CN113244902A - 天然高分子材料丝瓜络作为固相萃取吸附剂的应用 - Google Patents
天然高分子材料丝瓜络作为固相萃取吸附剂的应用 Download PDFInfo
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Abstract
本发明涉及天然高分子材料丝瓜络作为固相萃取吸附剂的应用,首先通过极性溶剂索氏提取清洗,然后干燥,即得到丝瓜络材料,然后将所得丝瓜络粉体填充于固相萃取小柱的柱筒中,进行固相萃取。该材料的清洗方法简单,安全易实施,原料便宜易得。利用该制备方法得到的材料重现性好,其作为固相萃取的填料用于油性样品中极性化合物的分离和富集,具有除杂效果好,回收率高,稳定性好等特点。
Description
技术领域
本发明首次采用了天然材料丝瓜络作为固相萃取的吸附介质并将其应用于极性化合物的样品前处理,属于分析化学技术领域。
背景技术
固相萃取技术(SPE)是出现于20世纪70年代中期的一种试样预处理技术。它设备简单,分离和浓缩合为一步,是目前样品处理最简捷、高效、灵活的一种手段。其中SPE吸附剂是SPE的核心,最常用的SPE吸附剂为十八烷基键合硅胶(C18)。近年来,为了使SPE技术的选择性和灵敏度进一步提高,开发新的固相萃取吸附剂成为SPE技术发展的主要方向。C8、氰基、氨基、苯基、双醇基填料、活性碳、硅胶、氧化铝、硅酸镁、高分子聚合物、离子交换剂、排斥色谱填料、亲和色谱填料和凝胶色谱填料等也被广泛用作固相萃取填料。
虽然许多新型固相萃取剂能综合应用多种作用机制,大大拓展了固相萃取方法的应用范围,但对于复杂基体中强极性化合物的萃取仍然是个难题。随着环境、食品和生物等复杂体系样品的增多,分析工作者急需一种解决上述问题的新型吸附剂。
随着人们对绿色分析化学重视程度的提高,天然吸附剂显示出广阔的应用前景。与传统的合成吸附剂相比,天然吸附剂具有毒性小、来源广、成本低和处理简单等独特优点。
发明内容
本发明的目的在于提供丝瓜络在固相萃取吸附中的应用,可用于复杂基质样品中痕量极性化合物的萃取。
本发明解决上述技术问题所采用的方案是:
天然高分子材料丝瓜络作为固相萃取吸附剂的应用,包括如下步骤:
(1)丝瓜络的预处理:将丝瓜络加入液氮磨碎,用NaOH溶液浸泡清洗,水洗至中性后置于索氏提取器中,分别加入水和甲醇,加热回流清洗,干燥得到预处理的丝瓜络粉体;
(2)将所得丝瓜络粉体填充于固相萃取小柱的柱筒中,进行固相萃取。
优选地,采用1mol/L的NaOH溶液对丝瓜络进行浸泡清洗。
优选地,步骤(1)丝瓜络磨碎至毫米级别。
优选地,所述固相萃取吸附剂用于极性化合物的萃取。
优选地,步骤(2)固相萃取过程中,所用的洗脱液为具有极性的单一或混合溶液,更加优选为中等极性至强极性的单一或混合溶液。
丝瓜络为葫芦科植物丝瓜成熟果实的维管束,是由多层丝状纤维纵横交织而成的立体多孔网状物,具有难分解、耐高温,稳定性好,具有抗强酸、碱的特性。其不溶于有机酸、无机酸、无机盐、脂溶剂等,表面含有羟基、醛基等极性基团,可以与极性化合物发生亲水作用、离子交换作用和氢键作用,因此丝瓜络可作为理想的极性化合物的固相萃取材料。目前已有文献将丝瓜络应用于污水处理,主要是对污水中重金属离子、染料分子等进行吸附,本申请创造性地将丝瓜络材料用于固相萃取介质,利用其表面存在能与极性化合物相互作用的官能团例如羟基、氨基等,同时还具有较好的脱吸附效果,使目标分析物可以通过较为简单的方式从固相萃取填料上解吸下来,实现进一步的检测以及丝瓜络的回收利用。
附图说明
图1为本发明实施例选用的丝瓜络的扫描电镜图;
图2为本发明实施例选用的丝瓜络的漫反射红外光谱图;
图3为采用丝瓜络对食用油中白藜芦醇的萃取分析结果;
图4为采用丝瓜络对发动机润滑油中苯并三氮唑的萃取分析结果。
具体实施方式
为更好的理解本发明,下面的实施例是对本发明的进一步说明,但本发明的内容不仅仅局限于下面的实施例。
