CN111588012A - 一种低金属残留防结块蜂胶粉的制备方法 - Google Patents
一种低金属残留防结块蜂胶粉的制备方法 Download PDFInfo
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- A—HUMAN NECESSITIES
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- A—HUMAN NECESSITIES
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Abstract
本发明公开了一种低金属残留防结块蜂胶粉的制备方法,属于蜂胶类产品制备技术领域。本发明用聚乙烯亚胺水溶液作为硅胶的浸渗液,作为螯合材料对金属离子能产生很强的螯合作用,能够高效吸附重金属离子,并且羧基化纤维素在重金属的催化作用下与乙醇发生酯化,吸收重金属离子后容易与蜂胶粉分离,因而本发明的蜂胶粉的重金属残留量较低;抗结剂由微晶纤维素和纳米二氧化钛组成,微晶纤维素不仅通过吸湿表现出良好的抗结性能,还能在冷冻保存状态下防止有水分冷冻结块,纳米二氧化钛对蜂胶粉中黄酮类物质起到防氧化作用,提高蜂胶粉中黄酮含量,另外它还具有良好的导电性能,减少蜂胶粉内部静电,从而避免蜂胶粉结块。
Description
技术领域
本发明公开了一种低金属残留防结块蜂胶粉的制备方法,属于蜂胶类产品制备技术领域。
背景技术
蜂胶粉,顾名思义就是粉末状的蜂胶制品,是从原蜂胶经低温提取后的纯蜂胶(98%)再经低温粉碎,添加食用,医用原辅料精致而成的蜂胶类产品。蜂胶呈黄褐色、棕褐色或青绿色,味微苦。其主要成分约含55%树脂和香膏,30%蜂蜡,10%芳香挥发油和5%花粉夹杂物,化学家从蜂胶中分离出黄酮、菇烯、有机酸、芳香醛、醇、脂、多糖类以及氨基酸、维生素、酶、矿物质等300多种成分因而受到医药和卫生界的广泛重视。蜂胶粉是运用现代工艺,把不含蜡的提纯蜂胶流浸膏进行热风干燥,干燥后的蜂胶块经粉碎、过筛,再向蜂胶中加入抗凝结剂超细二氧化硅,由此而来。蜂胶不溶于水,其有效成分多数溶于乙醇。所制备的蜂胶浸膏具有黏性,温度低于15℃时变脆,易粉碎;36℃时软化,65℃时成粘稠液体,因此蜂胶浸膏若采用常规干燥工艺,如热风干燥、真空干燥等不易烘干,耗时耗能,所制成的蜂胶干浸膏若采用常规粉碎机,由于易发热变粘,难以粉碎成粉。
蜂胶粉因不含蜡又含有二氧化硅,分散好,不凝结,易保存、运输使用,是目前食品、医药、日化企业最理想产品之一。食品:目前保健食品行业兴起,蜂胶粉其功效也广为人知,所以30%--90%的蜂胶片,蜂胶胶囊,蜂胶液,蜂胶酊等等一系列的保健食品都在用。医药:蜂胶其药理性大家都很熟悉了,所以在提高免疫力、预防肿瘤、抗氧化、保肝、降血脂、降血糖抗菌消炎、抗病毒、各种皮肤病以及消化、泌尿系统疾病、支气管炎、抗肿瘤、口腔溃疡等方面都得到了很好的作用。日化:蜂胶中黄酮类、黄酮醇、萜烯类、酶类、多种维生素、多酚类、多糖类、树脂、有机酸等有效物质被广泛的应用到了抗菌消炎牙膏、抗菌肥皂以及化妆品等领域。
目前的蜂胶粉的生产工艺多为由粗蜂胶经乙醇提取,去除蜂蜡及铅,回收除尽乙醇,冷冻干燥得到蜂胶干浸膏,低温粉碎成蜂胶粉,再添加适宜辅料而制成。采用此工艺生产常需要添置价格昂贵的冷冻干燥及低温粉碎设备,大大增加了生产成本。所生产的蜂胶粉通常要求贮藏条件需控制在20℃以下,否则蜂胶粉极易结块,也不便制成蜂胶的胶囊剂、片剂等固体制剂,从而限制了蜂胶的应用范围。
