CN107008226B - 花生油中黄曲霉素和苯并芘的去除工艺 - Google Patents
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Abstract
本发明属于油脂技术领域，公开了花生油中黄曲霉素和苯并芘的去除工艺，其包括如下步骤：步骤1）制备吸附剂，步骤2）吸附、离心，步骤3）吸附剂再生。本发明工艺能够有效地脱除黄曲霉素和苯并芘，操作步骤简单可行，适合工业化推广使用。
Description
技术领域
本发明属于油脂技术领域，具体涉及花生油中黄曲霉素和苯并芘的去除工艺。
背景技术
黄曲霉毒素主要是由黄曲霉菌和寄生曲霉菌产生的一类有毒二次代谢产物。迄今为止，已经发现的黄曲霉毒素包含黄曲霉毒素B1、B2等至少17种结构相似、特征已知的化合物。它具有很强的致突变、致畸和致癌作用，其中又以黄曲霉毒素B1的毒性最强，其毒性是氰化钾的10倍，砒霜的68倍，被世界卫生组织列为已知的最强致癌化学物质之一。花生是最容易遭受黄曲霉菌感染的农作物之一，影响以花生为生产原材料的花生油品质的主要因素也是黄曲霉毒素。国家对粮油制品中黄曲霉毒素含量控制极为严格。而目前新榨的花生油中，黄曲霉毒素的含量往往偏高，达不到国内食用或出口的要求。
苯并芘（Benzoapyrene），化学式：C20H12，英文表示BaP，是一种五环多环芳香烃类。结晶为黄色固体。这种物质是在300到600°C之间的不完全燃烧状态下产生。苯并芘存在于煤焦油中，而煤焦油可见于汽车废气、烟草与木材燃烧产生的烟，以及炭烤食物中。苯并芘为一种突变原和致癌物质，从18世纪以来，便发现与许多癌症有关。苯并芘在体内的代谢物二羟环氧苯并芘，产生致癌性的物质。花生油在加工过程中，高温易产生苯并芘。
现有技术已经有利用脱色剂来去除黄曲霉素和苯并芘的方法，比较常用的是活性白土，例如，吸附法脱除芝麻油中苯并芘及脱色效果研究，粮油食品科技2013年，其采用了活性白土对苯并芘进行脱除，但是苯并芘的脱除率仅为30%左右，采用活性炭和活性白土结合的方式，可以达到90%左右的脱除率，但是其脱除黄曲霉素的效果较差；无法将黄曲霉素和苯并芘二者同时有效地脱除。
开发一种花生油中黄曲霉素和苯并芘的去除工艺是油品精制行业需要解决的技术问题。申请人玉皇集团公司作为油品加工的龙头企业，率先进行了该研究。
发明内容
为了克服现有技术的缺陷，本发明提出了花生油中黄曲霉素和苯并芘的去除工艺，其能够有效地去除黄曲霉素和苯并芘，操作方式简单可行。
本发明是通过如下技术方案来实现的：
花生油中黄曲霉素和苯并芘的去除工艺，其包括如下步骤：步骤1）制备吸附剂，步骤2）吸附、离心，步骤3）吸附剂再生。
具体地，所述步骤1）制备吸附剂，包括如下步骤：
a）往硅藻土中加入两倍重量的质量分数为10%的盐酸溶液，超声波振荡30min，再添加占硅藻土1%重量份的十二烷基磺酸钠，继续超声波振荡30min，然后离心收集沉淀；
b）将方解石、高岭石以及海泡石按照5:3:2的质量比投入到粉碎机中粉碎处理，然后研磨成100目的粉末；
c）将a）所得沉淀和b）所得粉末按照2:3的质量比投入到搅拌器中，500rpm搅拌10min，得到基料，再与聚苯乙烯微球按照1:1的质量比添加到造粒机中，接着加入占基料质量30%的浓度为8wt%的聚乙烯醇水溶液，制成粒径为1mm的球状物；
d）将c）所得球状物置于80℃的烘箱中干燥60min，再投入到烧结炉中进行烧结，升温速率为10℃/分，烧结温度750℃，保温30min，取出，自然冷却至室温，即得吸附剂。
具体地，所述步骤2）吸附、离心，包括如下步骤：往花生油中添加1-2%质量份的吸附剂，加热至70℃，保温条件下，于100rpm搅拌30min，再静置60min，然后经过离心分离出沉淀物。
