CN113856639A - 一种低次烟叶固相萃取吸附剂的制备方法及其应用 - Google Patents
一种低次烟叶固相萃取吸附剂的制备方法及其应用 Download PDFInfo
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Abstract
本发明公开了一种低次烟叶固相萃取吸附剂的制备方法及其应用,包括以下步骤:S1.剪切低次烟叶,得到碎烟叶;S2.将所述碎烟叶加入至强碱溶液中,水浴加热回流后过滤,得到碎烟叶滤渣;S3.利用多层中速滤纸包覆所述碎烟叶滤渣,并用沸水清洗,得到低次烟叶固相萃取吸附剂粗产物;S4.将所述低次烟叶固相萃取吸附剂粗产物真空干燥,即得所述低次烟叶固相萃取吸附剂,所制备的吸附剂环境友好、成本低廉,对待测物的吸附效率高。
Description
技术领域
本发明涉及萃取分析领域,具体涉及一种低次烟叶固相萃取吸附剂的制备方法及其应用。
技术背景
随着生命科学、环境科学、食品安全及制药、合成化学等的快速发展,与其相匹配的高效、快速的样品前处理技术日益引起人们的广泛关注,其中固相萃取(SPE)是一种应用非常广泛的样品前处理方法,可以通过离线、在线等方式与色谱等技术联用,实现对复杂样品中分析物的分离分析。目前,烷基键合相(如C2、C8、C18)是固相萃取中应用最常见的萃取材料,这些固相萃取填料能对具有疏水性的化合物表现出吸附性能,然而在许多具体的实际应用中,分析对象种类多样,常用的烷基键合相固相萃取材料已不能满足要求。因此,开发新型固相萃取填料及其应用研究成为目前关注的焦点。
烟草中含有很多危害生命健康的化学物质,并且这些物质是许多疾病的致病因素,例如:肺部疾病、心血管疾病,哮喘、糖尿病及癌症等。因此,烟草中一些成分如烟碱等的存在对人们身体健康还是特别重要的。据分析,烟碱是烟草中含量且毒性较大的化合物,其又称为尼古丁。并且烟碱中特有的亚硝胺类化合物,是影响身体健康的一大类化合物。
公开号为CN201810579758.3的中国专利公开了一种固相微萃取-质谱联用在线富集检测烟草中烟碱类化合物的方法,先制备一种可用于烟草中烟碱成分富集的管内聚合物整体柱(In-tube SPME),进而建立一种In-tube SPME与API-MS在线检测实际样品烟草中有害身体健康的烟碱化合物含量的方法。该方法利用整体柱表面的氢键,π-π键及疏水性等与烟碱化合物之间非共价键相互作用,实现烟碱类有害物质的富集,低样品消耗、灵敏度高,但其纯化富集速度慢;
酚类物质在烟草以及烟气中广泛存在,并且和烟叶色泽,品质以及烟气生理强度等方面密切相关,是烟草工业中一类重要的化合物。卷烟中的多酚化合物因为沸点较高,在燃烧时不会直接进入烟气中,大部分都会分解成为简单酚类化合物进气烟气中。然而,有关烟气中的简单酚类化合物的报道大部分是负面的,例如:对呼吸道粘膜有强烈的刺激作用;引起辣味,涩味等,影响卷烟的口感;甚至还有辅助促癌作用。因此,卷烟烟气中的酚类化合物是有害成分,烟气中酚类物质的分析检测也成为国内外烟草行业研究的热点方向之一;
公开号为CN201611225093.3的中国专利公开了一种滇橄榄多酚的富集纯化方法,采用LiChrolut EN树脂的选择性吸附,对滇橄榄多酚进行选择吸附,但其吸附效果稳定性差,且吸附效率低。
现有技术中所运用的填料存在吸附效率低,且原料昂贵,使用后回收污染性大的问题。
发明内容
为解决上述问题,本发明提供一种低次烟叶固相萃取吸附剂的制备方法及其应用,所制备的吸附剂环境友好、成本低廉,对待测物的吸附效率高。
