Mulholland G K
Division of Nuclear Medicine, University of Michigan, Ann Arbor 48109.
Int J Rad Appl Instrum A. 1991;42(11):1003-8. doi: 10.1016/0883-2889(91)90001-h.
No-carrier-added trimethylsilyl[18F]fluoride (TMS[18F]F) was rapidly liberated from a variety of dry supports containing unreactive [18F]fluoride by simply heating with neat bistrimethylsilylsulfate. The supports included calcium phosphate, anion exchange resins, alumina, borosilicate and porous carbon beads, to which [18F]fluoride was applied by absorption or evaporation of aqueous solution. TMS[18F]F was evolved essentially free of entrained moisture or excess silylating agent and was efficiently absorbed and rapidly cleaved to free [18F]fluoride ion by 0.1% benzyltrimethylammonium methoxide in anhydrous methanol. Passage of this solution through a strong cation exchange column provided purified hydrogen[18F]fluoride, which was subsequently trapped on a quaternary 4-aminopyridinium resin and used for heterogeneous nucleophilic radiofluorination of 1,3,4,6-tetraacetyl-beta-mannopyranose-2-triflate in 70% yield. The purified [18F]fluoride was also used for solution phase nucleophilic labeling of ethyl [18F]4-fluorobenzoate following addition of K2 CO3/Kryptofix and DMSO. This approach provides a simplified way to ensure high reactivity in [18F]fluoride ion from cyclotron targets. It also may be used to salvage active [18F]fluoride ion from insoluble complexes and radiofluorination reaction residues.
通过与纯双三甲基硅基硫酸酯简单加热，可从各种含有无反应性[18F]氟化物的干燥载体中快速释放出无载体添加的三甲基硅基[18F]氟化物（TMS[18F]F）。这些载体包括磷酸钙、阴离子交换树脂、氧化铝、硼硅酸盐和多孔碳珠，通过水溶液的吸附或蒸发将[18F]氟化物施加于其上。TMS[18F]F基本上不含夹带的水分或过量的硅烷化剂而逸出，并被0.1%苄基三甲基氢氧化铵的无水甲醇溶液有效吸收并迅速裂解为游离的[18F]氟离子。该溶液通过强阳离子交换柱可得到纯化的氟化氢[18F]，随后将其捕获在季铵化的4-氨基吡啶树脂上，并用于1,3,4,6-四乙酰基-β-吡喃甘露糖-2-三氟甲磺酸酯的非均相亲核放射性氟化反应，产率为70%。在加入碳酸钾/穴醚和二甲基亚砜后，纯化的[18F]氟化物还用于4-氟苯甲酸乙酯的溶液相亲核标记。这种方法提供了一种简化的方式，以确保回旋加速器靶材产生的[18F]氟离子具有高反应活性。它还可用于从不溶性络合物和放射性氟化反应残渣中回收活性[18F]氟离子。