实施例1丝瓜络的预处理:
首先将丝瓜络加入液氮,磨碎至毫米级别,然后用1mol/L NaOH溶液浸泡清洗,水洗至中性后置于索氏提取器中,然后分别加入水和甲醇,加热回流清洗,最后60℃烘箱干燥,得到固相萃取剂丝瓜络。
实施例2丝瓜络应用于食用油中白藜芦醇的萃取分析
称取1g生活中常用的食用油于10mL容量瓶中,加入正己烷稀释至刻度线,作为上样液待用。
准确称取200mg实施例1所得丝瓜络于3mL带有筛板的SPE空柱管中,不断敲打使其填充均匀,上端盖上筛板压紧;将5mL去离子水、3mL丙酮和2mL正己烷依次通过该SPE萃取柱,流速小于1mL/min;接着将1mL上述上样液加入SPE柱,使其在重力作用下缓慢流过萃取柱,流速小于1mL/min;然后加入3mL正己烷/异丙醇(80/20,v/v)溶液作为清洗液,保持流速小于1mL/min通过萃取柱,以去除吸附在柱上的残余基质,并在真空泵负压下将清洗液抽干;最后加入1.5mL乙醇作为洗脱液,保持其流速小于1mL/min通过萃取柱并在真空泵负压下将洗脱液抽干,收集洗脱物于离心管中,置于40℃氮吹下浓缩至干,用200μL色谱纯异丙醇溶解残渣,取5μL进入高效液相色谱紫外检测仪(HPLC-UV)分析。
采用HPLC-UV进行定量检测,分析柱为Hisep C18-T(250mm×4.6mm i.d.,5μm);流动相条件为A:去离子水,流动相B:乙腈,流动相为A/B(60/40,v/v),流速为1mL/min;柱温为40℃;检测器波长为306nm。
检测结果:对食用油中白藜芦醇的加标回收率为77.4%,RSD为5.2%。附图3为添加白藜芦醇标样于食用油中后采用丝瓜络固相萃取后检测到的白藜芦醇色谱图。
实施例3丝瓜络应用于润滑油中苯并三氮唑的萃取分析
称取1g经过使用的发动机润滑油于10mL容量瓶中,加入正己烷稀释至刻度线,作为上样液待用。
准确称取200mg实施例1所得丝瓜络于3mL带有筛板的SPE空柱管中,不断敲打使其填充均匀,上端盖上筛板压紧;将5mL去离子水、3mL丙酮和2mL正己烷依次通过该SPE萃取柱,流速小于1mL/min;接着将1mL上述上样液加入SPE柱,使其在重力作用下缓慢流过萃取柱,流速小于1mL/min;然后加入3mL正己烷作为清洗液,保持流速小于1mL/min通过萃取柱,以去除吸附在柱上的残余基质,并在真空泵负压下将清洗液抽干;最后加入5mL正己烷/异丙醇(80/20,v/v)溶液作为洗脱液,保持其流速小于1mL/min通过萃取柱并在真空泵负压下将洗脱液抽干,收集洗脱物于离心管中,置于40℃氮吹下浓缩至干,用1mL色谱纯异丙醇溶解残渣,取5μL进入高效液相色谱紫外检测仪(HPLC-UV)分析。
采用HPLC-UV进行定量检测,分析柱为Hisep C18-T(250mm×4.6mm i.d.,5μm);流动相条件为A:去离子水,流动相B:乙腈,流动相梯度为0-8min:30-95%B,8-15min:95%B,15-16min:95-30%B,16-35min:30%B,流速为1mL/min;柱温为40℃;检测器波长为260nm。
检测结果:对发动机润滑油中苯并三氮唑的加标回收率为50.1%,RSD为10.1%。附图4为添加苯并三氮唑标样于发动机润滑油中后采用丝瓜络固相萃取后检测到的苯并三氮唑色谱图。
实施例4丝瓜络应用于肌肽的萃取分析
称取10mg肌肽标准品溶解于去离子水中,加入10mL容量瓶中,以去离子水稀释至刻度线,保存于4℃冰箱中,作为母液待用。将母液以乙腈稀释至浓度为1μg/mL,作为上样液待用。
