loss to the unsaturated fatty acid and the antioxidative activity.

[실시예 2] 중탄산나트륨 처리에 의한 산패방지 효과 실험 [Example 2] Experiment on prevention of rancidity by treatment with sodium bicarbonate

A. 중탄산나트륨 적정 농도 탐색 실험A. Saturation test of sodium bicarbonate

30g의 정제공정을 거친 산초유를 50 ml conical tube에 넣고, 다시 중탄산나트륨(NaHCO3)을 0.5, 1.0, 2% 농도로 투입하고, 25±2℃, 암상태로 5일 간격으로 30일간 산패도를 측정하였다. 30 g of purified colostrum was placed in a 50 ml conical tube and sodium bicarbonate (NaHCO 3 ) was added at a concentration of 0.5, 1.0, and 2%, and the mixture was incubated at 25 ± 2 ° C for 30 days Respectively.

그 결과, 탈검공정을 거치지 않은 산초유를 저온에 두었을 때 산가는 점차적으로 증가하는 반면 중탄산나트륨을 첨가한 산초유의 산가는 지속적으로 낮아지는 것으로 나타났다(도 7). 따라서 중탄산나트륨은 산초유의 산패를 지연하는 소재임을 알 수 있다. As a result, the acidity gradually increased when the uncoloured acidic colostrum was placed at a low temperature, while the acid value of the acidic acid added with sodium bicarbonate gradually decreased (FIG. 7). Therefore, it can be seen that sodium bicarbonate is a material delaying the acidosis of Sancho.

탄산수소나트륨은 속칭, 중탄산소다의 약칭이며, 무색의 결정이다. 물 100g에 대한 용해도는 8.8g(15℃)이고, 수용액은 가수분해하기 때문에 약알칼리성이 되며, 65℃ 이상으로 가열하면 CO2를 방출하여 탄산나트륨이 된다. 제산제로 가장 널리 사용된다. 백색의 분말이고 특유한 맛이 있다. 약알칼리성, 위내에서 위산을 중화하고 탄산가스를 발생한다. 이 탄산가스에 의해 위는 정당히 충혈되어 흡수력이 높아지는데 위가 팽만하고 트림이 나오는 수가 있다. 위산과다, 명치언저리의 쓰림, 구토 등에 유효한데, 위에 불쾌한 팽만감을 주거나 이차적으로 위산분비를 촉진하거나 하는 결점이 있다. 이것은 탄산염에 공통이다. 또한 베이킹 파우더, 수화(消火)제 등에 사용된다. Sodium bicarbonate is an abbreviation for sodium bicarbonate, and is a colorless crystal. Solubility in 100 g of water is 8.8 g (15 ° C). The aqueous solution becomes slightly alkaline due to hydrolysis. When heated above 65 ° C, it releases CO 2 and becomes sodium carbonate. It is most widely used as antacid. It is a white powder and has a distinctive taste. It is weakly alkaline, neutralizes stomach acid in the stomach and generates carbon dioxide gas. By this carbon dioxide gas, the stomach is properly congested and the absorption power is increased, but the stomach is swollen and the trim may come out. Gastric hyperplasia, soreness and vomiting of the mandible, but it has a drawback that it gives an unpleasant bloat on the stomach or secondary gastric acid secretion. This is common to carbonates. It is also used for baking powders, fire extinguishers and the like.

중탄산나트륨의 사용은 식품공전 상의 제약이 없으면서도 위해하지도 않은 장점이 있어 산초유의 저장 및 유통에 크게 도움이 될 것으로 기대된다.The use of sodium bicarbonate is expected to be very helpful for the storage and distribution of acid oil because it has the advantage of not having any restriction on food circulation and also not having to do it.

Claims (8)

인산을 혼합하여 산초유를 탈검하여 정제하고 저장성을 연장하게 되는 산초유 정제 및 저장성 연장 방법에 있어서,
상기 산초유에는 인산과 함께 초산을 더 혼합하는 것으로,
산초유 99.4 ~ 99.9중량% , 인산 0.05 ~ 0.3중량%, 초산 0.05 ~ 0.3중량%의 혼합비로 혼합하여 탈검 정제하여, 유지내 불순물인 단백질 및 인지질을 제거한 후, 상기 탈검 정제된 산초유에 수산화나트륨(NaOH)을 더 혼합하여 추가로 불순물을 정제하고 저장성을 연장하되,
상기 수산화나트륨(NaOH)을 1~3N의 농도로 혼합하며,
상기 탈검 정제되어 불포화지방산, 항산화 활성에 손실을 주지 않으면서도 시각적으로 좋게된 산초유에 중탄산나트륨을 더 추가하여 산패를 지연하는 것으로,
상기 중탄산나트륨은 전체중량의 0.5~2중량% 농도로 투입하고, 25±2℃ 온도 상태에서 암상태로 두면서 산초유의 산패를 방어하는 것을 특징으로 하는 산초유 정제 및 저장성 연장 방법
The present invention relates to a method for purifying an acidic colostrum by mixing phosphoric acid,
The acetic acid is further mixed with phosphoric acid in the acidic oil,
The mixture is mixed at a mixing ratio of 99.4 to 99.9% by weight of acidic colostrum, 0.05 to 0.3% by weight of phosphoric acid and 0.05 to 0.3% by weight of acetic acid to remove the proteins and phospholipids as impurities in the fat, (NaOH) to further purify the impurities and extend shelf life,
The sodium hydroxide (NaOH) was mixed at a concentration of 1 to 3 N,
The above defatted and purified unsaturated fatty acid and sodium bicarbonate are further added to the acidic colostrum which is visually improved without damaging the antioxidative activity to delay rancidity,
Wherein said sodium bicarbonate is added at a concentration of 0.5 to 2% by weight of the total weight of said sodium bicarbonate,
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