TW201713219A - A processing method for rice bran oil extraction - Google Patents
A processing method for rice bran oil extraction Download PDFInfo
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萃取米糠油的製程發明,先利用射頻快速加熱使米糠中的脂解酶失活,因為射頻電磁波的頻率較微波小,大幅增加穿透深度及增加米糠升溫的溫度分布均勻性,克服熱傳障礙,可用以提升米糠的量產安定性。再以乙醇取代傳統的正己烷作為萃取溶劑,不只提升萃取物的安全,亦可以說是友善生態的萃取溶劑,利用連續式聚焦式超音波和微波快速萃取米糠中的油脂和油溶性物質,由於聚焦式超音波效果比傳統式洗淨式超音波效果更佳且時間更縮短,唯容易生熱,故不適合溶劑先加熱萃取,此會造成聚焦式超音波設備故障,故改以後續再連接微波加熱設備,可快速加熱萃取物,以增加米糠油的萃取率,可以達到節能省時的效果。最後再將固液分離的萃取液利用微波真空濃縮米糠油,在真空系統下可降低乙醇溶劑的蒸發溫度,且利用微波可以快速加熱溶劑,並將蒸發的乙醇冷凝回收,亦可儘量避免米糠油因為高溫長時間而氧化。整體而言,此米糠油的萃取製程可快速、節能並提升米糠油的品質。 The invention of the process for extracting rice bran oil first uses radio frequency rapid heating to inactivate the lipolytic enzyme in the rice bran, because the frequency of the radio frequency electromagnetic wave is smaller than that of the microwave, greatly increasing the penetration depth and increasing the temperature distribution uniformity of the rice bran heating, and overcoming the heat transfer obstacle. It can be used to enhance the stability of the production of rice bran. Replacing traditional n-hexane with ethanol as an extraction solvent not only enhances the safety of the extract, but also is a friendly and ecological extraction solvent. It uses continuous focused ultrasound and microwave to quickly extract the oil and oil-soluble substances in rice bran. The focused ultrasonic effect is better than the traditional washing ultrasonic method and the time is shorter, but it is easy to generate heat, so it is not suitable for the solvent to be heated and extracted first. This will cause the focus ultrasonic device to malfunction, so it is changed to follow the microwave again. Heating equipment can quickly heat the extract to increase the extraction rate of rice bran oil, which can save energy and save time. Finally, the solid-liquid separation extract is concentrated by microwave vacuum to dilute the rice bran oil, the evaporation temperature of the ethanol solvent can be lowered under the vacuum system, and the solvent can be rapidly heated by the microwave, and the evaporated ethanol can be condensed and recovered, and the rice bran oil can be avoided as much as possible. Oxidized because of high temperature for a long time Overall, this rice bran oil extraction process is fast, energy efficient and enhances the quality of rice bran oil.
米糠是一種碾米工業的副產品,佔穀物的5-8%。由於米糠含有豐富的蛋白質,脂質,膳食纖維和抗氧化化合物,如:生育酚,生育三烯酚和谷維素,是值得開發利用的天然營養食品,整體而言,米糠中營養 成分佔稻米營養價值的60%,其中米糠中含油量約為15~20%,且米糠油(玄米油)是一種營養豐富的植物油,其中主要的脂肪酸為油酸(C16:1)佔40~50%,亞油酸(C18:2)佔30~40%和棕櫚酸(C16:0)佔12~18%(胡等,2013)。但由於米糠中含有脂解酶容易快速水解米糠脂質,造成油脂快速分解氧化酸敗,提升米糠(油)的酸價,故若要萃取米糠油前,首先需脂解酶失活,以增加米糠利用和儲藏的安定性。 Rice bran is a by-product of the rice milling industry, accounting for 5-8% of the grain. Because rice bran is rich in protein, lipids, dietary fiber and antioxidant compounds such as tocopherol, tocotrienol and oryzanol, it is a natural nutritious food worthy of development and utilization. Overall, rice bran nutrition The composition accounts for 60% of the nutritional value of rice, and the oil content of rice bran is about 15-20%, and rice bran oil (black rice oil) is a nutrient-rich vegetable oil, in which the main fatty acid is oleic acid (C16:1) accounted for 40~ 50%, linoleic acid (C18:2) accounted for 30-40% and palmitic acid (C16:0) accounted for 12-18% (Hu et al., 2013). However, because rice bran contains lipolytic enzymes, it can easily hydrolyze rice bran lipids, causing rapid decomposition of oils and oxidative rancidity, and increasing the acid value of rice bran (oil). Therefore, before extracting rice bran oil, firstly, lipolytic enzymes need to be inactivated to increase rice bran utilization. And the stability of storage.