本发明的技术方案是,提供一种低次烟叶固相萃取吸附剂的制备方法,包括以下步骤:
S1.剪切低次烟叶,得到碎烟叶,本步骤所使用的低次烟叶为经打叶复烤、仓储的烟叶,将所述低次烟叶剪切为小段,增大表面积,提高后续步骤的效率;
S2.将所述碎烟叶加入至强碱溶液中,水浴加热回流后过滤,得到碎烟叶滤渣,用热碱的目的在于去除烟叶表面的色素、蛋白等大分子杂质;
S3.利用多层中速滤纸包覆所述碎烟叶滤渣,并用沸水清洗,得到低次烟叶固相萃取吸附剂粗产物,沸水清洗的步骤为将所述由多层中速滤纸包裹的碎烟叶滤渣置于含有蒸馏水的烧瓶中,安装冷凝回流装置,加热烧瓶,使水沸腾,冷凝回流5-6h,充分将所述碎烟叶滤渣中残留的碱溶液去除,并通过中速滤纸过滤,得到除杂后的低次烟叶固相萃取吸附剂粗产物;
S4.将所述低次烟叶固相萃取吸附剂粗产物真空干燥,即得所述低次烟叶固相萃取吸附剂,真空干燥后便于保藏,且便于增大分析物的吸附量。
优选地,所述碎烟叶的长度为0.5-1.2cm,符合常用萃取柱的直径尺寸,便于将成品填充于萃取柱中。
优选地,所述强碱为NaOH、KOH中的一种或几种,NaOH、KOH去除烟叶表面的色素、蛋白等大分子杂质。
优选地,所述步骤S2中,强碱溶液的浓度为0.5-2 mol/L,浓度太低去除效果差,浓度太高对原料有损伤。
优选地,所述强碱溶液与所述碎烟叶的质量比为(5-10):1。
优选地,所述步骤S2中,所述加热温度为50-60℃,所述加热时间为3-5h。
优选地,所述步骤S3中,所述沸水与所述碎烟叶滤渣的质量比为(10-20):1,充分去除残留的强碱。
优选地,所述步骤S3中,所述中速滤纸的层数为3-4层,充分保留碎烟叶滤渣,避免溢出。
优选地,所述步骤S4中,真空干燥的温度为50-60℃。
进一步地,还提供一种低次烟叶固相萃取吸附剂的应用,将所述低次烟叶固相萃取吸附剂作为萃取柱填料用于富集纯化酚类或烟碱类物质,应用的具体步骤为,将所述低次烟叶固相萃取吸附剂作为填料装入带有筛板的SPE空柱管中,轻轻用手指敲打使填料填充均匀,上端盖上筛板压紧,成为烟叶吸附萃取柱,使液体样品溶液通过烟叶吸附萃取柱,保留其中被测物质,如酚类或烟碱类物质,再选用适当强度溶剂冲去杂质,然后用少量溶剂迅速洗脱被测物质,最后通过液相色谱对目标物进行浓度检测。
低次烟叶指的是GB2635-86中的中黄五级、上黄四级、青黄二级以下的各等级烟叶。这部分烟叶从其外观质量来讲,颜色棕黄、黄褐且带有青色、厚薄不均匀、叶片结构疏松、光泽度较弱、多带有明显的花片、残伤面积大及油分不足等;从内在吸食品质来讲,香味欠缺、香气质较粗糙、苦辣、刺激性涩味明显、余味不净、口腔舌部残留物较多。在烟草种植和生产过程中,有大量的低次烟叶产生,大约占烟叶总产量的 25%。目前,烟草行业内低次烟叶主要用于膨胀烟丝或薄片,且只在四类卷烟和五类卷烟中使用,比例大多低于10%。因此,低次烟叶面临着综合利用水平低、途径少、资源浪费非常严重等一系列问题。
本方案中,为提高低次烟叶的利用价值,采用简单的材料剪切和清洗步骤,然后用强碱溶液加热处理,去除烟叶表面的色素、蛋白等大分子杂质,再通过索氏提取装置采用蒸馏水加热回流,清洗烟叶表面残留强碱溶液,经真空干燥,制得所述低次烟叶固相萃取吸附剂,并将所述低次烟叶固相萃取吸附剂作为萃取柱填料用于富集纯化烟草中酚类或烟碱类物质。
