WO2020135061A1 - 低氰苷的木薯粉及其制备方法 - Google Patents

低氰苷的木薯粉及其制备方法 Download PDF

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WO2020135061A1
WO2020135061A1 PCT/CN2019/124707 CN2019124707W WO2020135061A1 WO 2020135061 A1 WO2020135061 A1 WO 2020135061A1 CN 2019124707 W CN2019124707 W CN 2019124707W WO 2020135061 A1 WO2020135061 A1 WO 2020135061A1
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cassava
cyanoside
low
content
powder
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French (fr)
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陆柏益
徐涛
钟永恒
陈祁
刘彦君
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Zhejiang University
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Zhejiang University
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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00—Shaping or working of foodstuffs characterised by the products
    • A23P10/40—Shaping or working of foodstuffs characterised by the products free-flowing powder or instant powder, i.e. powder which is reconstituted rapidly when liquid is added
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L19/00—Products from fruits or vegetables; Preparation or treatment thereof
    • A23L19/01—Instant products; Powders; Flakes; Granules
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L19/00—Products from fruits or vegetables; Preparation or treatment thereof
    • A23L19/10—Products from fruits or vegetables; Preparation or treatment thereof of tuberous or like starch containing root crops
    • A23L19/11—Cassava, manioc, tapioca, or fermented products thereof, e.g. gari
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
    • A23L5/20—Removal of unwanted matter, e.g. deodorisation or detoxification
    • A23L5/21—Removal of unwanted matter, e.g. deodorisation or detoxification by heating without chemical treatment, e.g. steam treatment, cooking
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
    • A23L5/20—Removal of unwanted matter, e.g. deodorisation or detoxification
    • A23L5/25—Removal of unwanted matter, e.g. deodorisation or detoxification using enzymes
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
    • A23L5/30—Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation
    • A23L5/32—Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation using phonon wave energy, e.g. sound or ultrasonic waves
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
    • Y02A40/90—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in food processing or handling, e.g. food conservation

Definitions

  • the invention relates to the technical field of food processing and preservation, in particular to a low-cyanoside cassava powder and a preparation method thereof.
  • Cyanosides are a class of secondary metabolites of glycosides that can be hydrolyzed to produce highly toxic hydrocyanic acid. They are also called cyanogenic glycosides and cyanoglycosides. It is widely found in legumes, Rosaceae, Euphorbiaceae and other plants, among which food-borne plants are cassava, almonds, loquat and so on.
  • the reaction of cyanoside to produce hydrocyanic acid involves two enzymes; cyanoside first decomposes under the action of linamarase to form cyanohydrin and sugar, cyanohydrin is very unstable, and naturally decomposes into the corresponding ketone, aldehyde compound and hydrocyanide acid.
  • Hydroxynitrile degrading enzymes can accelerate this degradation reaction.
  • Cyanoside and linamarase are located in different parts of the plant. When chewing or crushing plant food containing cyanoside, the cell structure is destroyed, so that linamarase and cyanoside can produce hydrocyanic acid, which is edible Fresh plants cause hydrocyanic acid poisoning. Therefore, reducing the content of cyanoside can reduce the risk of hydrocyanic acid poisoning. While ensuring enzyme activity, the cell structure is destroyed in advance, and the linseinase and cyanoside are increased. Exposure may reduce cyanoside content in plants.
  • Cassava (scientific name: Manihotesculenta) is an important food crop in tropical and subtropical regions. As of 2014, its global production reached 270 million, and the world's FAO also ranked cassava as the fourth most important crop in developing countries. Cassava roots are rich in starch, and cassava starch is widely used as food, feed and industrial raw materials.
  • CODEX STAN 238 and CODEX STAN 300 respectively stipulate the standards for sweet cassava and bitter cassava, with the content of hydrocyanic acid being 50mg/kg fresh weight, higher than the limit value bitter cassava, low Yu is sweet cassava.
  • the hydrocyanic acid in cassava is derived from the cyanoside which contains linamarin and phleboside. Among them, linamarin is about 90% of the total cyanoside and phlebidine is about 10% of the total cyanoside. Excessive consumption of fresh cassava may cause acute poisoning, and long-term consumption of large amounts of cassava may also cause neurological movement disorders. Therefore, the development of a method for degrading cyanoside in cassava to reduce the content of hydrocyanic acid in cassava can reduce the risk of cassava consumption and promote the development of the cassava industry.
  • the invention patent with patent number CN201310304627 discloses "a method for quickly detoxifying cassava flour”. The steps are: collecting fresh cassava and peeling and washing it, requiring the starch content of fresh cassava to be not less than 26.3%; adding water after crushing the fresh cassava Prepared into puree, the mass ratio of fresh cassava to water is 1: 0.8, through 80 mesh screen; dehydrate the puree with a plate and frame filter press, press filter under 1.8Mpa for 10min; dilute the dehydrated material to water to The slurry with 60% solids content is stirred at 30r/min for 20min, and then filtered with a plate and frame filter press at 1.7Mpa for 14min; after dehydration, the material is diluted with water to dilute the slurry to 60% solids content, with 35r/ Stir for 25min, then filter with 0.4Mpa in a belt filter press; pre-dry with 6.5 kg of high-pressure steam to a moisture content of 33%; dry with 7.5 kg of high
  • the patent number is CN201410391720, an invention patent, which discloses "the production method of sweet cassava powder”.