米糠經過微波加熱3min可破壞脂解酶,再配合真空包裝和低溫儲藏可使米糠穩定以延長保存時間(Ramzanzadeh et al.,1999 & 2000;Tao et al,1993)。Lakkakula等人(2004)亦曾研究以歐姆加熱以提高米糠的安定性並增加米糠油的萃取率。Thanonkaew等人(2012)曾分別利用熱風、微波、烘烤、蒸氣加熱以增加米糠的安定性,再冷壓榨米糠油,其中米糠油的明亮度、酸價、游離脂肪酸、過氧化價及抗氧化物質如:多酚、類黃酮和谷維素,大都是以微波加熱、熱風加熱優於烘烤、蒸氣,更優於未加熱處理的米糠油,但由於作者無法以微波加熱進行米糠量產加熱,故推薦熱風預加熱米糠。此更說明本專利以射頻加熱方式取代微波介電加熱和熱風方式,必可以成為米糠預加熱處理以增加安定性的主流製程。 Rice bran can be destroyed by lipothermal heating for 3 min, and then combined with vacuum packaging and low temperature storage to stabilize rice bran to prolong storage time (Ramzanzadeh et al., 1999 &2000; Tao et al, 1993). Lakkakula et al. (2004) also studied heating with ohms to increase the stability of rice bran and increase the extraction rate of rice bran oil. Thanonkaew et al. (2012) used hot air, microwave, baking and steam heating to increase the stability of rice bran, and then cold pressed rice bran oil. The brightness, acid value, free fatty acid, peroxide price and antioxidant of rice bran oil Substances such as polyphenols, flavonoids and oryzanol are mostly heated by microwaves and hot air, which are superior to baking and steam. They are better than unheated rice bran oil, but because the author cannot heat the rice bran by microwave heating, Hot air preheated rice bran is recommended. This further demonstrates that this patent replaces microwave dielectric heating and hot air by means of RF heating, and must be the mainstream process for preheating rice bran to increase stability.
米糠製油亦可先進行預處理,主要有蒸炒(烘炒)、造粒和擠壓膨發三種加工方法,再配合酵素反應以加速分解米糠,有助於萃取米糠油。例如可利用擠壓膨發輔助水酶法,此是先利用擠壓膨發將米糠中的澱粉降解以提升糊化度,且使米糠蛋白受熱失活後,再以1:7的液料比,加入2%蛋白酶,在56℃下反應2小時,米糠油的萃取率可達85%(周,2014)。另外,超音波輔助水酶法是利用纖維素酶、蛋白酶和澱粉酶先行分解米糠, 再利用超音所產生的空穴效應使米糠的細胞壁破碎,促進油脂的釋放,目前可以批式處理100g的米糠,加入1.5%酶反應3小時,液料比為1:6,再利用超音波萃取15min,米糠油的萃取率達到88%,且較能保存谷維素(魏等,2014)。 Rice bran oil can also be pretreated first, mainly including steaming (roasting), granulation and extrusion, and then reacting with enzyme to accelerate the decomposition of rice bran and help extract rice bran oil. For example, the extrusion-expansion assisted aqueous enzymatic method can be utilized, which firstly decomposes the starch in the rice bran by extrusion to increase the degree of gelatinization, and after the rice bran protein is deactivated by heat, the ratio of liquid to material is 1:7. 2% protease was added and reacted at 56 ° C for 2 hours, the extraction rate of rice bran oil reached 85% (week, 2014). In addition, the ultrasonic assisted aqueous enzymatic method utilizes cellulase, protease and amylase to decompose rice bran first. The cavitation effect of the supersonics is used to break the cell wall of rice bran and promote the release of oil. At present, 100 g of rice bran can be batch-treated, 1.5% enzyme reaction is added for 3 hours, and the liquid-to-liquid ratio is 1:6. After extraction for 15 min, the extraction rate of rice bran oil reached 88%, and it was more able to preserve oryzanol (Wei et al., 2014).