市场上存在的大量蜂胶产品,由于生产工艺的不完善,存在良莠不齐的情况,比如,脱杂质不完全,脱铅方法不科学,以及过滤不够精细,未脱除一些可溶性的非活性物质,或无法有效脱除致敏源,或提取工艺不够完善,不适当的参数会影响最终产品的总黄酮含量等,使得最终制得的蜂胶存在质量安全隐患,如:纯度不高、重金属残留量超标、总黄酮含量较低等。使得蜂胶的保健和辅助治疗的效用大打折扣。
因此,发明一种总黄酮含量高、重金属残留低、不易结块的蜂胶粉对蜂胶制品制备技术领域是很有必要的。
发明内容
本发明主要解决的技术问题,针对目前蜂胶粉的生产或提取工艺的不完善,导致蜂胶产品总黄酮含量低,重金属残留超标,并且保存状态中容易结块的缺陷,提供了一种低金属残留防结块蜂胶粉的制备方法。
为了解决上述技术问题,本发明所采用的技术方案是:
一种低金属残留防结块蜂胶粉的制备方法为:
(1)取天然蜂胶用乙醇水溶液分散软化,并加入纤维素吸附剂,制备得到蜂胶悬浮液,将纳米硅胶置于质量分数为25%的聚乙烯亚胺水溶液中,浸泡10~12min,过滤去除滤液,风干后置于抽滤漏斗的滤孔上,加入所制备的蜂胶悬浮液,进行抽滤,并用无水乙醇反复冲洗滤孔,取下方液体再进行抽滤3~4次,得到去金属蜂胶浸液;
(2)将上述去金属蜂胶浸液置于冷冻室中,进行冷冻,得到冷冻蜂胶块;
(3)将上述所得冷冻蜂胶块置于研磨粉碎机,进行粉碎,粉碎成50~100目的蜂胶块,随后送入气流粉碎机中,二次粉碎,并进行循环粉碎,筛选出粒度小于400目的粉粒,得到蜂胶粉体,将蜂胶粉体和抗结剂混合,用干粉搅拌机以300~500r/min的转速搅拌分散40~50min,得到低金属残留防结块蜂胶粉;
所述的纤维素吸附剂具体制备步骤为:
(1)在反应釜中将纳米纤维素分散于去离子水中,再添加溴化钠、四甲基哌啶,搅拌20~30min,再向反应釜中加入质量分数为10%的次氯酸钠溶液,调节pH为9.0~10.0,反应3~5h,制备得到羧基化纤维素;
(2)按重量份数计,将30~35份上述羧基化纤维素、50~60份质量分数为20%的双氧水、70~80份去离子水、10~15份废茶粉混合,搅拌分散得到混合胶液,将所得收集下层沉淀物,用去离子水洗涤沉淀3~5次后,烘干,得到纤维素吸附剂。
所述的低金属残留防结块蜂胶粉具体制备步骤(1)中所用乙醇水溶液为天然蜂胶质量的5倍,纤维素吸附剂占天然蜂胶质量5%。
所述的低金属残留防结块蜂胶粉具体制备步骤(1)中所用乙醇水溶液质量分数优选为50%。
所述的低金属残留防结块蜂胶粉具体制备步骤(2)中进行冷动的过程具体为:先调节冷冻室温度为-8~-12℃,冷冻10~15min,再降温至-15~-20℃,冷冻5~10 min,然后调节冷冻室温度至-25~-20℃,冷冻5~10min。
所述的低金属残留防结块蜂胶粉具体制备步骤(2)中冷冻前冷冻室预先抽湿使湿度控制为10~15%RH。
所述的低金属残留防结块蜂胶粉具体制备步骤(3)中蜂胶粉体和抗结剂混合质量比为30︰1。
所述的低金属残留防结块蜂胶粉具体制备步骤(3)中抗结剂由400目微晶纤维素和400目纳米二氧化钛按质量比为2︰1均匀混合而成。
所述的纤维素吸附剂具体制备步骤(1)中各组分原料,按重量份数计,包括30~35份纳米纤维素、300~350份去离子水、1~2份溴化钠、4~5份四甲基哌啶、 50~60份质量分数为10%的次氯酸钠溶液。
所述的纤维素吸附剂具体制备步骤(1)中调节pH时使用质量分数为20%的氨水达到。