具体地，所述步骤3）吸附剂再生，包括如下步骤：将步骤2）所得沉淀物投入到50-60℃的水中浸泡30min，取出，置于350-400℃煅烧3-5min，自然冷却。
本发明取得的有益效果主要包括但是并不限于以下几个方面：
本发明通过改性吸附剂可以同时去除黄曲霉素和苯并芘，去除效果好，大幅度提高了油品质量，杜绝了安全隐患；
本发明通过酸化和表面活性剂处理，用长链阳离子取代了硅藻土之间的阳离子，使得硅藻土层间距变大，同时硅藻土表面吸附了部分无机阳离子，使得疏水性提高，增加了吸附能力；
本发明利用造孔剂制备成大孔径颗粒吸附材料，比表面积大，吸附能力强；
本发明的吸附剂粒径较大，结构坚固，不会破裂，较容易从油品中脱除，保证了油品中无残留，还可以重复利用，有效地避免了材料浪费，给企业节约了成本。
具体实施方式
为了使本技术领域的人员更好地理解本申请中的技术方案，下面将结合本申请具体实施例，对本发明进行更加清楚、完整地描述，显然，所描述的实施例仅仅是本申请一部分实施例，而不是全部的实施例。基于本申请中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都应当属于本发明保护的范围。
实施例1
花生油中黄曲霉素和苯并芘的去除工艺，其包括如下步骤：
步骤1）制备吸附剂：
a）往硅藻土中加入两倍重量的质量分数为10%的盐酸溶液，超声波振荡30min，再添加占硅藻土1%重量份的十二烷基磺酸钠，继续超声波振荡30min，然后离心收集沉淀；超声波功率为2000w；
b）将方解石、高岭石以及海泡石按照5:3:2的质量比投入到粉碎机中粉碎处理，然后研磨成100目的粉末；
c）将a）所得沉淀和b）所得粉末按照2:3的质量比投入到搅拌器中，500rpm搅拌10min，得到基料，再与聚苯乙烯微球按照1:1的质量比添加到造粒机中，接着加入占基料质量30%的浓度为8wt%的聚乙烯醇水溶液，制成粒径为1mm的球状物；
d）将c）所得球状物置于80℃的烘箱中干燥60min，再投入到烧结炉中进行烧结，升温速率为10℃/分，烧结温度750℃，保温30min，取出，自然冷却至室温，即得吸附剂；
步骤2）吸附、离心：往花生油中添加2%质量份的吸附剂，加热至70℃，保温条件下，于100rpm搅拌30min，再静置60min，然后经过离心分离出沉淀物；
步骤3）吸附剂再生：将步骤2）所得沉淀物投入到50-60℃的水中浸泡30min，取出，置于350-400℃煅烧3-5min，自然冷却。
实施例2
花生油中黄曲霉素和苯并芘的去除工艺，其包括如下步骤：
步骤1）制备吸附剂：
a）往硅藻土中加入两倍重量的质量分数为10%的盐酸溶液，超声波振荡30min，再添加占硅藻土1%重量份的十二烷基磺酸钠，继续超声波振荡30min，然后离心收集沉淀；超声波功率为2000w；
b）将方解石、高岭石以及海泡石按照5:3:2的质量比投入到粉碎机中粉碎处理，然后研磨成100目的粉末；
c）将a）所得沉淀和b）所得粉末按照2:3的质量比投入到搅拌器中，500rpm搅拌10min，得到基料，再与聚苯乙烯微球按照1:1的质量比添加到造粒机中，接着加入占基料质量30%的浓度为8wt%的聚乙烯醇水溶液，制成粒径为1mm的球状物；
d）将c）所得球状物置于80℃的烘箱中干燥60min，再投入到烧结炉中进行烧结，升温速率为10℃/分，烧结温度750℃，保温30min，取出，自然冷却至室温，即得吸附剂；
步骤2）吸附、离心：往花生油中添加1%质量份的吸附剂，加热至70℃，保温条件下，于100rpm搅拌30min，再静置60min，然后经过离心分离出沉淀物；
步骤3）吸附剂再生：将步骤2）所得沉淀物投入到50-60℃的水中浸泡30min，取出，置于350-400℃煅烧3-5min，自然冷却。