將安定化後的米糠可利用不同方法製備米糠油,其中若採用壓榨法獲取米糠油,但由於米糠中的油脂含量只有15~20%,造成壓榨出油率較低,浸出法的出油率高,但油脂中的抗氧化成分,如:生育醇、谷維素損失較大,且常採用的正己烷浸出溫度為50~60℃,己烷為易燃、易爆的溶劑,對人體和環境有害,或以異丙醇作為浸出液,在60下,料液比為1:5,浸出時間為2小時,米糠油的萃取率可達89%(張和許,2007)。利用乙醇作為溶劑,米糠和乙醇比為1:6(g/mL),在20kHz,35℃下超音波萃取可獲得米糠油為10.8%,此較傳統乙醇或正己烷浸泡所提取的米糠油分別為6%和8%為高(Krishnan et al.,2015)。 Rice bran oil can be prepared by different methods after the stabilized rice bran. If the rice bran oil is obtained by pressing, but the oil content in the rice bran is only 15-20%, the oil yield of the pressing is lower, and the oil yield of the leaching method is lower. High, but the antioxidant components in the oil, such as: tocopherol, oryzanol loss, and often used hexane leaching temperature of 50 ~ 60 ° C, hexane is a flammable, explosive solvent, harmful to the human body and the environment Or isopropanol as the leachate, at 60, the ratio of material to liquid is 1:5, the leaching time is 2 hours, and the extraction rate of rice bran oil can reach 89% (Zhang Hexu, 2007). Using ethanol as a solvent, the ratio of rice bran to ethanol is 1:6 (g/mL), and the ultrasonic extraction at 20 kHz and 35 °C can obtain 10.8% of rice bran oil, which is different from the traditional rice or n-hexane soaked rice bran oil. It is high at 6% and 8% (Krishnan et al., 2015).
使用超臨界二氧化碳萃取米糠油,是無毒的萃取法,但由於設備成本昂貴,萃取時間長,量化成本高(周等,2014)。超臨界二氧化碳萃取法可透過控制CO2的流速((1-9mL/min),溫度(40-80℃)和壓力(20-40MPa)溫度萃取3小時以提高米糠油及谷維素的萃取率,甚至高於正己烷溶劑萃取米糠7小時的萃取量0.223g油/g米糠樣品(Tomita et al.,2014)。 The use of supercritical carbon dioxide to extract rice bran oil is a non-toxic extraction method, but due to the high cost of equipment, long extraction time and high cost of quantification (Wei et al., 2014). The supercritical carbon dioxide extraction method can increase the extraction rate of rice bran oil and oryzanol by controlling the flow rate of CO2 ((1-9mL/min), temperature (40-80°C) and pressure (20-40MPa) for 3 hours. An extraction amount of 0.223 g of oil/g rice bran sample (Tomita et al., 2014) was extracted with n-hexane solvent for 7 hours.
利用溶劑萃取米糠油,勢必要再進行加熱真空蒸發以去除或回收溶劑以提升米糠油的純度,此步驟亦相當的耗時耗能,需針對此步驟進行改善,以符合安全、節能、減碳之原則。 The solvent extraction of rice bran oil is necessary to carry out heating and vacuum evaporation to remove or recover the solvent to enhance the purity of the rice bran oil. This step is also quite time-consuming and energy-consuming. It is necessary to improve this step to meet safety, energy saving and carbon reduction. The principle.
