CN1611937A - 一种快速分析粉末大豆磷脂成分的方法 - Google Patents

一种快速分析粉末大豆磷脂成分的方法 Download PDF

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CN1611937A
CN1611937A CN 200310111969 CN200310111969A CN1611937A CN 1611937 A CN1611937 A CN 1611937A CN 200310111969 CN200310111969 CN 200310111969 CN 200310111969 A CN200310111969 A CN 200310111969A CN 1611937 A CN1611937 A CN 1611937A
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李卫
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Abstract

一种快速分析粉末大豆磷脂成分的方法。是采用2.5cm×7.5cm的载玻片制成的硅胶板作为薄层层析板，用一种高效展开剂，使粉末大豆磷脂成分在2.5cm×7.5cm的载玻片薄层层析板上得到快速展开和分离。然后用几种显色剂进行组合显色，不需要用价格昂贵的标准品，即可确定粉末大豆磷脂成分及含量。所需时间仅为20cm×20cm薄层层析板的1/5，展开剂用量仅为5～10ml。

Description

一种快速分析粉末大豆磷脂成分的方法
技术领域
本发明涉及产品分析检测领域，尤其涉及对现有粉末大豆磷脂成分的分析方法进行改进和创新，达到快速、简便、低成本地分析粉末大豆磷脂成分的目的。
背景技术
常规定磷法只能分析粉末大豆磷脂样品中总磷脂含量，不能确定粉末大豆磷脂样品中各磷脂成分(卵磷脂、脑磷脂、肌醇磷脂)及其含量。
国外通常采用高效液相色谱或核磁共振31P-NMR法对粉末大豆磷脂成分进行分析，但这两种仪器价格昂贵，普通实验室不具备。所以对粉末大豆磷脂成分进行分析，一直是困扰生产厂家的难题。
普通实验室通常采用薄层层析法对粉末大豆磷脂成分进行分析。其方法是采用20cm×20cm的薄层层析板，将粉末大豆磷脂用溶剂溶解，然后与各磷脂标准品溶液在同一直线处点样、展开(各点相距2～3cm)。用碘蒸汽显色。将粉末大豆磷脂各磷脂成分的斑点与各标准品斑点进行比较，从而确定粉末大豆磷脂的成分，进而确定其含量。该方法需要用到纯的标准品，而这些用于分析检测的纯标准品价格极贵，也很不稳定，难以保存，几乎是一次性使用。其次，20cm×20cm的薄层层析板用于分析需要耗费很长时间，而且展开剂的用量太大，造成很大的浪费和环境污染。
发明内容
根据现有粉末大豆磷脂成分分析方法所存在的上述缺点，本发明所要解决的粉末大豆磷脂成分分析方案是：要提供一种高效展开剂，使粉末大豆磷脂各磷脂成分在很小的薄层层析板上得到快速分离。其次，采用显色剂组合显色法确定各磷脂成分，不用价格昂贵的标准品。
为此，本发明的技术方案是：采用2.5cm×7.5cm的载玻片制成的硅胶板作为薄层层析板，点样后用高效展开剂展开，采用几种显色剂进行组合显色。具体方法是：
称取适量粉末大豆磷脂，用溶剂溶解配制成一定浓度。在距薄板下端0.5～1cm处点样。将已点样的薄层层析板放入到装有展开剂的层析缸中，当展开剂上升到薄层层析板高度的4/5处，取出薄层层析板。将上述薄层层析板在室温下放置几分钟，待溶剂挥发后，用显色剂1喷在薄板上，卵磷脂斑点会显示橙色，而其它磷脂斑点不显色。用显色剂2喷在薄板上，在烘箱中加热几分钟，脑磷脂斑点会显示粉红色。对上述两种显色剂不显色，而对碘蒸气显色的斑点即为肌醇磷脂。若要进行定量分析，可采用定磷分析法计算各磷脂的含量。
采用本发明方法对粉末大豆磷脂成分进行分析，所需时间仅为20cm×20cm大薄层层析板的1/5，展开剂用量减少了80％。进行定量分析时其结果与用20cm×20cm的大薄层层析板分析结果相同。
本发明所用展开剂如下：
展开剂为氯仿、甲醇、乙酸乙酯和水的混合物。其中氯仿含量为20～30％，甲醇含量为50～70％，乙酸乙酯含量为5～10％，水的含量为5～15％，(重量比)。调节pH至2～5。
本发明所用显色剂如下：
1.显色剂1
将醋酸、硝酸铋、碘化钾溶于水中，其中醋酸含量控制在0.5～5％。硝酸铋的含量控制在1～10％，碘化钾的含量控制在3～10％(重量比)。
2.显色剂2
将茚三酮溶于醇中配成0.1～1％的溶液。在此溶液中加入浓度为5～15％醋酸水溶液。醋酸水溶液的加入量控制在3～15％(重量比)。
具体实施方式1
粉末大豆磷脂成分的定性分析：用毛细管蘸取粉末大豆磷脂的氯仿浓溶液，在距薄层层析板底部约0.5～1cm处点样。将点样后的薄层层析板放入装有展开剂的烧杯中。烧杯上部用塑料薄膜封口，使溶剂不能挥发出来。待展开剂上升到薄层层析板高度的4/5处时，取出薄层层析板。将此薄层层析板在室温下放置几分钟，待溶剂挥发后，用显色剂1喷在薄板上，卵磷脂斑点会显示橙色，而其它磷脂斑点不显色。然后用显色剂2喷在薄板上，在烘箱中加热几分钟，脑磷脂斑点会显示粉红色。对上述两种显色剂不显色，而对碘蒸汽显棕色的斑点即为肌醇磷脂。
具体实施方式2
粉末大豆磷脂成分的定量分析：准确称取30mg粉末大豆磷脂，用氯仿溶解，制成1％的粉末大豆磷脂氯仿溶液。用微量注射器吸取10μl此溶液，在距薄层层析板底部约0.5～1cm处点样。将点样后的薄层层析板放入装有展开剂的烧杯中，烧杯上部用塑料薄膜封口，使溶剂不能挥发出来。待展开剂上升到薄层层析板高度的4/5处时，取出薄层层析板。将上述薄层层析板在室温下放置几分钟，待溶剂挥发后，用显色剂进行组合显色，采用定磷分析法计算各磷脂的含量。

