CN114618456A - 一种末端极性的反相色谱固定相及其制备方法 - Google Patents
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Abstract
本发明涉及液相色谱固定相，其特征在于键合相中末端含有极性基团，其结构式如下：
其中Silica Gel为硅胶，m＝1‑30，R为卤素原子。本发明还提供了上述液相色谱固定相的制备方法，通过水平聚合的方法在硅胶表面进行修饰，制备得到含有末端极性基团的耐纯水的反相色谱固定相。本发明提供的分离材料结构新颖，可以改善烷基链的分离选择性，适用于各类化合物的分离分析。
Description
技术领域
本发明涉及液相色谱固定相，具体地说是一种含有末端极性基团的反相色谱固定相。
技术背景
反相液相色谱具有柱效高、分离能力强、保留机理清楚等优点，是液相色谱分离模式中使用最为广泛的一种，广泛应用于生物大分子、蛋白质及酶的分离分析。反相色谱是以表面非极性载体为固定相，以比固定相极性强的溶剂为流动相的一种液相色谱分离模式。反相色谱固定相大多是硅胶表面键合疏水基团，基于样品中的不同组分和疏水基团之间疏水作用的不同而分离。
烷基固定相作为反相固定相中使用最多的一种固定相，如C18、C12、C8等固定相，对大多数化合物具有良好的分离选择性。但是当使用反相固定相对碱性化合物进行分析时，除了疏水作用，还伴随着碱性化合物和硅胶表面残留的硅烷醇之间的静电相互作用，因此会导致碱性化合物的峰形拖尾等[Borges,E.M.et al,J.Pharm.Biomed.Anal,2013,77,100-115]。同时单一的烷基链结构固定相不能在纯水条件使用，限制了其在反相弱保留化合物中的使用。为了进一步拓宽烷基色谱固定相的适用范围，同时提升分离选择性，需要开发出耐纯水的色谱固定相。当反相固定相中引入极性基团时，可以增加酸性化合物的保留，同时减弱碱性化合物的吸附，并且由于固定相的极性增加，对疏水性化合物的保留减弱，因此在分析不同种类样品时具有良好的选择性。
发明内容
本发明的目的是提供一种新型反相色谱固定相及其制备方法。该键合相包含末端极性基团同时含有疏水碳链，其制备方法简单，适用性广泛。
本发明的目技术方案是：液相色谱固定相，其特征在于结构为：
其中Silica Gel为硅胶，m＝1-30整数，R为卤素原子(F、Cl、Br中的一种)。
本发明还提供了上述固定相的制备方法，其特征在于包括如下步骤：
a.硅胶加入质量浓度为10～50wt％的强酸溶液中，加热回流搅拌1～48小时，过滤，固体用水洗涤至pH＝6～7，所得固体于干燥箱中100～160℃条件下干燥至恒重；所得干燥硅胶置于干湿度为10％～80％的气氛中12～72小时，使硅胶吸水增重干燥硅胶质量的1％～10％，得水合硅胶；
以每克硅胶计，强酸溶液的用量3-5mL；
b.硅水平聚合反应：在氮气和/或氩气保护下，在有机溶剂中加入带末端卤素的烷基硅烷偶联剂和步骤a所得水合硅胶；在25～60℃下反应3～48小时，过滤，依次用乙醇、乙腈、体积比1：1-3的甲醇水、乙醇、四氢呋喃洗涤，所得固体于干燥箱中40～80℃条件下干燥8～16小时，得到色谱固定相；
以每克硅胶计，硅烷偶联剂的用量为0.5-2.4mmol，有机溶剂的用量为4-10mL。
本发明具有如下优点：
1.结构新颖。本发明首次提出末端含有极性基团的反相色谱固定相。该固定相结构中末端带有极性卤素原子，可作为耐纯水的色谱固定相，同时也含有疏水碳链，可以改善绝大部分天然产物及药物的分离选择性，适用于各类样品的分离分析及纯化制备。
2.本发明提供的液相色谱固定相制备过程简单可靠，有利于实现产业化。
附图说明
图1为实施例5的色谱图。
具体实施方式
下面结合实例，对本发明做进一步说明。实例仅限于说明本发明，而非对本发明的限定。
实施例1
向100mL烧瓶中加入10g硅胶，加入100mL浓度为15wt％的盐酸溶液中，加热回流搅拌12小时，过滤，用水洗涤至pH＝6～7，所得固体于干燥箱中160℃条件下干燥24小时，所得干燥硅胶置于干湿度为30％的气氛中72小时，使硅胶吸水增重干燥硅胶质量的3％，得水合硅胶。
