CN111718598A - 一种低多环芳烃辣椒红的生产方法 - Google Patents
一种低多环芳烃辣椒红的生产方法 Download PDFInfo
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- 239000001688 paprika extract Substances 0.000 title claims abstract description 54
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- 235000018889 capsanthin Nutrition 0.000 title claims abstract description 51
- WRANYHFEXGNSND-LOFNIBRQSA-N capsanthin Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1=C(C)CC(O)CC1(C)C)C=CC=C(/C)C=CC(=O)C2(C)CCC(O)C2(C)C WRANYHFEXGNSND-LOFNIBRQSA-N 0.000 title claims abstract description 51
- VYIRVAXUEZSDNC-TXDLOWMYSA-N (3R,3'S,5'R)-3,3'-dihydroxy-beta-kappa-caroten-6'-one Chemical compound C([C@H](O)CC=1C)C(C)(C)C=1/C=C/C(/C)=C/C=C/C(/C)=C/C=C/C=C(C)C=CC=C(C)C=CC(=O)[C@]1(C)C[C@@H](O)CC1(C)C VYIRVAXUEZSDNC-TXDLOWMYSA-N 0.000 title claims abstract description 50
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 title claims abstract description 22
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- FMMWHPNWAFZXNH-UHFFFAOYSA-N Benz[a]pyrene Chemical compound C1=C2C3=CC=CC=C3C=C(C=C3)C2=C2C3=CC=CC2=C1 FMMWHPNWAFZXNH-UHFFFAOYSA-N 0.000 claims abstract description 25
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- 235000007862 Capsicum baccatum Nutrition 0.000 description 2
- VQEONGKQWIFHMN-UHFFFAOYSA-N Nordihydrocapsaicin Chemical compound COC1=CC(CNC(=O)CCCCCC(C)C)=CC=C1O VQEONGKQWIFHMN-UHFFFAOYSA-N 0.000 description 2
- JKQXZKUSFCKOGQ-LQFQNGICSA-N Z-zeaxanthin Natural products C([C@H](O)CC=1C)C(C)(C)C=1C=CC(C)=CC=CC(C)=CC=CC=C(C)C=CC=C(C)C=CC1=C(C)C[C@@H](O)CC1(C)C JKQXZKUSFCKOGQ-LQFQNGICSA-N 0.000 description 2
- QOPRSMDTRDMBNK-RNUUUQFGSA-N Zeaxanthin Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1=C(C)CCC(O)C1(C)C)C=CC=C(/C)C=CC2=C(C)CC(O)CC2(C)C QOPRSMDTRDMBNK-RNUUUQFGSA-N 0.000 description 2
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- KBPHJBAIARWVSC-XQIHNALSSA-N trans-lutein Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1=C(C)CC(O)CC1(C)C)C=CC=C(/C)C=CC2C(=CC(O)CC2(C)C)C KBPHJBAIARWVSC-XQIHNALSSA-N 0.000 description 2