Claims (4)

1.一种快速分析粉末大豆磷脂成分的方法。其特征是：用一种高效展开剂，使粉末大豆磷脂成分在2.5cm×7.5cm的载玻片制成的硅胶薄层层析板上得到快速完全展开和分离，然后用显色剂1和显色剂2进行组合显色，以确定粉末大豆磷脂中含有何种磷脂成分。整个分析过程不需用标准品。
2.根据权利要求1所述的快速分析粉末大豆磷脂成分的方法，其特征是高效展开剂是氯仿、甲醇、乙酸乙酯和水的混合物。其中氯仿含量为20～30％，甲醇含量为50～70％，乙酸乙酯含量为5～10％，水的含量为5～15％，(重量比)。调节pH至2～5。
3.根据权利要求1所述的快速分析粉末大豆磷脂成分的方法，其特征是显色剂1是醋酸、硝酸铋、碘化钾混合水溶液，其中醋酸含量为0.5～5％，硝酸铋的含量为1～10％，碘化钾的含量为3～10％(重量比)。
4.根据权利要求1所述的快速分析粉末大豆磷脂成分的方法，其特征是显色剂2是0.1～1％的茚三酮醇溶液中加入浓度为5～15％醋酸水溶液。醋酸水溶液的加入量为3～15％(重量比)。
CNB2003101119698A 2003-10-31 2003-10-31 一种分析粉末大豆磷脂成分的方法 Expired - Fee Related CN1297817C (zh)

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CN102175811A (zh) * 2011-01-10 2011-09-07 江苏省农业科学院 一种鉴别卵磷脂纯度的方法

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RU1778684C (ru) * 1990-10-10 1992-11-30 Институт физиологии растений им.К.А.Тимирязева Способ определени границ хроматографических зон отдельных классов фосфолипидов при разделении их смеси методом тонкослойной хроматографии
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CN102175811B (zh) * 2011-01-10 2012-05-09 江苏省农业科学院 一种鉴别卵磷脂纯度的方法

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