本发明的有益效果是:
(1)本发明用聚乙烯亚胺水溶液作为硅胶的浸渗液,由于聚乙烯亚胺是一种水溶性聚胺,线型大分子链中拥有大量的胺基原子,纳米硅胶经过浸渗后聚乙烯亚胺紧紧吸附在硅胶孔隙内表面,作为螯合材料对金属离子能产生很强的螯合作用,而纤维素吸附剂素包覆在螯合吸附材料的表面,构成纳米滤膜,制备纤维素吸附剂过程中利用四甲基吡啶将纳米纤维素表面羟甲基氧化形成羧基,使其表面粗糙、孔洞丰富,表面含有的羧基基团能够在水中电离出氢离子而呈酸性,离解后的负电基团为碳氢基团,能与溶液中的其他重金属阳离子吸附结合,迅速进入螯合材料中被吸附浓集,能够高效吸附重金属离子,并且羧基化纤维素在重金属的催化作用下与乙醇发生酯化,吸收重金属离子后容易与蜂胶粉分离,因而本发明的蜂胶粉的重金属残留量较低;
(2)本发明将天然蜂胶去金属处理后经冷冻、粉碎筛选,再添加抗结剂混合,得到低金属残留防结块蜂胶粉,其中抗结剂由微晶纤维素和纳米二氧化钛组成,蜂胶浸液采用气流磨粉碎过筛,可循环作业,且粉碎效果好,与粒度一致的抗结剂均匀混合形成高度分散、流动性良好的粉体,微晶纤维素不仅通过吸湿表现出良好的抗结性能,还能在冷冻保存状态下防止有水分冷冻结块,这是因为微晶纤维素能够抑制冰晶长大,因而有利于蜂胶粉的存取使用,无需等待温度变化方能使用蜂胶粉,扩大的蜂胶粉的使用温度范围,而纳米二氧化钛对蜂胶粉中黄酮类物质起到防氧化作用,提高蜂胶粉中黄酮含量,另外它还具有良好的导电性能,减少蜂胶粉内部静电,从而避免蜂胶粉结块,具有广阔的应用前景。
具体实施方式
按重量份数计,在反应釜中将30~35份纳米纤维素分散于300~350份去离子水中,再添加1~2份溴化钠、4~5份四甲基哌啶,搅拌20~30min,再向反应釜中加入50~60份质量分数为10%的次氯酸钠溶液,用质量分数为20%的氨水调节pH为9.0~10.0,反应3~5h,制备得到羧基化纤维素;按重量份数计,将30~35份上述羧基化纤维素、50~60份质量分数为20%的双氧水、70~80份去离子水、10~15份废茶粉混合,搅拌分散得到混合胶液,将所得收集下层沉淀物,用去离子水洗涤沉淀3~5次后,烘干,得到纤维素吸附剂;取天然蜂胶用其5倍质量的质量分数为50%的乙醇水溶液分散软化,并加入占天然蜂胶质量5%的上述纤维素吸附剂,制备得到蜂胶悬浮液,将纳米硅胶置于质量分数为25%的聚乙烯亚胺水溶液中,浸泡10~12min,过滤去除滤液,风干后置于抽滤漏斗的滤孔上,加入所制备的蜂胶悬浮液,进行抽滤,并用无水乙醇反复冲洗滤孔,取下方液体再进行抽滤3~4次,得到去金属蜂胶浸液;将上述去金属蜂胶浸液置于冷冻室中,进行冷冻,先调节冷冻室温度为-8~-12℃,冷冻10~15min,再降温至-15~-20℃,冷冻5~10 min,然后调节冷冻室温度至-25~-20℃,冷冻5~10min,得到冷冻蜂胶块,冷冻前冷冻室预先抽湿使湿度控制为10%RH~15%RH;将上述所得冷冻蜂胶块置于研磨粉碎机,进行粉碎,粉碎成50~100目的蜂胶块,随后送入气流粉碎机中,二次粉碎,并进行循环粉碎,筛选出粒度小于400目的粉粒,得到蜂胶粉体,将蜂胶粉体和抗结剂按质量比为30︰1混合,用干粉搅拌机以300~500r/min的转速搅拌分散40~50min,得到低金属残留防结块蜂胶粉,所述的抗结剂由400目微晶纤维素和400目纳米二氧化钛按质量比为2︰1均匀混合而成。
实施例1
纤维素吸附剂的制备:
按重量份数计,在反应釜中将30份纳米纤维素分散于300份去离子水中,再添加1份溴化钠、4份四甲基哌啶,搅拌20min,再向反应釜中加入50份质量分数为10%的次氯酸钠溶液,用质量分数为20%的氨水调节pH为9.0,反应3h,制备得到羧基化纤维素;
按重量份数计,将30份上述羧基化纤维素、50份质量分数为20%的双氧水、70份去离子水、10份废茶粉混合,搅拌分散得到混合胶液,将所得收集下层沉淀物,用去离子水洗涤沉淀3次后,烘干,得到纤维素吸附剂;
冷冻蜂胶块的制备:
取天然蜂胶用其5倍质量的质量分数为50%的乙醇水溶液分散软化,并加入占天然蜂胶质量5%的上述纤维素吸附剂,制备得到蜂胶悬浮液,将纳米硅胶置于质量分数为25%的聚乙烯亚胺水溶液中,浸泡10min,过滤去除滤液,风干后置于抽滤漏斗的滤孔上,加入所制备的蜂胶悬浮液,进行抽滤,并用无水乙醇反复冲洗滤孔,取下方液体再进行抽滤3次,得到去金属蜂胶浸液;
将上述去金属蜂胶浸液置于冷冻室中,进行冷冻,先调节冷冻室温度为-8℃,冷冻10min,再降温至-15℃,冷冻5min,然后调节冷冻室温度至-25℃,冷冻5min,得到冷冻蜂胶块,冷冻前冷冻室预先抽湿使湿度控制为10%RH;
低金属残留防结块蜂胶粉的制备:
将上述所得冷冻蜂胶块置于研磨粉碎机,进行粉碎,粉碎成50目的蜂胶块,随后送入气流粉碎机中,二次粉碎,并进行循环粉碎,筛选出粒度小于400目的粉粒,得到蜂胶粉体,将蜂胶粉体和抗结剂按质量比为30︰1混合,用干粉搅拌机以300r/min的转速搅拌分散40min,得到低金属残留防结块蜂胶粉,所述的抗结剂由400目微晶纤维素和400目纳米二氧化钛按质量比为2︰1均匀混合而成。
实施例2
纤维素吸附剂的制备:
按重量份数计,在反应釜中将32份纳米纤维素分散于320份去离子水中,再添加1份溴化钠、4份四甲基哌啶,搅拌25min,再向反应釜中加入55份质量分数为10%的次氯酸钠溶液,用质量分数为20%的氨水调节pH为9.5,反应4h,制备得到羧基化纤维素;
按重量份数计,将32份上述羧基化纤维素、55份质量分数为20%的双氧水、75份去离子水、12份废茶粉混合,搅拌分散得到混合胶液,将所得收集下层沉淀物,用去离子水洗涤沉淀4次后,烘干,得到纤维素吸附剂;
冷冻蜂胶块的制备:
取天然蜂胶用其5倍质量的质量分数为50%的乙醇水溶液分散软化,并加入占天然蜂胶质量5%的上述纤维素吸附剂,制备得到蜂胶悬浮液,将纳米硅胶置于质量分数为25%的聚乙烯亚胺水溶液中,浸泡11min,过滤去除滤液,风干后置于抽滤漏斗的滤孔上,加入所制备的蜂胶悬浮液,进行抽滤,并用无水乙醇反复冲洗滤孔,取下方液体再进行抽滤3次,得到去金属蜂胶浸液;
将上述去金属蜂胶浸液置于冷冻室中,进行冷冻,先调节冷冻室温度为-10℃,冷冻12min,再降温至-17℃,冷冻7 min,然后调节冷冻室温度至-22℃,冷冻7min,得到冷冻蜂胶块,冷冻前冷冻室预先抽湿使湿度控制为12%RH;
低金属残留防结块蜂胶粉的制备:
将上述所得冷冻蜂胶块置于研磨粉碎机,进行粉碎,粉碎成75目的蜂胶块,随后送入气流粉碎机中,二次粉碎,并进行循环粉碎,筛选出粒度小于400目的粉粒,得到蜂胶粉体,将蜂胶粉体和抗结剂按质量比为30︰1混合,用干粉搅拌机以400r/min的转速搅拌分散45min,得到低金属残留防结块蜂胶粉,所述的抗结剂由400目微晶纤维素和400目纳米二氧化钛按质量比为2︰1均匀混合而成。
实施例3
纤维素吸附剂的制备:
按重量份数计,在反应釜中将35份纳米纤维素分散于350份去离子水中,再添加2份溴化钠、5份四甲基哌啶,搅拌30min,再向反应釜中加入60份质量分数为10%的次氯酸钠溶液,用质量分数为20%的氨水调节pH为10.0,反应5h,制备得到羧基化纤维素;
按重量份数计,将35份上述羧基化纤维素、60份质量分数为20%的双氧水、80份去离子水、15份废茶粉混合,搅拌分散得到混合胶液,将所得收集下层沉淀物,用去离子水洗涤沉淀5次后,烘干,得到纤维素吸附剂;
冷冻蜂胶块的制备:
取天然蜂胶用其5倍质量的质量分数为50%的乙醇水溶液分散软化,并加入占天然蜂胶质量5%的上述纤维素吸附剂,制备得到蜂胶悬浮液,将纳米硅胶置于质量分数为25%的聚乙烯亚胺水溶液中,浸泡12min,过滤去除滤液,风干后置于抽滤漏斗的滤孔上,加入所制备的蜂胶悬浮液,进行抽滤,并用无水乙醇反复冲洗滤孔,取下方液体再进行抽滤4次,得到去金属蜂胶浸液;
将上述去金属蜂胶浸液置于冷冻室中,进行冷冻,先调节冷冻室温度为-12℃,冷冻15min,再降温至-20℃,冷冻10 min,然后调节冷冻室温度至-20℃,冷冻10min,得到冷冻蜂胶块,冷冻前冷冻室预先抽湿使湿度控制为15%RH;
低金属残留防结块蜂胶粉的制备:
将上述所得冷冻蜂胶块置于研磨粉碎机,进行粉碎,粉碎成100目的蜂胶块,随后送入气流粉碎机中,二次粉碎,并进行循环粉碎,筛选出粒度小于400目的粉粒,得到蜂胶粉体,将蜂胶粉体和抗结剂按质量比为30︰1混合,用干粉搅拌机以500r/min的转速搅拌分散50min,得到低金属残留防结块蜂胶粉,所述的抗结剂由400目微晶纤维素和400目纳米二氧化钛按质量比为2︰1均匀混合而成。
对比例1:与实施例2的制备方法基本相同,唯有不同的是缺少纤维素吸附剂。
对比例2:与实施例2的制备方法基本相同,唯有不同的是抗结剂中不含微晶纤维素与二氧化钛。
对比例3:深圳某公司生产的低金属残留防结块蜂胶粉。
重金属含量测试:采用《世界最新医学信息文摘》蜂胶制品中重金属元素的含量测定,采用微波消解、ICP-MS法测定蜂胶制品中的3种重金属元素(砷、铅、汞)。
抗结块性测试:将实施例和对比例中的蜂胶粉放置60℃烘箱中,进行加速试验,观察蜂胶粉的性状变化情况。
总黄酮含量测试:在室温下乙醇冷浸法对蜂胶总黄酮进行提取,得到蜂胶浸膏,测得总黄酮含量。
表1:蜂胶粉性能测定结果
检测项目 | 实例1 | 实例2 | 实例3 | 对比例1 | 对比例2 | 对比例3 |
铅含量(ppm) | 0.008 | 0.006 | 0.005 | 0.020 | 0.018 | 0.019 |
砷含量(ppm) | 0.006 | 0.004 | 0.003 | 0.015 | 0.012 | 0.013 |
汞含量(ppm) | 0.007 | 0.006 | 0.004 | 0.019 | 0.017 | 0.015 |
抗结块性 | 放置3个月未变软结块,粉末流动性好 | 放置3个月未变软结块,粉末流动性好 | 放置3个月未变软结块,粉末流动性好 | 放置10h变软结块 | 放置6h变软结块 | 放置24h变软结块 |
总黄酮含量(%) | 31.22 | 31.48 | 31.65 | 19.12 | 15.32 | 18.45 |
综合上述,从表1可以看出本发明的蜂胶粉重金属含量低,铅、砷、汞含量低, 抗结块性好,放置3个月未变软结块,粉末流动性好,总黄酮含量高,具有广阔应用前景。
以上所述仅为本发明的较佳方式,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (9)