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- 125000003158 alcohol group Chemical group 0.000 description 1
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- XJQPQKLURWNAAH-UHFFFAOYSA-N dihydrocapsaicin Chemical compound COC1=CC(CNC(=O)CCCCCCC(C)C)=CC=C1O XJQPQKLURWNAAH-UHFFFAOYSA-N 0.000 description 1
- RBCYRZPENADQGZ-UHFFFAOYSA-N dihydrocapsaicin Natural products COC1=CC(COC(=O)CCCCCCC(C)C)=CC=C1O RBCYRZPENADQGZ-UHFFFAOYSA-N 0.000 description 1
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- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
Classifications
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L19/00—Products from fruits or vegetables; Preparation or treatment thereof
- A23L19/09—Mashed or comminuted products, e.g. pulp, purée, sauce, or products made therefrom, e.g. snacks
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
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- A—HUMAN NECESSITIES
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- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
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- C09B67/0096—Purification; Precipitation; Filtration
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Abstract
本发明公开了一种低多环芳烃辣椒红的生产方法,该方法包括:将辣椒干燥、粉碎、造粒、浸提、过滤,得到辣椒红色素浸出液;色素浸出液经动态液‑液萃取脱辣后,经低压层析柱吸附后得到低苯并芘色素溶液;低苯并芘色素溶液经浓缩后得到低苯并芘辣椒红产品。本发明首次采用低压层析柱的方法在提取过程中以动态吸附的方式对辣椒红脱辣浸提液进行苯并芘的脱除,从而达到脱除苯并芘的目的,同时基于辣椒红在溶剂中被所用层析柱吸附率极少,对辣椒红的得率无显著影响。本发明采用物理吸附的方式,避免了外源物质的引入或化学处理造成产品本身性质的改变;同时简化了工艺流程,操作简单,成本低,便于工业化生产,为天然色素安全指标的控制提供了参考。
Description
技术领域
本发明属于食品添加剂精制技术领域,具体涉及一种低多环芳烃辣椒红的生产方法。
背景技术
辣椒红色素(Paprika red pigment)是从成熟红辣椒果皮中提取的天然红色素,主要组分为辣椒红素(Capsanthin)、辣椒玉红素(Capsorubin)、β-胡萝卜素(β-carotene)和玉米黄质(zeaxanthin)等,其显色强度是其他色素的10倍,广泛于食品、饮料、化妆品及医药等行业,是国际上公认的最好的A类红色素。辣椒红色素是红辣椒中呈鲜艳红色的部分。
传统的辣椒红色素主要制备工艺:将辣椒干燥、粉碎,采用溶剂浸提法得到辣椒红色素的粗提液,然后再采用碱液或乙醇等溶剂萃取脱除辣味物质,并蒸馏出其中的溶剂得到精制的辣椒红色素。