低次烟叶作为固相萃取的吸附介质,作为复杂基质样品中多种类型有机化合物的SPE萃取吸附剂,能纯化富集其中的生物活性物质,如烟叶中绿原酸、芸香苷及麦芽酚等酚类化合物及尼古丁等烟碱类物质,可萃取上述物质的原因在于,烟叶是一种天然的生物质,孔隙结构相当丰富,是一种具有毛细管多孔性特殊结构的物质,烟叶经打叶复烤、切丝等工艺可制成仍具有毛细管多孔结构、尺寸均匀、蓬松且具有丰富极性羟基和疏水性芳香基等功能基团的烟丝,可以与分析物发生疏水作用、π-π作用、亲水作用和氢键作用等,吸附能力强,稳定性高;另一方面,将低次烟叶直接用作萃取柱的填料用于萃取分析,经处理使烟叶表面纤维暴露,接触面增大,改善了对于待分析物的吸附和萃取能力,对于待分析对象的渗透性好,过柱速度快,仅需30-60s/ml,不需要真空抽溶液,仅靠重力作用,待分析溶液就能自动流下来通过烟叶吸附萃取柱,而同样的样液通过市售的SPE柱在自重作用下需70-90s/ml,本方案操作便捷,减少试验设备和工序,环境友好、方法简单、经济实惠,选用的低次烟叶材料天然、成本低廉、性能稳定。
本发明的有益效果在于:
1.本方案以低次烟叶作为原料制备萃取柱的填料,孔隙结构相当丰富,是一种具有毛细管多孔性特殊结构的物质,烟叶经打叶复烤、切丝等工艺可制成仍具有毛细管多孔结构、尺寸均匀、蓬松,经处理使烟叶表面纤维暴露,接触面增大,改善了对于待分析物的吸附和萃取能力,对于待分析对象的渗透性好,不需要真空抽溶液,仅靠重力作用,待分析溶液就能自动流下来通过烟叶吸附萃取柱,速度快,效率高;
2.本方案所制备的低次烟叶固相萃取吸附剂具有极性羟基和疏水性芳香基,可以与烟叶中绿原酸、芸香苷及麦芽酚等酚类化合物及尼古丁等烟碱类物质发生疏水作用、π-π作用、亲水作用和氢键作用等,吸附能力强,稳定性高;
3.本发明环境友好、方法简单、经济实惠,选用的低次烟叶材料天然、成本低廉,提高了低次烟叶的利用价值。
附图说明
图1为实施例6-9中的检测结果;
图2为对比例1-4中的检测结果。
具体实施方式
下面结合实施例对本发明作进一步的详细描述。
本领域技术人员将会理解,下列实施例仅用于说明本发明,而不应视为限定本发明的范围。实施例中未注明具体技术或条件者,按照本领域内的文献所描述的技术或条件或者按照产品说明书进行。所用试剂或仪器未注明生产厂商者,均为可以通过购买获得的常规产品。
实施例1
一种低次烟叶固相萃取吸附剂的制备方法,包括以下步骤:
S1. 称取一定量经打叶复烤、仓储的低次烟叶,剪碎成0.5 cm长短的碎片,得到碎烟叶;
S2.将所述碎烟叶加入5倍质量比的、0.5mol/L的NaOH溶液,于50 ℃下水浴 3h,然后抽滤,去掉滤液,得到碎烟叶滤渣;
S3.将所述碎烟叶滤渣用3层中速滤纸包裹,置于索氏提取器中,加入10倍质量的蒸馏水,加热至沸腾,冷凝回流3h,得到低次烟叶固相萃取吸附剂粗产物;
S4.将所述低次烟叶固相萃取吸附剂粗产物冷却至室温,从中速滤纸中取出所述低次烟叶固相萃取吸附剂粗产物,50℃真空干燥,即得所述低次烟叶固相萃取吸附剂。
实施例2
一种低次烟叶固相萃取吸附剂的制备方法,包括以下步骤:
S1. 称取一定量经打叶复烤、仓储的低次烟叶,剪碎成1.2 cm长短的碎片,得到碎烟叶;
S2.将所述碎烟叶加入10倍质量比的、2 mol/L的NaOH溶液,于60 ℃下水浴 5 h,然后抽滤,去掉滤液,得到碎烟叶滤渣;
S3.将所述碎烟叶滤渣用4层中速滤纸包裹,置于索氏提取器中,加入20倍质量的蒸馏水,加热至沸腾,冷凝回流5h,得到低次烟叶固相萃取吸附剂粗产物;
S4.将所述低次烟叶固相萃取吸附剂粗产物冷却至室温,从中速滤纸中取出所述低次烟叶固相萃取吸附剂粗产物,60℃真空干燥,即得所述低次烟叶固相萃取吸附剂。