  • the steps are: fresh cassava is washed and the outer skin is removed; the cassava is crushed using a crushing device to obtain cassava grains with a particle size of 3 mm or less; naturally dried Or air-dried cassava grains at 40°C ⁇ 50°C to make the moisture content ⁇ 15.0%, dried cassava grains are obtained; the dried cassava grains are crushed by a dry mill in a primary stage, and then passed through a 50-70 mesh sieve, followed by secondary crushing, over 100 Mesh sieve to get whole cassava powder.
  • Ultrasound refers to sound waves with a frequency exceeding the hearing limit of the human ear (20kHz). According to their different applications in the food industry clock, they can be divided into two categories: high frequency (100kHz ⁇ 1MHz), low power ( ⁇ 1W/cm 2 ) and low Frequency (20 ⁇ 100kHz) and high power (10 ⁇ 1000W/cm 2 ).
  • High-frequency low-power ultrasound is mostly used in non-destructive analysis and quality assessment, such as evaluating the hardness and maturity of food; low-frequency high-intensity ultrasound is also called power ultrasound, which is often used in food modification, such as sterilization to extend shelf life Period, degradation of pesticide residues, etc.
  • the cavitation effect is the main principle of the application of ultrasonic waves in the food industry.
  • the cavitation effect refers to the phenomenon of the formation, growth, and rupture of tiny bubbles in the fluid.
  • the rupture of cavitation bubbles will cause high temperatures in the bubbles (up to 5500 °C), High pressure (up to 50Mpa) hot spots, which can accelerate the rupture of cells, promote the dissolution of biologically active substances, increase the possibility of contact between the substrate and the enzyme, and also increase the generation of free radicals in the medium.
  • the invention patent with patent number CN201710840986 discloses "a method of ultrasonic degradation of mycotoxins", using 20kHz, 100 ⁇ 550W ultrasonic treatment containing aflatoxin B1, deoxynivalenol, zearalenone and ochre Two or more aqueous solutions of aspergillus toxin showed that ultrasonic waves can efficiently degrade these mycotoxins with a degradation rate of up to 96.4%.
  • ultrasonic waves can effectively improve the catalytic activity of the enzyme and increase the efficiency of the enzymatic reaction.
  • Low-intensity, short-time ultrasonic action can activate catalytic enzymes, but too high power and long processing time may also lead to enzyme inactivation, and different enzymes have different responses to ultrasonic intensity and time.
  • the mechanical shear force generated by the cavitation effect of ultrasonic waves can directly modify the structure of the enzyme, such as loosening the enzyme polymer and exposing its active site, thereby increasing the activity of the enzyme.
  • the technical problem to be solved by the present invention is to provide a low cyanoside cassava powder and preparation method thereof.
  • the cassava powder obtained has a cyanoside content of less than 15 mg/kg.
  • the preparation method of the present invention is simple to operate and easy to implement without affecting cassava The nutritional quality of the starch content of the powder.
  • the preparation method of the present invention has no selectivity for cassava raw materials, and both sweet cassava and bitter cassava can be produced by the preparation method of the present invention.
  • the present invention provides a method for preparing cassava powder with low cyanide content.
  • Fresh cassava fresh cassava after harvesting
  • the raw materials are dried and crushed to obtain low-cyanoside cassava powder.
  • the ultrasonic power corresponding to the raw material after every 5 kg of ultrasonic treatment is 500 to 3000 watts (that is, the ultrasonic power corresponding to each kilogram of raw material is 100 to 600 watts).
  • the power of the ultrasonic wave per kilogram of raw material is 600 watts.
  • the drying is natural sun drying or hot air drying, and when it is hot air drying, the temperature is ⁇ 70°C.
  • the fresh cassava is sweet cassava or bitter cassava
  • Sweet cassava is SC9, SC12, SC6068, GR9, GR10, GR891, bread cassava, Limin 1;
  • the present invention also provides a low-cyanoside cassava powder prepared according to the above method, with a total cyanoside content ⁇ 15 mg/kg and a hydrocyanic acid content ⁇ 2 mg/kg.
  • the preparation method of cassava grains, cassava silk or cassava pulp is:
  • the cassava powder using the low cyanoside of the present invention has a total cyanoside content of less than 15 mg/kg and a hydrocyanic acid content of less than 2 mg/kg. It has inherent white, light yellow, pink or other colors inherent in cassava roots. Raw materials such as tapioca starch and tapioca powder should have an odor, no odor, and no black spots and mildew spots visible to the naked eye.
  • the present invention can obtain a low-cyanoside cassava powder whose total cyanoside content is less than 15 mg/kg, and the preparation method is simple and efficient.