随着人们对食品安全意识的不断提升,食品添加剂安全指标的管控也越来越严格。目前市场上关于辣椒红中产品中PAHs和苯并芘的管控逐渐受到客户的重视。传统工艺生产的辣椒红产品PAHs含量达到100ppb以上,苯并芘单项达到30ppb以上,远远无法满足PHAs<50ppb,苯并芘<10ppb的要求。多环芳烃类物质的含量如果得不到有效管控,势必会影响到未来辣椒红产业化的发展。而目前并未有关于辣椒红多环芳烃类物质控制的相关文献报道,无法实现保证辣椒红得率的前提下,达到多环芳烃类物质有效分离的目的。
发明内容
为了克服背景技术所述的不足,本发明提供一种低多环芳烃辣椒红的生产方法,本发明首次采用低压层析柱的方法在提取过程中以动态吸附的方式对辣椒红脱辣浸提液进行苯并芘的脱除,从而达到脱除苯并芘的目的,同时基于辣椒红在溶剂中不会被所用层析柱吸附,对辣椒红的得率无显著影响。
本发明提供的生产方法包括如下步骤:将辣椒浸提、过滤,得到辣椒红色素浸出液;色素浸出液经动态液-液萃取脱辣后,经低压层析柱吸附后得到低苯并芘色素溶液;低苯并芘色素溶液浓缩。
本发明提供的生产方法优选技术方案包括如下步骤:
将辣椒颗粒和萃取溶剂在平转式浸出器中混合,得到色素浸出液;将所述色素浸出液与乙醇溶液在液-液连续萃取器中混合,脱去辣味物质,得色素脱辣浸出液;将所述色素脱辣浸出液经过低压层析柱进行吸附处理后得到低苯并芘色素液;将所述低苯并芘色素液进行减压浓缩。
本发明提供的生产方法更优选的技术方案为:
(1)制备原料:将成熟的辣椒在30-50℃的条件下烘干,粉碎,造粒,得到辣椒颗粒;
(2)浸提辣椒红:将辣椒颗粒输送进入到连续式浸出器内部,在输送过程中通过喷淋管喷淋萃取溶剂,使萃取溶剂与辣椒颗粒混合均匀,通过萃取溶剂将辣椒红浸提出来,得到色素浸出液;
(3)动态脱辣:将所述色素浸出液与乙醇溶液在液-液连续萃取器中混合,脱去辣味物质,得色素脱辣浸出液;
(4)动态吸附:将所述色素脱辣浸出液经过低压层析柱进行吸附处理后得到低苯并芘色素液;
(5)浓缩:将所述低苯并芘色素液进行减压浓缩得到低苯并芘辣椒红产品。
优选的,在步骤(2)中,使用的连续式浸出器为平转式浸出器、环形浸出器、卫星式浸出器或履带式浸出器;使用的萃取溶剂为含有4-7个碳的烷烃类溶剂,优选为植物油抽提溶剂,萃取溶剂喷淋时的温度为40-50℃,喷淋量为1000-1500L/h。
优选的,在步骤(3)中,色素浸出液和醇类脱辣剂温度可以为30℃~50℃,色素浸出液流量可以为0.5m3/h~1.5m3/h,醇类脱辣剂的流量可以为1m3/h~3m3/h,乙醇溶液浓度体积百分数为40%~90%;液-液连续萃取器中上层为色素浸出液,下层为醇类溶剂,醇类溶剂可以萃取色素浸出液中的辣椒素、二氢辣素和降二氢辣素等辣味物质。脱除辣味物质后,得到脱辣的色素浸出液。
优选的,在步骤(4)中,低压柱层析所用填料为硅胶、硅藻土、白土、高岭土和活性炭的两种以上的混合;层析柱填料粒径大小为20目~300目;层析柱填料用量与辣椒颗粒投料量的比例为1:1~50。
优选的,在步骤(5)中,所述浓缩的温度为40℃~100℃,浓缩的压力为-0.03Mpa~-0.06Mpa;
优选的,还包括步骤(6)脱溶剂残留,进行脱溶剂残留处理。在步骤(6)中,脱溶剂残留温度为60~100℃,脱溶剂残留压力为-0.03~-0.08mPa,脱溶剂残留时间为0.5~5h。
本发明提供的更优选的生产方法为:步骤(2)使用的连续式浸出器为平转式浸出器、环形浸出器、卫星式浸出器或履带式浸出器;使用的萃取溶剂为植物油抽提溶剂,萃取溶剂喷淋时的温度为40-50℃,喷淋量为1000-1500L/h;步骤(3)中,所述的色素浸出液与乙醇溶液在液-液连续萃取器中混合,色素浸出液和乙醇溶液温度为30℃~50℃;色素浸出液流量可以为0.5m3/h~1.5m3/h,乙醇溶液的流量为1m3/h~3m3/h;所用乙醇溶液浓度体积百分数为40%~90%;步骤(4)中,低压层析柱所用填料为硅藻土、白土、高岭土和活性炭的两种以上混合;填料粒径大小为20目~300目;低压层析柱其填料用量与辣椒颗粒投料量的比例为1:1~50;步骤(5)中,浓缩的温度为40℃~100℃,压力为-0.03Mpa~-0.06Mpa;还包括步骤(6)脱溶剂残留:进行脱溶剂残留处理;其中,脱溶剂残留温度为60~100℃,压力为-0.03~-0.08mPa,时间为0.5~5h。
本发明与现有技术相比,其优点在于:本发明首次采用低压柱层析的方法在提取过程中以动态吸附的方式对辣椒红脱辣浸提液进行多环芳烃类物质的脱除,从而达到低多环芳烃的高品质辣椒红生产的目的,同时基于辣椒红在溶剂中被所用层析柱吸附率极低,对辣椒红的得率无显著影响。本发明采用物理吸附的方式,避免了外源物质的引入或化学处理造成产品本身性质的改变;另外,生产过程中直接对脱辣液体进行吸附分离,简化了工艺流程,操作简单,工艺成本低,便于工业化生产,为天然色素安全指标的控制提供了参考。
具体实施方式
实施例1
