中文摘要：用于食品中手性农药残留检测的气相色谱柱的制作方法，包括以下步骤：(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。本发明所制备的气相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 pesticide residues in food detecting, chiral GC column preparing method involves obtaining cyclodextrin derivatives. The cyclodextrin derivatives and 3-((2,3)-propylene propoxyl propyl trimethoxysilane are added in ethanol solution, hydrochloric acid catalyst and tetramethoxysilane monomer solution is added, the precipitate is filtered off, to obtain supernatant, followed by adding leaching solution, washing inner surface of the capillary quartz with dichloromethane, rinsing so that the inner surface of the capillary forming a silicon hydroxyl, to obtain liquid filled capillary column.
 
USE - Method for preparing pesticide residues chiral GC column for detecting chiral pesticide residual in grain, vegetable and melon fruit and other food product.
 
DETAILED DESCRIPTION - A pesticide residues in food detecting, chiral GC column preparing method involves taking cyclodextrin as reaction raw material, cyclodextrin substituted hydroxyl groups on 2,6-position to obtain cyclodextrin derivatives. The cyclodextrin derivatives and 3-((2,3)-propylene propoxyl propyl trimethoxysilane are added in ethanol solution, hydrochloric acid catalyst and tetramethoxysilane monomer solution is added and mixture ultrasound and centrifuged, the precipitate is filtered off, to obtain supernatant, followed by adding leaching solution, washing inner surface of the capillary quartz with dichloromethane, and with sodium hydroxide solution, rinsing with water, so that the inner surface of the capillary forming a silicon hydroxyl, to obtain clear liquid filled capillary column, after a period of time, blown out of the last temperature for aging.
主权项：一种用于食品中手性农药残留检测的气相色谱柱的制作方 法，包括以下步骤：
(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所述的气相色谱柱的制作方法，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所述的气相色谱柱的制作方法，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所述的气相色谱柱的制作方法，环糊精为β-环 糊精。
申请号： CN201510641699.4
公开/公告号： CN105353061A
申请日：2015-09-30
公开/公告日：2016-02-24
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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