实施例3
一种低次烟叶固相萃取吸附剂的制备方法,包括以下步骤:
S1. 称取一定量经打叶复烤、仓储的低次烟叶,剪碎成1 cm长短的碎片,得到碎烟叶;
S2.将所述碎烟叶加入8倍质量比的、1 mol/L的NaOH溶液,于55 ℃下水浴 4 h,然后抽滤,去掉滤液,得到碎烟叶滤渣;
S3.将所述碎烟叶滤渣用3层中速滤纸包裹,置于索氏提取器中,加入15倍质量的蒸馏水,加热至沸腾,冷凝回流4h,得到低次烟叶固相萃取吸附剂粗产物;
S4.将所述低次烟叶固相萃取吸附剂粗产物冷却至室温,从中速滤纸中取出所述低次烟叶固相萃取吸附剂粗产物,55℃真空干燥,即得所述低次烟叶固相萃取吸附剂。
实施例4
一种低次烟叶固相萃取吸附剂的制备方法,包括以下步骤:
S1. 称取一定量经打叶复烤、仓储的低次烟叶,剪碎成0.5 cm长短的碎片,得到碎烟叶;
S2.将所述碎烟叶加入6倍质量比的、2 mol/L的NaOH溶液,于60 ℃下水浴 5 h,然后抽滤,去掉滤液,得到碎烟叶滤渣;
S3.将所述碎烟叶滤渣用3层中速滤纸包裹,置于索氏提取器中,加入15倍质量的蒸馏水,加热至沸腾,冷凝回流3h,得到低次烟叶固相萃取吸附剂粗产物;
S4.将所述低次烟叶固相萃取吸附剂粗产物冷却至室温,从中速滤纸中取出所述低次烟叶固相萃取吸附剂粗产物,50℃真空干燥,即得所述低次烟叶固相萃取吸附剂。
实施例5
一种低次烟叶固相萃取吸附剂的制备方法,包括以下步骤:
S1. 称取一定量经打叶复烤、仓储的低次烟叶,剪碎成0.5 cm长短的碎片,得到碎烟叶;
S2.将所述碎烟叶加入5倍质量比的、2 mol/L的NaOH溶液,于60 ℃下水浴 5 h,然后抽滤,去掉滤液,得到碎烟叶滤渣;
S3.将所述碎烟叶滤渣用4层中速滤纸包裹,置于索氏提取器中,加入20倍质量的蒸馏水,加热至沸腾,冷凝回流5h,得到低次烟叶固相萃取吸附剂粗产物;
S4.将所述低次烟叶固相萃取吸附剂粗产物冷却至室温,从中速滤纸中取出所述低次烟叶固相萃取吸附剂粗产物,60℃真空干燥,即得所述低次烟叶固相萃取吸附剂。
实施例6
一种低次烟叶固相萃取吸附剂的应用,包括以下步骤:
首先,制备低次烟叶固相萃取吸附剂,步骤如下:
S1. 称取一定量经打叶复烤、仓储的低次烟叶,剪碎成0.5 cm长短的碎片,得到碎烟叶;
S2.将所述碎烟叶加入6倍质量比的、2 mol/L的NaOH溶液,于60 ℃下水浴 5 h,然后抽滤,去掉滤液,得到碎烟叶滤渣;
S3.将所述碎烟叶滤渣用3层中速滤纸包裹,置于索氏提取器中,加入15倍质量的蒸馏水,加热至沸腾,冷凝回流3h,得到低次烟叶固相萃取吸附剂粗产物;
S4.将所述低次烟叶固相萃取吸附剂粗产物冷却至室温,从中速滤纸中取出所述低次烟叶固相萃取吸附剂粗产物,50℃真空干燥,即得所述低次烟叶固相萃取吸附剂。
其次,利用所述低次烟叶固相萃取吸附剂制备萃取柱,步骤如下:
将所述低次烟叶固相萃取吸附剂作为填料装入带有筛板的SPE空柱管中,轻轻用手指敲打使填料填充均匀,上端盖上筛板压紧,成为烟叶吸附萃取柱,其中,填料的装填高度为2-3cm。
最后,将所制备的萃取柱用于烟草中酚类的检测,本实施例中,选取3份烟草样品,检测的目标物为绿原酸,利用所述萃取柱富集所述目标物后按照YCT202-2006所述的检测条件进行检测,结果如图1所示。
实施例7
一种低次烟叶固相萃取吸附剂的应用,包括以下步骤:
首先,制备低次烟叶固相萃取吸附剂,步骤如下:
S1. 称取一定量经打叶复烤、仓储的低次烟叶,剪碎成1 cm长短的碎片,得到碎烟叶;
