中文摘要：一种用于食品中农药残留检测的色谱柱，通过以下步骤制得：(1)将环糊精2,6-位羟基上的氢取代为醚，合成出环糊精衍生物；(2)将合成出的环糊精衍生物和3-[(2,3)-环氧丙氧]丙基三甲氧基硅烷在乙醇溶液中反应，接着加入单体四甲氧基硅烷和催化剂盐酸溶液，反应分离后得到清液；(3)对石英毛细管内表面进行前处理，使毛细管内表面形成硅羟基；(4)把清液填充到毛细管柱中，制作成气相色谱柱。本发明所制备的色谱柱能够应用到各种粮食、蔬菜和瓜果等食品中手性农药残留的检测。
外文摘要：NOVELTY - A Chromatographic column is obtained by taking cyclodextrin as reaction raw material.The cyclodextrin derivative and 3-((2, 3)-epoxy propoxy) propyl group trimethoxy silane are synthesized and reacted with alcohol solution and filtered a precipitate based on centrifugal separation. Dichloromethane solution and sodium hydroxide solution are added with inner surface of a quartz capillary tube. The quartz capillary tube inner surface is filled with silicon hydroxyl. The blood capillary column is filled with clear liquid and raised temperature for aging process to obtain the finished product.
 
USE - Chromatographic column for detecting pesticide residue in food.
 
DETAILED DESCRIPTION - A Chromatographic column is obtained by taking cyclodextrin as reaction raw material, hydroxyl and hydrogen substitute ether with a synthesizing cyclodextrin derivative. The cyclodextrin derivative and 3-((2, 3)-epoxy propoxy) propyl group trimethoxy silane are synthesized and reacted with alcohol solution, added with monomer tetramethoxysilane and catalyst hydrochloric acid solution by a mixing using ultrasonic stirrer to obtain clear liquid and filtered a precipitate based on centrifugal separation. Dichloromethane solution and sodium hydroxide solution are added with inner surface of a quartz capillary tube. The quartz capillary tube inner surface is filled with silicon hydroxyl and dichloromethane solution for clean water washing process. The blood capillary column is filled with clear liquid and raised temperature for aging process to obtain the finished product.
 
主权项：.一种用于食品中农药残留检测的色谱柱，该气相色谱柱通过 以下步骤制得：
(1)以环糊精作为反应原料，将环糊精2,6-位羟基上的氢取代 为醚，合成出环糊精衍生物；
(2)将合成出的环糊精衍生物和3-[(2,3)-环氧丙氧]丙基三甲 氧基硅烷在乙醇溶液中反应，接着加入单体四甲氧基硅烷和催化剂盐 酸溶液，然后将混合物超声搅拌，离心分离，滤去沉淀物，得到清液；
(3)对石英毛细管内表面用二氯甲烷溶液进行沥洗，再用氢氧 化钠溶液进行沥洗，然后用清水冲洗，使毛细管内表面形成硅羟基；
(4)把清液填充到毛细管柱中，在柱中保持一段时间后，将柱 内液体吹出，最后程序升温进行老化。
2.根据权利要求1所述的色谱柱，其中与环糊精进行醚化的试剂 为氯甲基甲醚。
3.根据权利要求1所述的色谱柱，步骤(4)的老化工艺条件为： 升温速率为0.5-2℃/min，温度为150-180℃，保温4-8小时。
4.根据权利要求1所述的色谱柱，环糊精为β-环糊精。
申请号：CN201510638012.1
公开/公告号：CN105241983A
申请日：2015-09-30
公开/公告日：2016-01-13
申请/专利权人：赵林萍
发明/设计人：赵林萍
分类号：G01N30/60
主分类号：G01N30/60
法律状态：实质审查
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