Improvement of Silica Gel Column Packing Materials - pursuit of Functionality -

首先，制备了3种高效液相色谱柱填料(3-吗啉丙基)-[3-(1-哌氨基)丙基]-和(3-哌啶丙基)硅基硅胶，并考察了它们对水溶性维生素等水溶性有机物的分离能力。样品溶液中的6种维生素(抗坏血酸、烟酸、硫胺素、盐酸吡哆醇、醋酸羟钴胺和黄素腺嘌呤二核苷酸)在不到12min内即可完全分离，色谱柱为吗丙基硅胶(MPS)柱，以磷酸盐缓冲液为洗脱液。MPS色谱柱还成功地用于调味品和三磷酸腺苷(AMP、ADP和ATP)混合物中三种核苷酸物质(5‘-肌苷酸、5’-鸟氨酸和5‘-黄烷酸)的测定。然后，通过3-氨丙基硅胶与相应的酸性氯化物反应，制备了新的萘甲酰基和邻氨基丙基硅基硅胶，发现它们适合于上述核酸相关化合物的分离。这一结果现在正被应用于ATPase活性的测量。成功申请了MPS及相关凝胶的制备和性能专利。

To begin with, three types of high-performance liquid chromatographic column packing materials ((3-morpholinopropyl)-[3-(1-pirazynyl) propyl]-, and (3-piperidinopropyl) silyl silica gels) were prepared and examined for their ability to separate water-soluble organic compounds such as water-soluble vitamins. Six vitamins (ascorbic acid, nicotinic acid, thiamine hydrochloride, pyridoxine hydrochloride, hydroxocobalamin acetate, and flavin adenine dinucleotide) in sample solutions could be completely separated within less than 12 min by UV detection on a column packed with morpholinopropylsilyl silica gel (MPS) by using a phosphate buffer as an eluent. The MPS column was successfully used also for the determination of three nucleotidic substances (5'-inosinic acid, 5'-guanylic acid and 5'-xanthylic acid) in seasonings and the mixture of adenosine morno-, di- and triphosphates (AMP, ADP and ATP). Next, naphthoyl- and anthroylaminopropylsilyl silica gels were newly prepared by the reaction of 3-aminopropylsilyl silica gel with the corresponding acid chlorides and found to be suitable for the separation of the nucleic acid related compounds above mentioned including the related nucleosides. The results are now being applied to the measurement of an ATPase activity. Patents on the preparation and the performance of MPS and the related gels was successfully applied.