本製程發明包括三部分,第一部分為射頻加熱促使米糠安定性,第二部分為使用乙醇作為萃取溶劑,以聚焦式超音波和微波快速萃取米糠中的油脂和油溶性物質如:維生素E和谷維素等,第三部分為利用微波真空濃縮固液分離的萃取液以純化米糠油,以蒸發回收乙醇以達到製程安全、節時、節能和環境友善之目標。 The invention consists of three parts. The first part is RF heating to promote the stability of rice bran. The second part uses ethanol as the extraction solvent to extract the oil and oil-soluble substances in rice bran by focused ultrasound and microwave, such as: vitamin E and oryzanol. Etc., the third part is to use microwave vacuum to concentrate the solid-liquid separation extract to purify rice bran oil to evaporate and recover ethanol to achieve the goal of safe process, time saving, energy saving and environmental friendliness.
圖一 係為本發明方法的流程圖。 Figure 1 is a flow chart of the method of the present invention.
先將米糠裝於耐高溫的聚丙烯(PP)塑膠盒中,再放置於射頻加熱系統中,一般而言,米糠重量增加會加大射頻輸出,故需調整適當的射頻電極板間距操作(圖1),才能獲得較大的升溫速率。以1kg米糠置於不同射頻電極板間距加熱下的升溫情形(圖2),由於米糠的升溫是主要藉由極性水分在射頻電極快速改變正、負電極以造成快速旋轉而摩擦升溫,在射頻電極板間距為5、6、8、10和12cm下需1、1.5、2、3和3.5cm才能達到100℃左右。若再考慮射頻加熱米糠的溫度均勻性,故1kg米糠則以選擇在射頻電極板間距為6cm下加熱2min為宜,且由圖3的米糠升溫曲線及脂解酶失活的效果,表示脂解酶確實可以因為射頻加熱升溫而失去活性。再將經射頻抑酶組和未處理(控制組)的米糠25℃下進行米糠儲藏安定性試驗,由表1的結果得知在儲藏1週時,控制組米糠的酸價和過氧化價均較射頻處理組增加,且射頻處理組的酸價在後續儲藏至4週均未有顯著變化,然而控制組的米糠之酸價已是射頻處理組的2.5倍以上,表示射頻加熱抑酶確實可增加米糠的安定性,便於後續米糠油的萃取。 Firstly, the rice bran is placed in a high temperature resistant polypropylene (PP) plastic box and placed in an RF heating system. Generally, the weight increase of the rice bran will increase the RF output, so it is necessary to adjust the appropriate RF electrode plate spacing operation (Fig. 1), in order to obtain a larger heating rate. The temperature rise of 1kg rice bran placed under the heating of different RF electrode plates (Fig. 2), because the temperature rise of rice bran is mainly caused by the polar moisture in the RF electrode rapidly changing the positive and negative electrodes to cause rapid rotation and friction heating, at the RF electrode It is required to be 1, 5, 2, 3 and 3.5 cm at a distance of 5, 6, 8, 10 and 12 cm to reach about 100 °C. If we consider the temperature uniformity of the RF heating rice bran, 1kg rice bran is preferably heated at a distance of 6cm from the RF electrode plate for 2min, and the rice radix heating curve and the lipolytic enzyme inactivation effect of Figure 3 indicate lipolysis. Enzymes can indeed lose activity due to RF heating. The rice bran storage stability test was carried out at 25 ° C in the RF inhibitory group and the untreated (control group). The results of Table 1 show that the acid value and peroxide price of the rice bran in the control group were both at 1 week of storage. Compared with the RF treatment group, the acid value of the RF treatment group did not change significantly after 4 weeks of storage. However, the acid value of the rice bran in the control group was more than 2.5 times that of the RF treatment group, indicating that the RF heating inhibitor could indeed be used. Increase the stability of rice bran to facilitate the extraction of subsequent rice bran oil.