1.一种低金属残留防结块蜂胶粉的制备方法,其特征在于具体制备步骤为:
(1)取天然蜂胶用乙醇水溶液分散软化,并加入纤维素吸附剂,制备得到蜂胶悬浮液,将纳米硅胶置于质量分数为25%的聚乙烯亚胺水溶液中,浸泡10~12min,过滤去除滤液,风干后置于抽滤漏斗的滤孔上,加入所制备的蜂胶悬浮液,进行抽滤,并用无水乙醇反复冲洗滤孔,取下方液体再进行抽滤3~4次,得到去金属蜂胶浸液;
(2)将上述去金属蜂胶浸液置于冷冻室中,进行冷冻,得到冷冻蜂胶块;
(3)将上述所得冷冻蜂胶块置于研磨粉碎机,进行粉碎,粉碎成50~100目的蜂胶块,随后送入气流粉碎机中,二次粉碎,并进行循环粉碎,筛选出粒度小于400目的粉粒,得到蜂胶粉体,将蜂胶粉体和抗结剂混合,用干粉搅拌机以300~500r/min的转速搅拌分散40~50min,得到低金属残留防结块蜂胶粉;
所述的纤维素吸附剂具体制备步骤为:
(1)在反应釜中将纳米纤维素分散于去离子水中,再添加溴化钠、四甲基哌啶,搅拌20~30min,再向反应釜中加入质量分数为10%的次氯酸钠溶液,调节pH为9.0~10.0,反应3~5h,制备得到羧基化纤维素;
(2)按重量份数计,将30~35份上述羧基化纤维素、50~60份质量分数为20%的双氧水、70~80份去离子水、10~15份废茶粉混合,搅拌分散得到混合胶液,将所得收集下层沉淀物,用去离子水洗涤沉淀3~5次后,烘干,得到纤维素吸附剂。
2.根据权利要求1所述的一种低金属残留防结块蜂胶粉的制备方法,其特征在于:
所述的低金属残留防结块蜂胶粉具体制备步骤(1)中所用乙醇水溶液为天然蜂胶质量的5倍,纤维素吸附剂占天然蜂胶质量5%。
3.根据权利要求1所述的一种低金属残留防结块蜂胶粉的制备方法,其特征在于:所述的低金属残留防结块蜂胶粉具体制备步骤(1)中所用乙醇水溶液质量分数优选为50%。
4.根据权利要求1所述的一种低金属残留防结块蜂胶粉的制备方法,其特征在于:所述的低金属残留防结块蜂胶粉具体制备步骤(2)中进行冷动的过程具体为:先调节冷冻室温度为-8~-12℃,冷冻10~15min,再降温至-15~-20℃,冷冻5~10 min,然后调节冷冻室温度至-25~-20℃,冷冻5~10min。
5.根据权利要求1所述的一种低金属残留防结块蜂胶粉的制备方法,其特征在于:所述的低金属残留防结块蜂胶粉具体制备步骤(2)中冷冻前冷冻室预先抽湿使湿度控制为10~15%RH。
6.根据权利要求1所述的一种低金属残留防结块蜂胶粉的制备方法,其特征在于:
所述的低金属残留防结块蜂胶粉具体制备步骤(3)中蜂胶粉体和抗结剂混合质量比为30︰1。
7.根据权利要求1所述的一种低金属残留防结块蜂胶粉的制备方法,其特征在于:所述的低金属残留防结块蜂胶粉具体制备步骤(3)中抗结剂由400目微晶纤维素和400目纳米二氧化钛按质量比为2︰1均匀混合而成。
8.根据权利要求1所述的一种低金属残留防结块蜂胶粉的制备方法,其特征在于:所述的纤维素吸附剂具体制备步骤(1)中各组分原料,按重量份数计,包括30~35份纳米纤维素、300~350份去离子水、1~2份溴化钠、4~5份四甲基哌啶、 50~60份质量分数为10%的次氯酸钠溶液。
9.根据权利要求1所述的一种低金属残留防结块蜂胶粉的制备方法,其特征在于:所述的纤维素吸附剂具体制备步骤(1)中调节pH时使用质量分数为20%的氨水达到。
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