CN114377044A - 一种芹菜籽提取物的制备方法 - Google Patents
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Abstract
本发明属于食品加工领域,提供了一种芹菜籽提取物的制备方法:(1)将芹菜籽用乙醇溶液超声波辅助提取,获得乙醇提取物;(2)将乙醇提取物,加入分子蒸馏设备,设置刮板转速30‑50 rpm,刮板温度60℃‑85℃,真空度0.5‑2mto,进料量0.5‑1 mL/min,收集轻组分瓶内的液体,即为芹菜籽提取物。本发明的芹菜籽提取物具有较好的抑制尿酸生成和清除自由基的效果,相比目前市场芹菜籽粗加工产品,其活性成分含量高,更有益于人体健康。本发明的原料资源极为丰富且成本低,生产设备要求低,加工工艺简便。
Description
技术领域
本发明属于食品加工领域,涉及一种芹菜籽提取物的制备方法及其产品。
背景技术
芹菜籽为芹菜的种子,最早的药用记载于《神农本草经》,芹菜籽不仅含有丰富的营养元素,还含有多种化学成分。芹菜籽自《新修本草》后被人们所熟知,越来越多的应用到临床中。近年来,对芹菜的研究大多集中在茎、叶等方面,针对芹菜籽的化学成分及药理作用的系统性研究较少,芹菜籽具有较好的降血脂、降尿酸作用。
目前市面上的芹菜籽产品大多是芹菜籽直接打粉进行使用,产品利用度不是很大;目前市面上的芹菜籽提取物大多是水溶性提取物,通过水提法提取芹菜籽中的有效成分,浓缩后烘干制成,产品功效性成分损失较大,产率较低。
发明内容
针对目前芹菜籽精深加工产品较少的问题,本发明提供一种芹菜籽提取物的制备方法,原料资源极为丰富且成本低,生产设备要求低,加工工艺简便。
本发明的另一目的是提供一种上述制备方法获得的产品,活性成分含量高,具有较好的抑制尿酸生成效果。
为实现上述目的,本发明采用如下技术方案。
一种芹菜籽提取物的制备方法,包括以下步骤:
(1)将芹菜籽用乙醇溶液超声波辅助提取,获得乙醇提取物;
(2)将乙醇提取物,加入分子蒸馏设备,设置刮板转速30-50 rpm,刮板温度60℃-85℃,真空度0.5-2mto,进料量0.5-1 mL/min,收集轻组分瓶内的液体,即为芹菜籽提取物。
优选地,步骤(1)中,芹菜籽与乙醇溶液的质量体积比为1:25-40。
优选地,步骤(1)中,所述提取条件为:超声频率40 kHz,超声温度35-60℃,超声时间15-90min。
优选地,步骤(1)中,所述乙醇溶液的浓度20%-50%v/v。
优选地,步骤(2)后还包括冷冻干燥获得芹菜籽提取物粉的步骤。
一种上述方法获得的芹菜籽提取物。所述提取物具有降低尿酸、清除自由基、抗氧化的作用。
一种上述芹菜籽提取物可用作食品或药品的原料或辅料。
本发明具有以下优点:
本发明的芹菜籽提取物制备方法,以芹菜籽作为主要原料,获得了高纯度芹菜籽提取物,获得的产品呈深棕色。本发明的芹菜籽提取物具有较好的抑制尿酸生成和清除自由基的效果,相比目前市场芹菜籽粗加工产品,其活性成分含量高,更有益于人体健康。本发明的原料资源极为丰富且成本低,生产设备要求低,加工工艺简便。开发的新型芹菜籽食品可作为新资源食品,目前该类型产品尚属市场空白,市场前景广阔,可为企业及地方带来良好的经济效益。
附图说明
图1是乙醇浓度、提取时间和提取温度对提取量的影响;
图2是不同分子蒸馏条件对提取量的影响;
图3是芹菜籽提取物;
图4是尿酸浓度-峰面积标准曲线;
图5是不同样品尿酸生成抑制率。
具体实施方式
下面结合实施例和附图对本发明做进一步说明,但本发明不受下述实施例的限制。
实施例1 芹菜籽提取物的制备和条件优化
1. 超声提取条件筛选