稱取20g的已經射頻處理的米糠加入20倍的95%乙醇400mL,料液比為1:20分別置於聚焦式超音波耳萃取及微波萃取設備中,萃取時間控制在1、3、5和7min,結果米糠油的萃取率在5min時最高分別可達0.2125和0.239g油/g米糠(表2)。然而以洗淨式超音波進行米糠油的萃取20、40、60、80和100min,則萃取米糠油的產率會隨著萃取時間而漸漸增加,至100min也才能萃取到0.2025g油/g米糠(表3),故聚焦式超音波的萃取效率明顯高於洗淨式超音波。另一方面,利用超臨界二氧化碳萃取米糠油120min和180min可得到0.06和0.18g油/g米糠,故超臨界二氧化碳萃取時間遠較超音波和微波萃取長,不只設備昂貴,且萃取效果也不佳。最後結合聚焦式超音波和微波萃取,分別是處理1.5min,使總萃取時間達3min,則米糠油的萃取量為0.2275g油/g米糠,故結合聚焦式超音波和微波萃取可明顯縮短萃取時間。 Weigh 20g of RF-treated rice bran and add 20 times of 95% ethanol to 400mL. The ratio of material to liquid is 1:20 in the focused ultrasonic ear extraction and microwave extraction equipment. The extraction time is controlled at 1, 3, 5 and At 7 min, the extraction rate of rice bran oil reached a maximum of 0.2125 and 0.239 g oil/g rice bran at 5 min (Table 2). However, with the extraction of rice bran oil by washing ultrasonic waves for 20, 40, 60, 80 and 100 min, the yield of extracted rice bran oil will gradually increase with the extraction time, and it will be extracted to 0.2025 g oil/g rice bran after 100 min. (Table 3), so the extraction efficiency of the focused ultrasonic wave is significantly higher than that of the washed ultrasonic wave. On the other hand, the extraction of rice bran oil with supercritical carbon dioxide for 120min and 180min can obtain 0.06 and 0.18g oil/g rice bran, so the supercritical carbon dioxide extraction time is much longer than that of ultrasonic and microwave extraction, not only expensive equipment, but also excellent extraction effect. . Finally, combined with focused ultrasound and microwave extraction, the treatment is 1.5min, the total extraction time is 3min, then the extraction amount of rice bran oil is 0.2275g oil / g rice bran, so combined with focused ultrasound and microwave extraction can significantly shorten the extraction time.
將前述的米糠乙醇萃取液400mL先經固液離心分離後可獲得乙醇萃取液,若是利用50℃的水浴槽,進行旋轉式減壓濃縮時,需要30~40min方能完成乙醇的回收,以取得米糠油。然而使用微波真空濃縮400mL乙醇萃取液,只需10min即完成乙醇的蒸發冷凝作業,收集得到米糠油,故利用微波真空濃縮技術可加速乙醇萃取溶劑的回收作業。 The above-mentioned rice bran ethanol extract 400mL is firstly centrifuged to obtain an ethanol extract. If a 50°C water bath is used for rotary decompression and concentration, it takes 30 to 40 minutes to complete the ethanol recovery. Rice bran oil. However, using microwave vacuum to concentrate 400mL ethanol extract, it takes only 10 minutes to complete the evaporation and condensation operation of ethanol, and the rice bran oil is collected. Therefore, the microwave vacuum concentration technology can accelerate the recovery of ethanol extraction solvent.
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CN112806523A (en) * | 2021-02-03 | 2021-05-18 | 湖南米珍宝生物高科技有限公司 | Method for radio frequency processing of stabilized rice bran |
CN115053926A (en) * | 2022-06-07 | 2022-09-16 | 宁波市农业科学研究院 | Method for improving low-temperature storage quality of brown rice |
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CN115053926A (en) * | 2022-06-07 | 2022-09-16 | 宁波市农业科学研究院 | Method for improving low-temperature storage quality of brown rice |
CN115053926B (en) * | 2022-06-07 | 2023-10-20 | 宁波市农业科学研究院 | Method for improving low-temperature storage quality of brown rice |
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