在氮气保护下，向100mL烧瓶中加入10g水合硅胶(粒径为5μm，孔径为10nm)、3.9g11-氯十一烷基三氯硅烷(摩尔数为12mmol)和60mL二甲苯，在25℃下反应3小时，过滤，依次用乙醇、乙腈、体积比1：1的甲醇水、乙醇、四氢呋喃洗涤，所得固体在干燥箱中80℃条件下干燥16个小时，得到色谱固定相1，结构如下：
实施例2
与实施例1不同之处在于使用8-氯辛基三氯硅烷(摩尔数为16mmol)代替11-氯十一烷基三氯硅烷(摩尔数为12mmol)，得到色谱固定相2，结构如下：
实施例3
向100mL烧瓶中加入10g硅胶，加入100mL浓度为25wt％的盐酸溶液中，加热回流搅拌2小时，过滤，用水洗涤至pH＝6～7，所得固体于干燥箱中160℃条件下干燥16小时，所得干燥硅胶置于干湿度为50％的气氛中12小时，使硅胶吸水增重干燥硅胶质量的2.7％，得水合硅胶。
在氮气保护下，向100mL烧瓶中加入10g水合硅胶(粒径为2.5μm，孔径为10nm)、4.7g 18-溴十八烷基三氯硅烷(摩尔数为14mmol)和80mL二甲苯，在40℃下反应6小时，过滤，依次用乙醇、乙腈、体积比1：2的甲醇水、乙醇、四氢呋喃洗涤，所得固体在干燥箱中60℃条件下干燥12个小时，得到色谱固定相3，结构如下：
实施例4
与实施例3不同之处在于使用30-氯三十烷基三氯硅烷(摩尔数为8mmol)代替18-溴十八烷基三氯硅烷(摩尔数为14mmol)，得到色谱固定相4，结构如下：
实施例5
使用实施例1所得色谱固定相1装填4.6×50mm色谱柱，用于浸润性测试样品的分离分析。如图1所示，填料在纯水浸润后，各化合物仍得到很好的分离，说明填料的浸润性良好。色谱条件为：
色谱柱：4.6×50mm；
样品：浸润性测试混标(尿嘧啶1mg/mL，胞嘧啶1.2mg/mL，胸腺嘧啶2mg/mL)；
溶剂：A：乙腈，B：100mM甲酸铵(pH＝3.2)；
洗脱：A：B＝90：10；
流速：1.0mL/min；
柱温：30℃；
检测：DAD(190nm-400nm)&UV(254nm)。
Claims (9)
1.一种末端极性的反相色谱固定相，其特征在于：键合相中含有极性末端基团及疏水碳链；其结构式如下：
其中Silica Gel为硅胶，m＝1-30整数，R为卤素原子(F、Cl、Br中的一种)。
2.按照权利要求1所述的色谱固定相，其特征在于：每克硅胶上含有0.5-2.4mmolR。
3.一种权利要求1或2所述的固定相的制备方法，其特征在于，包括如下步骤：
a.硅胶加入质量浓度为10～50wt％的强酸溶液中，加热回流搅拌1～48小时，过滤，固体用水洗涤至pH＝6～7，所得固体于干燥箱中100～160℃条件下干燥至恒重；所得干燥硅胶置于干湿度为10％～80％的气氛中12～72小时，使硅胶吸水增重干燥硅胶质量的1％～10％，得水合硅胶；
b.水平聚合反应：在氮气和/或氩气保护下，在有机溶剂中加入带末端卤素的烷基硅烷偶联剂和步骤a所得水合硅胶；在25～60℃下反应3～48小时，过滤，依次用乙醇、乙腈、体积比1：1-3的甲醇水、乙醇、四氢呋喃洗涤，所得固体于干燥箱中40～80℃条件下干燥8～16小时，得到色谱固定相。
4.按照权利要求3所述的制备方法，其特征在于：步骤a所用的强酸为盐酸、硝酸、硫酸中的一种。
5.按照权利要求3所述的制备方法，其特征在于：步骤b所用的硅烷偶联剂有如下结构：
其中，X为氯、甲氧基或乙氧基中的一种或二种以上，m＝1-30整数，R为卤素基团(F、Cl、Br中的一种)。
6.按照权利要求3所述的制备方法，其特征在于：步骤b所用的有机溶剂为二氯甲烷、乙腈、氯苯、甲苯、二甲苯、正庚烷、异辛烷中的一种。
7.按照权利要求3所述的制备方法，其特征在于：
步骤a所用的强酸溶液的用量为每克硅胶3-5mL；
步骤b所用的有机溶剂的用量为每克硅胶4-10mL；
步骤b所用的硅烷偶联剂的用量为每克硅胶0.5-2.4mmol。
8.一种权利要求1或2所述的固定相在色谱分离过程中的应用。
9.按照权利要求8所述的应用，其特征在于：色谱分离模式为反相色谱分离。
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