  • the preparation method is suitable for both sweet cassava and bitter cassava, and can effectively reduce the content of cyanoside in cassava flour, but has no significant effect on other nutritional qualities such as starch content, protein content, fat content, etc.
  • the method is simple, efficient and has no maturation process, and the obtained cassava powder has great potential for further processing.
  • FIG. 1 is an overlapping display diagram of linamarin and MRM.
  • The% in the following examples, unless otherwise specified, are all mass percentages.
  • the production water used in the following examples meets drinking water standards.
  • the cassava grain size is about 3mm
  • the cassava silk cross-sectional diameter is about 3-4mm
  • the length is about 2cm.
  • cassava flour After crushing the dried cassava grains with a dry grinder to an 80 mesh steel sieve, cassava flour was obtained.
  • 5kg of chopped cassava silk was immersed in 7500mL of warm water at 40°C, and placed in an ultrasound system, and ultrasonicated at a frequency of 53kHz and 1500W for 15 minutes (ie, the power of ultrasonic wave per kg of raw material was 300W).
  • the dried cassava shreds were crushed with a dry grinder to an 80 mesh steel sieve to obtain cassava flour.
  • cassava flour After crushing the dried cassava grains with a dry grinder to an 80 mesh steel sieve, cassava flour was obtained.
  • the cassava After filtering the ultrasonic cassava pulp, the cassava is naturally dried until the moisture content is 8.9%, and dried cassava pieces are obtained.
  • cassava flour After crushing the dried cassava grains with a dry grinder to an 80 mesh steel sieve, cassava flour was obtained.
  • the cassava After filtering the ultrasonic cassava pulp, the cassava is naturally dried until the moisture content is 9.4%, and dried cassava pieces are obtained.
  • Example 2 in “A method for rapid detoxification of cassava flour” produces cassava flour, as follows:
  • step (1) the cleaned raw material is obtained, using water as a medium, the fresh cassava raw material and the water distribution ratio is 1: 0.8, and the crushing is carried out.
  • the fineness of the crushed material passes through the 80 mesh aperture and the pass rate is 100%.
  • step (3) The material obtained in step (2) is dehydrated by a plate and frame filter press.
  • the working pressure of the plate and frame filter press is 1.8Mpa, and the filter press time is 10 minutes.
  • step (3) Add water to the material obtained in step (3), adjust the solid content of the material to 60%, select the stirring speed of the material at 30r/min, and stir the time at 20min, then enter the plate and frame filter press The machine is dehydrated, the working pressure of the plate and frame filter press is 1.7Mpa, and the filter press time is 14 minutes.
  • step (4) Add water to the material obtained in step (4), adjust the solid content of the material to 60%, the material stirring speed to 35 rpm, and the stirring time to 25 minutes.
  • the working pressure of the belt filter press is 0.4Mpa, continuous feeding and continuous discharging.
  • step (6) The raw material obtained in step (6) is pre-dried, the pre-dried steam pressure is 6.5 kg, the inlet temperature is 135°C, the outlet temperature is 75°C, and the pre-dried moisture product moisture is 33%; The steam pressure is 7.5 kg, the inlet temperature is 170°C, the outlet temperature is below 40°C, and the water content is below 13.0%.
  • step (7) The raw materials obtained in step (7) are crushed, and the fineness of the product is passed through a 120-mesh sieve 100% to obtain cassava powder.
  • the moisture content of the dried cassava grains is less than 13.0%.
  • the determination of ash content adopts the first method in "GB 5009.4-2016 National Food Safety Standard Determination of Ash in Food", the determination of total ash in food; the determination of protein content adopts "GB 5009.5-2016 National Food Safety Standard for Protein in Food
  • the first method in "Determination”, Kjeldahl nitrogen determination method; the determination of fat content adopts the first method in "GB 500500-2016 National Food Safety Standard Determination of Fat in Food", Soxhlet extraction method; soluble sugar content
  • the detection adopts "NY/T2742-2015 Determination of Soluble Sugar in Fruits and Products 3,5-Dinitrosalicylic Acid Colorimetric Method”; the determination of starch content adopts "GB500500-2016 National Food Safety National Standards for the Determination of Starch in Food
  • the second method in the "acid hydrolysis method; the determination of the content of hydrocyanic acid adopts the second method in the "GB 5509.36-2016 National Food Safety Standard for the Determination of Cyanide in Food", gas chromatography.
  • the content of cyanoside is determined by LC-MS. The specific steps are as follows:
  • Ion source ESI source
  • the cassava flour obtained in Examples 1 to 6, Comparative Examples 1 to 2, Comparative Example 3-1, Comparative Example 3-2, Comparative Example 4 and Comparative Example 5 and SC9 in Baishali Autonomous County of Hainan province and Qiongzhong Li Nationality in Hainan province were tested
  • the cassava varieties of Comparative Example 3-2, Comparative Example 4 and Comparative Example 5 are sweet cassava, and the cassava varieties of Examples 5 to 6 are bitter cassava.
  • # indicates that this indicator is compared with fresh cassava of the same variety and the same origin, P ⁇ 0.05.