(1)称取1 kg净洗干燥的芹菜籽,加入25-40L的20-50%乙醇溶液,25-55℃下40kHz超声波辅助提取15-90 min,获得乙醇提取物;
(2)将乙醇提取物,加入分子蒸馏设备,设置刮板转速35 rpm,刮板温度85℃,真空度2mto,进料量1.0 mL/min,收集轻组分瓶内的液体,获得提取液;
(3)将提取液-50℃冷冻干燥48h,获得芹菜籽提取物粉。
根据原料芹菜籽和提取物的质量计算提取量(g/100g)对提取条件进行单变量筛选,结果如图1所示。由结果可知,随着乙醇浓度从20%变化为50%,提取量先增加后降低,提取量的峰值在35%浓度处。随着提取时间从15min延长至60min,提取量增加明显,而超过60min后提取量呈现下降趋势。随着提取温度从25℃提高到45℃,提取量逐渐升高,高于45℃后呈现略下降的趋势。因此,选择35%乙醇溶液为提取液,在45℃下超声提取60min进行下一步筛选。
2. 分子蒸馏条件筛选
(1)称取2kg净洗干燥的芹菜籽,加入70L的35%乙醇溶液,45℃下40kHz超声波辅助提取60min,获得乙醇提取物;
(2)将乙醇提取物,加入分子蒸馏设备,设置刮板转速30-50 rpm,刮板温度60℃-85℃,真空度0.5-2mto,进料量0.5-1.5 mL/min,收集轻组分瓶内的液体,获得提取液;
(3)将提取液-50℃冷冻干燥48h,获得芹菜籽提取物粉。
根据原料芹菜籽和提取物的质量计算提取量(g/100g)对提取条件进行单变量筛选,结果如图2所示:随着刮板转速由30rpm升至50rpm,提取率升高,35rpm后变化较小;随着刮板温度由60℃提高至85℃,提取量逐渐升高,80℃后略有下降;随着真空度的提高,提取量一直呈增加的趋势;随着进料料量由0.5-1.0 mL/min提高,提取量降低并不显著,进料量超过1.0 mL/min后出现较快下降。
实施例2 芹菜籽提取物的对尿酸生成的抑制作用
1. 提取物制备
(1)称取1 kg净洗干燥的芹菜籽,加入35L的35%乙醇溶液,45℃下40 kHz超声波辅助提取1h,获得乙醇提取物;
(2)将乙醇提取物,加入分子蒸馏设备,设置刮板转速35 rpm,刮板温度80℃,真空度2 mto,进料量1.0 mL/min,收集轻组分瓶内的液体,获得芹菜籽提取液(图3A);
(3)将芹菜籽浓缩物-50℃冷冻干燥48h,获得如图3B所示的芹菜籽提取物粉,记为样品1。
按照CN110585252A实施例2的方法获得富含黄酮的芹菜籽提取物,记为样品2。
按照CN112716989A实施例1的方法获得含芹菜苷的芹菜籽提取物,记为样品3。
2. 不同提取物的尿酸生成抑制率
称取不同提取物以70%乙醇溶液制备成200 mg/L的待测样品液(含1%v/v DMSO)。2mL容量瓶中加入20 μL不同的待测样品液再加入400 μL PBS缓冲溶液(pH 7.4),旋涡振荡混匀,37℃孵化30 min,然后加入40 μL浓度为400 mmol/L的黄嘌呤氧化酶储备液,旋涡振荡混匀,37℃反应30 min后,加入1 mol/L的盐酸500 μL终止反应,反应液用纯水定容到刻度,获得检测液,每个待测样品平行操作3次,反应同时设置阳性对照组(500 mmol/L别嘌呤醇)、阴性对照组(缓冲液)。所有检测液进行HPLC分析尿酸含量,以峰面积-不同尿酸浓度制作标准曲线(图4)、拟合回归曲线y=1065.46+8852.73x(R2=0.9966),计算不同样品的尿酸生成抑制率。
HPLC色谱条件如下:
流动相:0.02 mol/L PBS缓冲溶液(pH 7.4,含甲醇1%v/v)
流速:1.0 mL/min