a)将成熟的辣椒在30℃的条件下烘干,粉碎,造粒,得到辣椒颗粒,取3000Kg辣椒颗粒(色价为16.6),采用平转式连续浸出器,以植物油抽提溶剂作为萃取溶剂,喷淋温度为45℃,喷淋量为1000L/h,萃取得到色素浸出液。将所述色素浸出液与70%乙醇在液-液萃取器中于45℃,200r/min条件下混合脱除辣味物质,色素浸出液流量为1m3/h,70%乙醇流量为2m3/h,得到脱辣的色素浸出液。
b)将所述脱辣的色素浸出液以1Bv/h的流速进行以100目活性炭和100目硅藻土按5:1混合作为填料的层析柱吸附,层析柱填料的用量为30kg,收集下端口流出液,得到脱除多环芳烃类物质的辣椒红溶液。
c)将上述脱除多环芳烃类物质的辣椒红溶液于60℃,-0.08mPa的条件下减压浓缩回收溶剂,并于78℃、-0.08mPa的条件下脱溶剂残留处理3.5h,得到脱除多环芳烃类物质的辣椒红183.8kg。
实施例2
a)将成熟的辣椒在30℃的条件下烘干,粉碎,造粒,得到辣椒颗粒,取3000Kg辣椒颗粒(色价为17.6),采用平转式连续浸出器,以植物油抽提溶剂作为萃取溶剂,喷淋温度为45℃,喷淋量为1000L/h,萃取得到色素浸出液。将所述色素浸出液与70%乙醇在液-液萃取器中于45℃,200r/min条件下混合脱除辣味物质,色素浸出液流量为1m3/h,70%乙醇流量为2m3/h,得到脱辣的色素浸出液。
b)将所述脱辣的色素浸出液以1.5Bv/h的流速进行以100目活性炭、活性白土和硅藻土按4:1:1混合作为填料的层析柱吸附,层析柱填料的用量为50kg,收集下端口流出液,得到脱除多环芳烃类物质的辣椒红溶液。
c)将上述脱除多环芳烃类物质的辣椒红溶液于70℃,-0.07mPa的条件下减压浓缩回收溶剂,并于74℃、-0.07mPa的条件下脱溶剂残留处理4h,得到脱除多环芳烃类物质的辣椒红170.9kg。
实施例3
a)将成熟的辣椒在30℃的条件下烘干,粉碎,造粒,得到辣椒颗粒,取3000Kg辣椒颗粒(色价为16.9),采用平转式连续浸出器,以植物油抽提溶剂作为萃取溶剂,喷淋温度为45℃,喷淋量为1000L/h,萃取得到色素浸出液。将所述色素浸出液与70%乙醇在液-液萃取器中于45℃,200r/min条件下混合脱除辣味物质,色素浸出液流量为1m3/h,70%乙醇流量为2m3/h,得到脱辣的色素浸出液。
b)将所述脱辣的色素浸出液以1.2Bv/h的流速进行以200目活性炭和80目活性白土按7:1混合作为填料的层析柱吸附,层析柱填料的用量为70kg,收集下端口流出液,得到脱除多环芳烃类物质的辣椒红溶液。
c)将上述脱除多环芳烃类物质的辣椒红溶液于74℃,-0.09mPa的条件下减压浓缩回收溶剂,并于74℃、-0.08mPa的条件下脱溶剂残留处理3h,得到脱除多环芳烃类物质的辣椒红194.1kg。
对比例1
a)将成熟的辣椒在30℃的条件下烘干,粉碎,造粒,得到辣椒颗粒,取3000Kg辣椒颗粒(色价为16.8),采用平转式连续浸出器,以植物油抽提溶剂作为萃取溶剂,喷淋温度为45℃,喷淋量为1000L/h,萃取得到色素浸出液。将所述色素浸出液与70%乙醇在液-液萃取器中于45℃,200r/min条件下混合脱除辣味物质,色素浸出液流量为1m3/h,70%乙醇流量为2m3/h,得到脱辣的色素浸出液。
b)将上述脱辣的色素浸出液于60℃,-0.08mPa的条件下减压浓缩回收溶剂,并于78℃、-0.09mPa的条件下脱溶剂残留处理3h,得到辣椒红精制料188.9kg。
对比例2
取3000Kg辣椒颗粒(色价为16.5),采用平转式连续浸出器,以植物油抽提溶剂作为萃取溶剂,喷淋温度为40℃,喷淋量为1500L/h,萃取得到色素浸出液。将所述色素浸出液经真空浓缩后得到辣椒红浓缩液250.86Kg,真空浓缩的压力为-0.06MPa。向辣椒红浓缩液中加入70%的乙醇500Kg进行脱辣处理,于75℃、-0.08mPa的条件下脱溶剂残留处理3.5h,得到辣椒红精制料190.6kg。
对实施例和比较例制备的辣椒红进行检测,吸光度按照GB/10783-2008的方法进行检测,吸光比为同一辣椒红色素溶液A470nm与A454nm的比值,PHAs采用HPLC的方法进行检测。检测结果如表1所示。
表1实施例1~3和比较例制备的辣椒红色素检测结果对比
根据表1的结果可知,实施例与比较例制备的辣椒红色价和得率接近,但实施例制备的辣椒红PHAs和苯并芘均显著低于比较例。表明实施例的方法在保证产品得率的前提下对PHAs和苯并芘具有良好的去除效果。
最后应说明的是:显然,上述实施例仅是为清楚地说明本发明所作的举例,而并非对实施方式的限定。对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引申出的显而易见的变化或变动仍处于本发明的保护范围之中。