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Abstract

一种低氰苷的木薯粉的制备方法，包括以下步骤：采收后的新鲜木薯经清洗、去皮、切碎，所得到的木薯粒、木薯丝或木薯浆作为原料；将原料浸没在温度为35-50℃温水中进行超声波处理10-30分钟，超声波的频率为20kHz-100kHz，得超声波处理后原料；将超声波处理后原料进行干燥、粉碎，得低氰苷的木薯粉。所得木薯粉的氰苷含量低于15mg/kg。

Description

低氰苷的木薯粉及其制备方法 技术领域
本发明涉及食品加工与保鲜技术领域，具体涉及一种低氰苷的木薯粉及其制备方法。
背景技术
氰苷是一类可以水解生成高毒性氢氰酸的糖苷类植物次生代谢产物，亦称生氰糖苷、氰醇苷等。其广泛存在于豆科、蔷薇科、大戟科等的植物中，其中的食源性植物有木薯、杏仁、枇杷等。氰苷产生氢氰酸的反应有两种酶的参与；氰苷首先在亚麻苦苷酶的作用下分解生成氰醇和糖，氰醇很不稳定，自然分解为相应的酮、醛化合物和氢氰酸。羟腈分解酶可加速这一降解反应。氰苷和亚麻苦苷酶处于植物的不同部位，当咀嚼或破碎含氰苷的植物食品时，其细胞结构被破坏，使得亚麻苦苷酶可以和氰苷作用产生氢氰酸，这便是食用新鲜植物引起氢氰酸中毒的原因，因此，降低氰苷的含量即可降低氢氰酸的中毒风险，而在保证酶活的同时，提前破坏细胞结构，增大亚麻苦苷酶和氰苷的接触，可能降低植物中的氰苷含量。
木薯(学名:Manihot esculenta)是热带、亚热带地区的重要粮食作物。截至2014年，其全球产量达2.7亿，世界粮农组织也将木薯列为发展中国家的第四大重要作物。木薯块根富含淀粉，木薯淀粉被广泛用作食物、饲料和工业原料。国际食品法典委员会的法典标准中，CODEX STAN 238和CODEX STAN 300分别规定了甜木薯和苦木薯的标准，以氢氰酸含量为50mg/kg鲜重为限，高于限定值为苦木薯，低于则为甜木薯。木薯中的氢氰酸来源于其含有亚麻苦苷和百脉根苷等氰苷，其中亚麻苦苷占总氰苷约为90％，百脉根苷占总氰苷约为10％。过量食用鲜木薯可能导致急性中毒，长期大量食用木薯也可能引起神经性运动失调。因此，研发降解木薯中的氰苷的方法，从而降低木薯中氢氰酸含量的方法可降低因食用木薯而带来的风险，促进木薯产业的发展。
专利号为CN201310304627的发明专利，公开了“一种木薯粉快速脱毒的方法”，其步骤为，收集鲜木薯并去皮洗净，要求鲜木薯淀粉含量不小于26.3％；粉碎鲜木薯后加水调配成原浆，鲜木薯与水的质量比为1：0.8，过80目筛网；用板框压滤机对原浆进行脱水，在1.8Mpa下压滤10min；对脱水后物料加水稀释至含固量为60％的浆液，以30r/min搅拌20min，后以板框压滤机在1.7Mpa压滤14min；对脱水后物料再加水稀释至含固量为60％的浆液，以35r/min搅拌25min，后以带式压滤机以0.4Mpa进行压滤；以6.5公斤的高压蒸汽进行预干燥至水分含量为33％；以7.5公斤的高压蒸汽进行干燥至水分含量小于13.57％；粉碎物料后 过120目筛网，得脱毒后的木薯粉。虽然食用该方法可以得到低氢氰酸的木薯粉，且对原料中的氢氰酸含量没有要求，但是由于采用了重复地稀释和脱水过程，木薯中的可溶性营养物质损失严重，时间成本及能耗、水资源消耗均较高。
专利号为CN201410391720的发明专利，公开了“甜木薯全粉的生产制作方法”，其步骤，鲜木薯洗净、去除外表皮；使用破碎设备破碎木薯获得粒度小于等于3mm的木薯粒；自然晒干或在40℃～50℃风干木薯粒，使其水分含量≤15.0％，得干木薯粒；干木薯粒通过干磨机一级粉碎，过50～70目筛，后进行二级粉碎，过100目筛，得木薯全粉。虽然该方法可以得到含有除外表皮外的所有物质的木薯全粉，但是其要求木薯的原料为氢氰酸含量不超过50mg/kg的甜木薯，而专利号为CN201310304627的发明专利，公开了“一种木薯粉快速脱毒的方法”，其检测了多种木薯品种(系)的氢氰酸含量，结果显示，大多数样品氢氰酸含量大于50mg/kg。因此，虽然得到的甜木薯全粉的氢氰酸含量极低，但是对于氢氰酸含量高的木薯原料不适用。