进样量:20 μL
柱温:室温
检测器:二极管阵列检测器
检测波长:254 nm。
结果如图5所示,结果显示,本发明的提取物对尿酸生成的抑制与阳性对照无差异(p>0.05);显著优于现有技术中以总黄酮和芹菜素为主要成分的芹菜籽提取物。
实施例3 芹菜籽提取物的对自由基的清除作用
1. 提取物制备
(1)称取1 kg净洗干燥的芹菜籽,加入35L的35%乙醇溶液,45℃下40 kHz超声波辅助提取1h,获得乙醇提取物;
(2)将乙醇提取物,加入分子蒸馏设备,设置刮板转速35 rpm,刮板温度80℃,真空度2 mto,进料量1.0 mL/min,收集轻组分瓶内的液体,获得芹菜籽提取液;
(3)将芹菜籽浓缩物-50℃冷冻干燥48h,获得芹菜籽提取物。
参照刘长江等的方法(刘长江,刘辉,李斌,李钇潼. 不同方法提取芹菜籽精油的比较研究[J]. 食品科技,2009,v.34;No.210(04): 182-185)采用水蒸气蒸馏法提取芹菜籽精油:将1000 g 过筛后样品加入3000 mL蒸馏水(含80 g/L NaCl),加热沸腾产生过热水蒸气在常压下蒸馏至蒸馏液无油珠,同时在溶剂瓶中加入1000 mL乙醚(50℃水浴加热)同步循环萃取蒸馏出芹菜籽油。收集油水混合液,加入无水硫酸钠干燥除去水分,过滤,滤液旋转蒸发除去溶剂,得淡黄绿色芹菜籽精油。
2. 芹菜籽精油和芹菜籽提取物抗氧化能力和自由基清除能力
参照段光东等的方法(段光东,姜子涛,李荣,李清鹏,孙建平.芹菜籽精油抗氧化能力的研究[J]. 中国调味品,2009,v.34;No.v.34(09): 50-53+56),测定1中获得的芹菜籽精油和芹菜籽提取物的DPPH自由基和羟基自由基的清除率;
参照杨坤等的方法(杨坤,赵谋明,孙为正,赵强忠,林恋竹. 7种海参提取物酶法制备及其抗氧化活性研究[J]. 中国食品学报,2019,19(09): 127-136),测定1中获得的芹菜籽精油和芹菜籽提取物的氧自由基清除能力,将Trolox作为标准品,换算得到样品的氧自由基清除能力,即达到每千克芹菜籽的氧自由基清除能力所需Torlox的量(mmol)。
表1 芹菜籽精油和芹菜籽提取物抗氧化能力对比
从表1中可知,相比于芹菜籽精油,本发明获得的芹菜籽提取物对DPPH自由基和羟基自由基的清除率均远高于芹菜籽精油。
Claims (8)
1.一种芹菜籽提取物的制备方法,其特征在于,包括以下步骤:
(1)将芹菜籽用乙醇溶液超声波辅助提取,获得乙醇提取物;
(2)将乙醇提取物,加入分子蒸馏设备,设置刮板转速30-50 rpm,刮板温度60℃-85℃,真空度0.5-2mto,进料量0.5-1 mL/min,收集轻组分瓶内的液体,即为芹菜籽提取物。
2.根据权利要求1所述的制备方法,其特征在于,步骤(1)中,芹菜籽与乙醇溶液的质量体积比为1:25-40。
3. 根据权利要求1所述的制备方法,其特征在于,步骤(1)中,所述提取条件为:超声频率40 kHz,超声温度35-60℃,超声时间15-90min。
4.根据权利要求1所述的制备方法,其特征在于,步骤(1)中,所述乙醇溶液的浓度20%-50%v/v。
5.根据权利要求1所述的制备方法,其特征在于,步骤(2)后还包括冷冻干燥获得芹菜籽提取物粉的步骤。
6.一种如权利要求1-5任一所述的制备方法获得的芹菜籽提取物。
7.一种含有如权利要求6所述的芹菜籽提取物的食品或药品。
8.根据权利要求7所述的食品或药品,其特征在于,所述芹菜籽提取物作为降低尿酸、清除自由基和抗氧化的原料或辅料使用。
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