准确称取40mg实施例1所得丝瓜络于1mL带有筛板的SPE空柱管中,不断敲打使其填充均匀,上端盖上筛板压紧;将2mL乙腈通过该SPE萃取柱,流速小于1mL/min;接着将0.2mL上述上样液加入SPE柱,使其在重力作用下缓慢流过萃取柱,流速小于1mL/min;然后加入1mL乙腈作为清洗液,保持流速小于1mL/min通过萃取柱,以去除未吸附在材料上或者吸附力度不强的物质,并在真空泵负压下将清洗液抽干;最后加入1mL去离子水作为洗脱液,保持其流速小于1mL/min通过萃取柱并在真空泵负压下将洗脱液抽干,收集洗脱物于离心管中,置于高速离心机中以10000r/min离心10min,取5μL上清液进入高效液相色谱-串联质谱(HPLC-MS/MS)分析。
液相色谱条件:分析柱为Pntulips BP-C18(150mm×2.1mm i.d.,5μm);流动相A:去离子水,流动相B:乙腈;流动相为A/B(50/50,v/v);进样量:5μL;流速:0.2mL/min;柱温:40℃。
质谱条件:离子源:电喷雾离子源(ESI);扫描方式:多反应监测(MRM),设置母离子为227.1,子离子为110.1MRM定量通道。脱溶剂(DL)管温度250℃,加热模块温度400℃,雾化气流速3mL/min,干燥气流速15mL/min。
检测结果:对肌肽的萃取回收率为72.2%,RSD为7.3%。
实施例5丝瓜络应用于咪唑丙酸的萃取分析
称取10mg咪唑丙酸标准品溶解于去离子水中,加入10mL容量瓶中,以去离子水稀释至刻度线,保存于4℃冰箱中,作为母液待用。将母液以乙腈稀释至浓度为1μg/mL,作为上样液待用。
准确称取40mg实施例1所得丝瓜络于1mL带有筛板的SPE空柱管中,不断敲打使其填充均匀,上端盖上筛板压紧;将2mL乙腈通过该SPE萃取柱,流速小于1mL/min;接着将0.2mL上述上样液加入SPE柱,使其在重力作用下缓慢流过萃取柱,流速小于1mL/min;然后加入1mL乙腈作为清洗液,保持流速小于1mL/min通过萃取柱,以去除未吸附在材料上或者吸附力度不强的物质,并在真空泵负压下将清洗液抽干;最后加入1mL去离子水作为洗脱液,保持其流速小于1mL/min通过萃取柱并在真空泵负压下将洗脱液抽干,收集洗脱物于离心管中,置于高速离心机中以10000r/min离心10min,取5μL上清液进入高效液相色谱-串联质谱(HPLC-MS/MS)分析。
液相色谱条件:分析柱为Pntulips BP-C18(150mm×2.1mm i.d.,5μm);流动相A:去离子水,流动相B:乙腈;流动相为A/B(50/50,v/v);进样量:5μL;流速:0.2mL/min;柱温:40℃。
质谱条件:离子源:电喷雾离子源(ESI);扫描方式:多反应监测(MRM),设置母离子为141.0,子离子为81.0MRM定量通道。脱溶剂(DL)管温度250℃,加热模块温度400℃,雾化气流速3mL/min,干燥气流速15mL/min。
检测结果:对咪唑丙酸的萃取回收率为70.0%,RSD为6.1%。
以上所述是本发明的优选实施方式而已,当然不能以此来限定本发明之权利范围,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和变动,这些改进和变动也视为本发明的保护范围。
Claims (5)
1.天然高分子材料丝瓜络作为固相萃取吸附剂的应用,其特征在于,包括如下步骤:
(1)丝瓜络的预处理:将丝瓜络加入液氮磨碎,用NaOH溶液浸泡清洗,水洗至中性后置于索氏提取器中,分别加入水和甲醇,加热回流清洗,干燥得到预处理的丝瓜络粉体;
(2)将所得丝瓜络粉体填充于固相萃取小柱的柱筒中,进行固相萃取。
2.根据权利要求1所述的应用,其特征在于,采用1mol/L的NaOH溶液对丝瓜络进行浸泡清洗。
3.根据权利要求1所述的应用,其特征在于,步骤(1)丝瓜络磨碎至毫米级。
4.根据权利要求1所述的应用,其特征在于,所述固相萃取吸附剂用于极性化合物的萃取。
5.根据权利要求1所述的应用,其特征在于,步骤(2)固相萃取过程中,所用的洗脱液为具有极性的单一或混合溶液。
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