超声波是指频率超过人耳听力极限(20kHz)的声波，根据其在食品工业钟的应用范围不同，可分为两类：高频率(100kHz～1MHz)低功率(<1W/cm 2)和低频率(20～100kHz)高功率(10～1000W/cm 2)。高频率低功率超声波大多应用在无损分析及质量评估中，如评估食品的硬度、成熟度等；低频率高强度的超声波也被称为功率超声波，常用于食品的改性，如杀菌以延长货架期、降解农药残留等。空化效应是超声波在食品工业中应用的主要原理，空化效应是指流体中的微小气泡形成、生长、破裂的现象，空化气泡的破裂会在气泡局部产生高温(可达5500℃)、高压(可达50Mpa)的热点，这可以加速细胞的破裂，促进其中生物活性物质的溶出，增大底物与酶的接触可能，也会增加介质中的自由基的产生。专利号为CN201710840986的发明专利，公开了“一种真菌毒素的超声波降解方法”，利用20kHz，100～550W的超声波处理含有黄曲霉毒素B1、脱氧雪腐镰刀烯醇、玉米赤霉烯酮和赭曲霉毒素中两种或两种以上的水溶液，结果表明超声波可以高效降解这些真菌毒素，降解率最高可达96.4％。
空化作用除了物理上的机械效应直接加速反应外，目前也有实验表明，超声波而可以有效提高酶的催化活性，增大酶促反应的效率。低强度、短时间的超声波作用，可以活化催化酶，但是功率过高、处理时间过长也有可能导致酶的失活，且不同的酶对超声强度和时间的反应不同。超声波的空化效应产生的机械剪切力可以直接对酶的结构进行修饰改性，如使酶聚合体变得松散，暴露其活性位点，从而提高酶的活性。但是长时间、高强度的超声波也会产生大量活泼自由基以及过强的机械剪切力，导致酶的结构被破坏而失活。木薯中的氰苷位 于细胞质，而可以降解氰苷产生氢氰酸的亚麻苦苷酶位于木薯的细胞壁，超声波处理可以促进氰苷和亚麻苦苷酶的接触，合适强度和处理时间的超声波处理也有可能促进亚麻苦苷酶的活性，进而加快氰苷降解成挥发性的氢氰酸，从而降低木薯产品中的氰苷和氢氰酸含量。但是目前还未见超声波应用于亚麻苦苷、百脉根苷等的去除的研究报道。
发明内容
本发明要解决的技术问题是提供一种低氰苷的木薯粉及其制备方法，所得木薯粉的氰苷含量低于15mg/kg，本发明的制备方法操作简单，易于实现，不会影响木薯粉的淀粉含量等营养品质。本发明的制备方法对于木薯原料没有选择性，甜木薯、苦木薯均可采用本发明中的制备方法进行生产。
为了解决上述技术问题，本发明提供一种低氰苷的木薯粉的制备方法，新鲜木薯(采收后的新鲜木薯)经清洗、去皮、切碎，所得到木薯粒、木薯丝或木薯浆作为原料，还包括以下步骤：
将原料浸没在温度为35～50℃温水中进行超声波处理10～30分钟，超声波的频率为20kHz～100kHz；得超声波处理后原料；
将超声波处理后原料经干燥、粉碎，得低氰苷的木薯粉。
作为本发明的低氰苷的木薯粉的制备方法的改进：每5kg超声波处理后原料对应的超声波的功率为500～3000瓦(即，每千克原料对应的超声波的功率为100～600瓦)。优选的，每千克原料对应的超声波的功率为600瓦。
作为本发明的低氰苷的木薯粉的制备方法的进一步改进：干燥至含水率≤13.0％(重量％)；粉碎至80目筛网。
作为本发明的低氰苷的木薯粉的制备方法的进一步改进：所述干燥为自然晒干或热风烘干，当为热风烘干时，温度≤70℃。
作为本发明的低氰苷的木薯粉的制备方法的进一步改进：所述鲜木薯为甜木薯或苦木薯；
甜木薯为SC9、SC12、SC6068、GR9、GR10、GR891、面包木薯、利民1号；
苦木薯为SC6、SC7、SC8、SC124、SC201、GR4、GR911、F499。
本发明还同时提供了按照上述方法制备而得的低氰苷的木薯粉，总氰苷含量＜15mg/kg，氢氰酸含量＜2mg/kg。
在本发明的制备方法中：木薯粒、木薯丝或木薯浆的制备方法为：
a、新鲜木薯在采收后，以带压力的水清洗去除其表面残留的土壤，然后以木薯去皮机或人工去除外皮以及内皮，保留木薯肉；
b、使用搅碎机将木薯肉切碎成木薯粒、以切丝机将木薯肉切成木薯丝或以粉碎机将木薯肉打碎成匀浆，备用；
采用本发明的低氰苷的木薯粉，其总氰苷含量在15mg/kg以下，氢氰酸含量在2mg/kg以下，具有固有的白色、浅黄色、粉红色或木薯块根固有其他色泽，具木薯淀粉、木薯粉等原料应有气味，无杂味，无肉眼可见的黑点和霉点。
与现有技术相比，本发明可以获得一种低氰苷的木薯粉，其总氰苷含量低于15mg/kg，且制备方法操作简单、高效。