S2.将所述碎烟叶加入10倍质量比的、1 mol/L的NaOH溶液,于60 ℃下水浴 5 h,然后抽滤,去掉滤液,得到碎烟叶滤渣;
S3.将所述碎烟叶滤渣用3层中速滤纸包裹,置于索氏提取器中,加入15倍质量的蒸馏水,加热至沸腾,冷凝回流3h,得到低次烟叶固相萃取吸附剂粗产物;
S4.将所述低次烟叶固相萃取吸附剂粗产物冷却至室温,从中速滤纸中取出所述低次烟叶固相萃取吸附剂粗产物,50℃真空干燥,即得所述低次烟叶固相萃取吸附剂。
其次,利用所述低次烟叶固相萃取吸附剂制备萃取柱,步骤如下:
将所述低次烟叶固相萃取吸附剂作为填料装入带有筛板的SPE空柱管中,轻轻用手指敲打使填料填充均匀,上端盖上筛板压紧,成为烟叶吸附萃取柱,其中,填料的装填高度为2-3cm。
最后,将所制备的萃取柱用于烟草中酚类的检测,本实施例中,以烟草为样品,检测的目标物为芸香苷,利用所述萃取柱富集所述目标物后按照YCT202-2006所述的检测方法进行检测,结果如图1所示。
实施例8
一种低次烟叶固相萃取吸附剂的应用,包括以下步骤:
首先,制备低次烟叶固相萃取吸附剂,步骤如下:
S1. 称取一定量经打叶复烤、仓储的低次烟叶,剪碎成1 cm长短的碎片,得到碎烟叶;
S2.将所述碎烟叶加入10倍质量比的、1 mol/L的KOH溶液,于60 ℃下水浴 5 h,然后抽滤,去掉滤液,得到碎烟叶滤渣;
S3.将所述碎烟叶滤渣用4层中速滤纸包裹,置于索氏提取器中,加入20倍质量的蒸馏水,加热至沸腾,冷凝回流3h,得到低次烟叶固相萃取吸附剂粗产物;
S4.将所述低次烟叶固相萃取吸附剂粗产物冷却至室温,从中速滤纸中取出所述低次烟叶固相萃取吸附剂粗产物,60℃真空干燥,即得所述低次烟叶固相萃取吸附剂。
其次,利用所述低次烟叶固相萃取吸附剂制备萃取柱,步骤如下:
将所述低次烟叶固相萃取吸附剂作为填料装入带有筛板的SPE空柱管中,轻轻用手指敲打使填料填充均匀,上端盖上筛板压紧,成为烟叶吸附萃取柱,其中,填料的装填高度为2-3cm。
最后,将所制备的萃取柱用于烟草中酚类的检测,本实施例中,以烟草为样品,检测的目标物为乙基麦芽酚,利用所述萃取柱富集所述目标物后按照GB 5009.250-2016所述的检测方法进行检测,结果如图1所示。
实施例9
一种低次烟叶固相萃取吸附剂的应用,包括以下步骤:
首先,制备低次烟叶固相萃取吸附剂,步骤如下:
S1. 称取一定量经打叶复烤、仓储的低次烟叶,剪碎成0.5 cm长短的碎片,得到碎烟叶;
S2.将所述碎烟叶加入6倍质量比的、2 mol/L的NaOH溶液,于60 ℃下水浴 5 h,然后抽滤,去掉滤液,得到碎烟叶滤渣;
S3.将所述碎烟叶滤渣用3层中速滤纸包裹,置于索氏提取器中,加入15倍质量的蒸馏水,加热至沸腾,冷凝回流3h,得到低次烟叶固相萃取吸附剂粗产物;
S4.将所述低次烟叶固相萃取吸附剂粗产物冷却至室温,从中速滤纸中取出所述低次烟叶固相萃取吸附剂粗产物,50℃真空干燥,即得所述低次烟叶固相萃取吸附剂。
其次,利用所述低次烟叶固相萃取吸附剂制备萃取柱,步骤如下:
将所述低次烟叶固相萃取吸附剂作为填料装入带有筛板的SPE空柱管中,轻轻用手指敲打使填料填充均匀,上端盖上筛板压紧,成为烟叶吸附萃取柱,其中,填料的装填高度为2-3cm。
最后,将所制备的萃取柱用于烟草中烟碱类的检测,本实施例中,以烟草为样品,检测的目标物为尼古丁,利用所述萃取柱富集所述目标物后按照GB T 23355-2009所述的检测方法进行检测,结果如图1所示。