实施例3
本发明吸附剂对黄曲霉素和苯并芘的性能测试：
油品选择：
选择黄曲霉素和苯并芘含量不同的两个批次的花生油样品进行测试；
样品一：黄曲霉素Bl含量为50μg/L，苯并芘含量为20μg/L；
样品二：黄曲霉素Bl含量为100μg/L，苯并芘含量为10μg/L。
吸附剂选择：
吸附剂分别选择活性白土、活性炭、沸石以及本发明实施例1的吸附剂；操作工艺同实施例1。
测试方法：
离心分离去除沉淀后，用酶联免疫法测试油品中黄曲霉素Bl的含量；液相色谱-串联质谱法测试油品中苯并芘的含量。样品一的试验结果见表1，样品二的试验结果见表2：
表1
| 组别 | 活性白土 | 活性炭 | 沸石 | 实施例1 |
| 未处理前黄曲霉素浓度μg/L | 50 | 50 | 50 | 50 |
| 处理后黄曲霉素浓度μg/L | 2.7 | 3.8 | 4.6 | 0.4 |
| 未处理前苯并芘浓度μg/L | 20 | 20 | 20 | 20 |
| 处理后苯并芘浓度μg/L | 4.67 | 1.68 | 3.54 | 0.51 |
表2
| 组别 | 活性白土 | 活性炭 | 沸石 | 实施例1 |
| 未处理前黄曲霉素浓度μg/L | 100 | 100 | 100 | 100 |
| 处理后黄曲霉素浓度μg/L | 5.9 | 8.4 | 10.1 | 1.2 |
| 未处理前苯并芘浓度μg/L | 10 | 10 | 10 | 10 |
| 处理后苯并芘浓度μg/L | 2.37 | 0.91 | 1.69 | 0.23 |
结论：本发明吸附剂能够有效地脱除黄曲霉素和苯并芘，效果明显优于现有技术常用的活性白土、活性炭以及沸石；吸附剂使用后，可通过简单工艺再生，避免了原料浪费，减轻了企业成本。
在本说明书的描述中，参考术语“一个实施例”、“一些实施例”、“示例”、“具体示例”、或“一些示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中，对上述术语的示意性表述不必须针对的是相同的实施例或示例。尽管上面已经示出和描述了本发明的实施例，可以理解的是，上述实施例是示例性的，不能理解为对本发明的限制，本领域的普通技术人员在本发明的范围内可以对上述实施例进行变化、修改、替换和变型。
Claims (1)
1.花生油中黄曲霉素和苯并芘的去除工艺，其包括如下步骤
步骤1）制备吸附剂：
a）往硅藻土中加入两倍重量的质量分数为10%的盐酸溶液，超声波振荡30min，再添加占硅藻土1%重量份的十二烷基磺酸钠，继续超声波振荡30min，然后离心收集沉淀；
b）将方解石、高岭石以及海泡石按照5:3:2的质量比投入到粉碎机中粉碎处理，然后研磨成100目的粉末；
c）将a）所得沉淀和b）所得粉末按照2:3的质量比投入到搅拌器中，500rpm搅拌10min，得到基料，再与聚苯乙烯微球按照1:1的质量比添加到造粒机中，接着加入占基料质量30%的浓度为8wt%的聚乙烯醇水溶液，制成粒径为1mm的球状物；
d）将c）所得球状物置于80℃的烘箱中干燥60min，再投入到烧结炉中进行烧结，升温速率为10℃/分，烧结温度750℃，保温30min，取出，自然冷却至室温，即得吸附剂；
步骤2）吸附、离心，包括如下步骤：往花生油中添加1-2%质量份的吸附剂，加热至70℃，保温条件下，于100rpm搅拌30min，再静置60min，然后经过离心分离出沉淀物；
步骤3）吸附剂再生，包括如下步骤：将步骤2）所得沉淀物投入到50-60℃的水中浸泡30min，取出，置于350-400℃煅烧3-5min，自然冷却。
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