该制备方法同时适用于甜木薯与苦木薯，且可以有效降低木薯粉中的氰苷含量，而对其他营养品质如淀粉含量、蛋白质含量、脂肪含量等无显著影响。同时方法操作简单、高效，无熟化过程，得到的木薯粉进一步加工潜能大。
附图说明
下面结合附图对本发明的具体实施方式作进一步详细说明。
图1为亚麻苦苷与百脉根苷MRM重叠显示图。
具体实施方式
下面结合具体实施例对本发明进行进一步描述，但本发明的保护范围并不仅限于此：
下述实施例中的新鲜木薯原料，如无特殊说明，均为产自海南省白沙黎族自治县，品种均为SC9。
下述实施例中的％，如无特殊说明，均为质量百分含量。下述实施例中所用的生产用水符合饮用水标准。木薯粒粒径约为3mm，木薯丝横截面直径约为3～4mm，长度约为2cm。
实施例1、
将采收2天内的新鲜木薯洗净，人工去除木薯内皮以及外皮，保证没有木薯皮的残留，而影响木薯粉的氰苷含量。使用搅碎机切碎木薯肉以获得木薯粒。
以35℃的温水7500mL浸没切好的木薯粒5kg，并置于超声仪中，以20kHz频率，500瓦功率超声10分钟(即，每千克原料对应的超声波的功率为100瓦)。
取出超声过的木薯粒，滤除水分，以电热鼓风干燥箱在40℃下烘干木薯粒至水分含量为10.2％，得干木薯粒。
以干磨机粉碎干木薯粒至过80目钢筛后，得木薯粉。
实施例2、
将采收2天内的新鲜木薯洗净，以木薯去皮机去除木薯内皮以及外皮，保证没有木薯皮 的残留，而影响木薯粉的氰苷含量。
使用切丝机将木薯肉切碎成木薯丝。
以40℃的温水7500mL浸没切好的木薯丝5kg，并置于超声仪中，以53kHz频率，1500瓦功率超声15分钟(即，每千克原料对应的超声波的功率为300瓦)。
取出超声过的木薯丝，以电热鼓风干燥箱50℃烘干木薯粒至水分含量为9.6％，得干木薯丝。
以干磨机粉碎干木薯丝至过80目钢筛，得木薯粉。
实施例3、
将采收2天内的新鲜木薯洗净，人工去除木薯内皮以及外皮，保证没有木薯皮的残留，而影响木薯粉的氰苷含量。
使用搅碎机切碎木薯肉以获得木薯粒。
以45℃的温水7500mL浸没切好的木薯粒5kg，并置于超声仪中，以70kHz频率，2200瓦功率超声20分钟(即，每千克原料对应的超声波的功率为440瓦)。
取出超声过的木薯粒，滤除水分，以电热鼓风干燥箱在40℃下烘干木薯粒至水分含量为11.3％，得干木薯粒。
以干磨机粉碎干木薯粒至过80目钢筛后，得木薯粉。
实施例4、
将采收2天内的新鲜木薯洗净，人工去除木薯内皮以及外皮，保证没有木薯皮的残留，而影响木薯粉的氰苷含量。使用粉碎机将木薯肉打碎成匀浆。
以50℃的温水7500mL混合粉碎好的木薯浆5kg，并置于超声仪中，以100kHz频率，3000瓦功率超声30分钟(即，每千克原料对应的超声波的功率为600瓦)。
过滤超声过的木薯浆，自然晒干木薯至水分含量为8.9％，得干木薯块。
以干磨机粉碎干木薯块至过80目钢筛，得木薯粉。
实施例5、
将采收2天内自海南省琼中黎族苗族自治县的品种为SC6的苦木薯洗净，以木薯去皮机去除木薯内皮以及外皮，保证没有木薯皮的残留，而影响木薯粉的氰苷含量。使用搅碎机切碎木薯肉以获得木薯粒。
以50℃的温水7500mL浸没切好的木薯粒5kg，并置于超声仪中，以100kHz频率，3000瓦功率超声30分钟(即，每千克原料对应的超声波的功率为600瓦)。
取出超声过的木薯粒，以电热鼓风干燥箱55℃烘干木薯粒至水分含量为10.2％，得干木 薯粒。
以干磨机粉碎干木薯粒至过80目钢筛后，得木薯粉。
实施例6、
将采收2天内自海南省东方市的品种为GR911的苦木薯洗净，人工去除木薯内皮以及外皮，保证没有木薯皮的残留，而影响木薯粉的氰苷含量。使用粉碎机将木薯肉打碎成匀浆。
以50℃的温水7500mL混合粉碎好的木薯浆5kg，并置于超声仪中，以100kHz频率，3000瓦功率超声30分钟(即，每千克原料对应的超声波的功率为600瓦)。
过滤超声过的木薯浆，自然晒干木薯至水分含量为9.4％，得干木薯块。
以干磨机粉碎干木薯块至过80目钢筛，得木薯粉。
对比例1
参考专利号CN201310304627的发明专利，“一种木薯粉快速脱毒的方法”中的实施例2生产木薯粉，具体如下：
(1)将采收的新鲜木薯洗净，以木薯去皮机去除木薯内皮以及外皮，保证没有木薯皮的残留，而影响木薯粉的氰苷含量。