Claims (10)
1.一种低多环芳烃辣椒红的生产方法,其特征在于,所述的方法包括如下步骤:
将辣椒浸提、过滤,得到辣椒红色素浸出液;色素浸出液经动态液-液萃取脱辣后,经低压层析柱吸附后得到低苯并芘色素溶液;低苯并芘色素溶液浓缩。
2.根据权利要求1所述的生产方法,其特征在于,所述的方法包括如下步骤:
将辣椒颗粒和萃取溶剂在平转式浸出器中混合,得到色素浸出液;将所述色素浸出液与乙醇溶液在液-液连续萃取器中混合,脱去辣味物质,得色素脱辣浸出液;将所述色素脱辣浸出液经过低压层析柱进行吸附处理后得到低苯并芘色素液;将所述低苯并芘色素液进行减压浓缩。
3.根据权利要求2所述的生产方法,其特征在于,所述的方法包括如下步骤:
(1)制备原料:将成熟的辣椒在30-50℃的条件下烘干,粉碎,造粒,得到辣椒颗粒;
(2)浸提辣椒红:将辣椒颗粒输送进入到连续式浸出器内部,在输送过
(3)程中通过喷淋管喷淋萃取溶剂,使萃取溶剂与辣椒颗粒混合均匀,通过萃取溶剂将辣椒红浸提出来,得到色素浸出液;动态脱辣:将所述色素浸出液与乙醇溶液在液-液连续萃取器中混合,脱去辣味物质,得色素脱辣浸出液;
(4)动态吸附:将所述色素脱辣浸出液经过低压层析柱进行吸附处理后得到低苯并芘色素液;
(5)浓缩:将所述低苯并芘色素液进行减压浓缩。
4.根据权利要求3所述的生产方法,其特征在于,步骤(2)中,使用的连续式浸出器为平转式浸出器、环形浸出器、卫星式浸出器或履带式浸出器;使用的萃取溶剂为4~7个碳的烷烃类溶剂,萃取溶剂喷淋时的温度为40-50℃,喷淋量为1000-1500L/h。
5.根据权利要求3所述的生产方法,其特征在于,步骤(3)中,所述的色素浸出液与乙醇溶液在液-液连续萃取器中混合,色素浸出液和乙醇溶液温度为30℃~50℃;色素浸出液流量可以为0.5m3/h~1.5m3/h,乙醇溶液的流量为1m3/h~3m3/h;所用乙醇溶液浓度体积百分数为40%~90%。
6.根据权利要求3所述的生产方法,其特征在于,步骤(4)中,低压层析柱所用填料为硅藻土、白土、高岭土和活性炭的两种以上混合;填料粒径大小为20目~300目;低压层析柱其填料用量与辣椒颗粒投料量的比例为1:1~50。
7.根据权利要求3所述的生产方法,其特征在于,步骤(5)中,浓缩的温度为40℃~100℃,压力为-0.03Mpa~-0.06Mpa。
8.根据权利要求3所述的生产方法,其特征在于,还包括步骤(6)脱溶剂残留:进行脱溶剂残留处理;其中,脱溶剂残留温度为60~100℃,压力为-0.03~-0.08mPa,时间为0.5~5h。
9.根据权利要求3所述的生产方法,其特征在于,步骤(2)中,使用的连续式浸出器为平转式浸出器、环形浸出器、卫星式浸出器或履带式浸出器;使用的萃取溶剂为植物油抽提溶剂,萃取溶剂喷淋时的温度为40-50℃,喷淋量为1000-1500L/h;步骤(3)中,所述的色素浸出液与乙醇溶液在液-液连续萃取器中混合,色素浸出液和乙醇溶液温度为30℃~50℃;色素浸出液流量可以为0.5m3/h~1.5m3/h,乙醇溶液的流量为1m3/h~3m3/h;所用乙醇溶液浓度体积百分数为40%~90%;步骤(4)中,低压层析柱所用填料为硅藻土、白土、高岭土和活性炭的两种以上混合;填料粒径大小为20目~300目;低压层析柱其填料用量与辣椒颗粒投料量的比例为1:1~50;步骤(5)中,浓缩的温度为40℃~100℃,压力为-0.03Mpa~-0.06Mpa;还包括步骤(6)脱溶剂残留:进行脱溶剂残留处理;其中,脱溶剂残留温度为60~100℃,压力为-0.03~-0.08mPa,时间为0.5~5h。
10.根据权利要求3所述的生产方法,其特征在于包括如下步骤:
a)将成熟的辣椒在30℃的条件下烘干,粉碎,造粒,得到辣椒颗粒,取3000Kg辣椒颗粒,采用平转式连续浸出器,以植物油抽提溶剂作为萃取溶剂,喷淋温度为45℃,喷淋量为1000L/h,萃取得到色素浸出液;将所述色素浸出液与70%乙醇在液-液萃取器中于45℃,200r/min条件下混合脱除辣味物质,色素浸出液流量为1m3/h,70%乙醇流量为2m3/h,得到脱辣的色素浸出液;
b)将所述脱辣的色素浸出液以1.2Bv/h的流速进行以200目活性炭和80目活性白土按7:1混合作为填料的层析柱吸附,层析柱填料的用量为70kg,收集下端口流出液,得到脱除多环芳烃类物质的辣椒红溶液;
c)将上述脱除多环芳烃类物质的辣椒红溶液于74℃,-0.09mPa的条件下减压浓缩回收溶剂,并于74℃、-0.08mPa的条件下脱溶剂残留处理3h,得到脱除多环芳烃类物质的辣椒红。
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