对比例1
利用LiChrolut EN树脂作为填料制备萃取柱,步骤如下:
将LiChrolut EN树脂作为填料装入带有筛板的SPE空柱管中,轻轻用手指敲打使填料填充均匀,上端盖上筛板压紧,成为烟叶吸附萃取柱,其中,填料的装填高度为2-3cm。
将所制备的萃取柱用于烟草中烟碱类的检测,本实施例中,以烟草为样品,检测的目标物为尼古丁,利用所述萃取柱富集所述目标物后按照GB T 23355-2009所述的检测方法进行检测,结果如图2所示。
对比例2
用市售的ALN中性氧化铝柱SPE固相萃取柱用于烟草中酚类的检测,本实施例中,以烟草为样品,检测的目标物为绿原酸,利用所述萃取柱富集所述目标物后按照YCT202-2006所述的检测条件进行检测,结果如图2所示。
对比例3
用市售的PLS固相萃取柱用于烟草中酚类的检测,本实施例中,以烟草为样品,检测的目标物为芸香苷,利用所述萃取柱富集所述目标物后按照YCT202-2006所述的检测方法进行检测,结果如图2所示。
对比例4
用市售的SI固相萃取柱用于烟草中酚类的检测,本实施例中,以烟草为样品,检测的目标物为乙基麦芽酚,利用所述萃取柱富集所述目标物后按照GB 5009.250-2016所述的检测方法进行检测,结果如图2所示。
以上所述,仅为本发明的具体实施方式,但本发明的保护范围并不局限于此,任何属于本技术领域的技术人员在本发明揭露的技术范围内,可轻易想到的变化或替换,都应涵盖在本发明的保护范围之内。因此,本发明的保护范围应该以权利要求的保护范围为准。
Claims (10)
1.一种低次烟叶固相萃取吸附剂的制备方法,其特征在于,包括以下步骤:
S1.剪切低次烟叶,得到碎烟叶;
S2.将所述碎烟叶加入至强碱溶液中,水浴加热回流后过滤,得到碎烟叶滤渣;
S3.利用多层中速滤纸包覆所述碎烟叶滤渣,并用沸水清洗,得到低次烟叶固相萃取吸附剂粗产物;
S4.将所述低次烟叶固相萃取吸附剂粗产物真空干燥,即得所述低次烟叶固相萃取吸附剂。
2.根据权利要求1所述的一种低次烟叶固相萃取吸附剂的制备方法,其特征在于,所述碎烟叶的长度为0.5-1.2cm。
3.根据权利要求1所述的一种低次烟叶固相萃取吸附剂的制备方法,其特征在于,所述强碱为NaOH、KOH中的一种或几种。
4.根据权利要求1所述的一种低次烟叶固相萃取吸附剂的制备方法,其特征在于,所述步骤S2中,强碱溶液的浓度为0.5-2 mol/L。
5.根据权利要求4所述的一种低次烟叶固相萃取吸附剂的制备方法,其特征在于,所述强碱溶液与所述碎烟叶的质量比为(5-10):1。
6.根据权利要求1所述的一种低次烟叶固相萃取吸附剂的制备方法,其特征在于,所述步骤S2中,所述加热温度为50-60℃,所述加热时间为3-5h。
7.根据权利要求1所述的一种低次烟叶固相萃取吸附剂的制备方法,其特征在于,所述步骤S3中,所述沸水与所述碎烟叶滤渣的质量比为(10-20):1。
8.根据权利要求1所述的一种低次烟叶固相萃取吸附剂的制备方法,其特征在于,所述步骤S3中,所述中速滤纸的层数为3-4层。
9.根据权利要求1所述的一种低次烟叶固相萃取吸附剂的制备方法,其特征在于,所述步骤S4中,真空干燥的温度为50-60℃。
10.一种如权利要求1-9所述的制备方法所制备的低次烟叶固相萃取吸附剂的应用,其特征在于,将所述低次烟叶固相萃取吸附剂作为萃取柱填料用于富集纯化烟草中酚类或烟碱类物质。
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