(2)在步骤(1)得到清洗干净的原料，以水为介质，鲜木薯原料与水的配水为1：0.8，进行粉碎，粉碎物的细度通过80目孔径通过率为100％进入下一工序。
(3)在步骤(2)中得到物料利用板框式压滤机进行脱水，板框式压滤机的工作压力在1.8Mpa，压滤时间为10分钟。
(4)在在步骤(3)中得到的物料进行加水，调至物料的含固量度选择在60％，物料的搅拌速度选择在30r/min、搅拌时间在20min后，进入板框式压滤机进行脱水，板框式压滤机的工作压力在1.7Mpa，压滤时间为14分钟。
(5)在步骤(4)分中得到的物料进行加水，调至物料的含固量度选择在60％，物料的搅拌速度选择在35转/分钟、搅拌时间在25分钟。
(6)在步骤(5)得到的进入带式压滤机进行脱水，带式压滤机工作压力为0.4Mpa，连续进料、连续出料。
(7)在步骤(6)得到的原料进行预干燥，预干燥蒸汽压力为6.5公斤，进口温度为135℃，出口温度为75℃，预干燥水分制品水分为33％；接着进行干燥，干燥的蒸汽压力为7.5公斤，进口温度170℃，出口温度40℃以下，水分为13.0％以下。
(8)在步骤(7)中的到的原料进行粉碎，使产品细度通过120目筛100％，得木薯粉。
对比例2
参考专利号CN201410391720的发明专利，“甜木薯全粉的生产制作方法”中的实施例1生产木薯粉，具体为：
将采收2天内的新鲜木薯洗净，以木薯去皮机去除木薯内皮以及外皮，保证没有木薯皮的残留，而影响木薯全粉的氰苷含量。
使用搅碎机进行破碎，重复3次，获得木薯粒，木薯粒的粒度小于3mm。
将木薯粒平摊于洁净彩带条上，移至太阳下自然晒干，晒干木薯粒水分含量低于13.0％。
使用干磨机对自然晒干木薯粒进行粉碎，然后使用50目进行筛分，将被截留部分再次进行干磨，直至物料全部能通过50目筛；再使用超细微粉碎机来对一级破碎所得木薯粗粉进行进一步粉碎，直至所得木薯全粉能全部通过100目筛。
对比例3-1、将水温由50℃改成60℃，其余等同于实施例4。
对比例3-2、将水温由50℃改成25℃，且将超声处理时间由30分钟改成60分钟，其余等同于实施例4。
对比例4、将“以100kHz频率，3000瓦功率超声30分钟”改成“以100kHz频率，4000瓦功率超声25分钟(即，每千克原料对应的超声波的功率为800瓦)”；其余等同于实施例4。
实验1、
灰分含量测定采用《GB 5009.4-2016食品安全国家标准食品中灰分的测定》中的第一法，食品中总灰分的测定；蛋白质含量的测定采用《GB 5009.5-2016食品安全国家标准食品中蛋白质的测定》中的第一法，凯氏定氮法；脂肪含量的测定采用《GB 5009.6-2016食品安全国家标准食品中脂肪的测定》中的第一法，索氏抽提法；可溶性糖含量的检测采用《NY/T 2742-2015水果及制品可溶性糖的测定3,5-二硝基水杨酸比色法》；淀粉含量的测定采用《GB 5009.9-2016食品安全国家标准食品中淀粉的测定》中的第二法，酸水解法；氢氰酸含量的测定采用《GB 5009.36-2016食品安全国家标准食品中氰化物的测定》中的第二法，气相色谱法。
氰苷含量的测定采用LC-MS的方法，具体的操作步骤如下：
(1)称取0.1g试样(精确到0.1mg)于15mL塑料离心管中，加入5mL的甲醇+水(70+30，V+V)，漩涡震荡5s；
(2)将(1)中得到的悬浊液在25℃水中，以500W、53kHz超声辅助提取15min，立即于4200r/min离心10min，取全部上清液；
(3)往残渣中再次加入5mL的甲醇+水(70+30，V+V)，按上述条件提取、离心，合并 两次提取液于100mL容量瓶中，用水定容至刻度，混匀，得提取液；
(4)将(3)中提取液过0.22μm水系滤膜，得待测液；
(5)按下述色谱及质谱条件检测(4)中待测液
色谱条件：
a)色谱柱：Agilient Eclipse Plus C18(50×2.1,1.8μm)；
b)流动相及洗脱条件见表1：
表1、流动相及梯度洗脱条件
Figure PCTCN2019124707-appb-000001
c)柱温：30℃；
d)进样量：5μL；
质谱条件：
a)离子源：ESI源；
b)扫描方式：正离子扫描模式；
c)干燥气温度:325℃；
d)干燥气流量:5L/min；
e)鞘气温度:350℃；
f)鞘气流速:11L/min；
g)雾化气压力:45Psi；
h)毛细管电压:3500V；
i)检测方式：多反应监测模式；
j)监测离子对、碰撞能量见表2：
表2、亚麻苦苷及百脉根苷的保留时间、检测离子对、碰撞能量和裂解电压
Figure PCTCN2019124707-appb-000002
Figure PCTCN2019124707-appb-000003
k)亚麻苦苷与百脉根苷标准物质多反应监测质谱图见图1：
检测实施例1～6、对比例1～2、对比例3-1、对比例3-2、对比例4及对比例5得到的木薯粉以及海南省白沙黎族自治县的SC9、海南省琼中黎族苗族自治县SC6、海南省东方市的GR911的新鲜木薯的灰分、蛋白质、脂肪、淀粉、氰苷、氢氰酸的含量，其中实施例1～4、对比例1～2、对比例3-1、对比例3-2、对比例4及对比例5的木薯品种为甜木薯，实施例5～6的木薯品种为苦木薯，结果均为占干重含量，见表3。采用SPSS 20.0统计软件包进行数据处理与分析，结果以均数±标准差(mean±SD)表示，组间均数比较用t检验，P<0.05为差异有统计学意义。与相应的鲜木薯相比，实施例1～4的木薯粉样品的氰苷、氢氰酸含量均有显著降低，除实施例4的可溶性糖外，其余营养品质指标无显著变化，可溶性糖损失较对比例1小；虽然对比例1的木薯粉的氰苷、氢氰酸含量同样有显著降低，但是灰分、脂肪、蛋白质及可溶性糖的含量亦有显著的损失，其中可溶性糖的损失尤为明显，且氰苷和氢氰酸检测结果方差大，表明该方法稳定性较差；对比例2的灰分、淀粉、蛋白质、脂肪、可溶性糖含量与相应的鲜木薯相比没有统计学上的显著变化，但是对比例2因为没有额外降解氰苷的处理，其氰苷、氢氰酸含量与鲜木薯无显著差异；实施例5～6的氰苷、氢氰酸含量均显著低于鲜木薯，说明此方法对甜木薯、苦木薯均有降低其氰苷含量的效果；对比例3-1、对比例3-2及对比例4的氰苷、氢氰酸含量均高于实施例1～4，过高的功率、温度或处理时间过长对酶的活性可能有抑制作用。
表3木薯粉及鲜木薯营养品质检测结果表
Figure PCTCN2019124707-appb-000004
Figure PCTCN2019124707-appb-000005
注：#表示该指标与其相同品种、相同产地的鲜木薯相比较，P<0.05。
最后，还需要注意的是，以上列举的仅是本发明的若干个具体实施例。显然，本发明不限于以上实施例，还可以有许多变形。本领域的普通技术人员能从本发明公开的内容直接导出或联想到的所有变形，均应认为是本发明的保护范围。

Claims (6)

  1. 低氰苷的木薯粉的制备方法，新鲜木薯经清洗、去皮、切碎，所得的木薯粒、木薯丝或木薯浆作为原料，其特征是还包括以下步骤：
    将原料浸没在温度为35～50℃温水中进行超声波处理10～30分钟，超声波的频率为20kHz～100kHz，得超声波处理后原料；
    每千克原料对应的超声波的功率为100～600瓦；
    将超声波处理后原料经干燥、粉碎，得低氰苷的木薯粉，所得木薯粉总氰苷含量＜15mg/kg，氢氰酸含量＜2mg/kg；
    其中，木薯粒、木薯丝或木薯浆的制备方法为：
    a、新鲜木薯在采收后，以带压力的水清洗去除其表面残留的土壤，然后以木薯去皮机或人工去除外皮以及内皮，保留木薯肉；
    b、使用搅碎机将木薯肉切碎成木薯粒、以切丝机将木薯肉切成木薯丝或以粉碎机将木薯肉打碎成匀浆，备用。
  2. 根据权利要求1所述的低氰苷的木薯粉的制备方法，其特征是：每千克原料对应的超声波的功率为600瓦。
  3. 根据权利要求1所述的低氰苷的木薯粉的制备方法，其特征是：干燥至含水率≤13.0％；粉碎至80目筛网。
  4. 根据权利要求3所述的低氰苷的木薯粉的制备方法，其特征是：所述干燥为自然晒干或热风烘干，当为热风烘干时，温度≤70℃。
  5. 根据权利要求1～4任一所述的低氰苷的木薯粉的制备方法，其特征是：所述鲜木薯为甜木薯或苦木薯。
  6. 根据权利要求5所述的低氰苷的木薯粉的制备方法，其特征是：
    甜木薯为SC9、SC12、SC6068、GR9、GR10、GR891、面包木薯、利民1号；
    苦木薯为SC6、SC7、SC8、SC124、SC201、GR4、GR911、F499。
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