The effect of structure modification of chondroitin sulfate C on its enantioselectivity to several representative basic drugs in capillary electrophoresis was investigated. Chemical desulfation showed no remarkable decrease in selectivity, whereas depolymerization with chondroitinase ABC resulted in complete loss of selectivity. Comparison with chondroitin sulfate A indicated considerable decrease in selectivity with this isomer. The great retention of enantioselectivity in the desulfated derivative suggests that the selectivity comes from the difference of the magnitude of an interaction in the multipoint mechanism between a part of the drug molecule and a functional group in chondroitin sulfate C other than the sulfate group. The sulfate group is not considered to play a major role for chiral separation. The complete loss of selectivity by depolymerization is consistent with a general tendency of lower selectivity in smaller saccharides, and the priority of chondroitin sulfate C to chondroitin sulfate A suggests the importance of the hydroxyl group at C in the galactosamine 4 residue. During the course of this work we observed heavy tailing of the peaks of basic drugs in some batches of uncoated fused-silica capillaries under acidic conditions and solved this problem by oubly coating capillaries with Polybrene followed by chondroitin sulfate C. On the other hand, we demonstrated the usefulness of a special technique which uses a short, wider bore PTFE tube-attached capillary for the study of the effect of depolymerization, in order to minimize sample amount.

目的 将多聚乙酰神经氨糖酸用作分离双氢吡啶类药物对映体的毛细管电泳手性选择剂，建立新药马来酸氨氯地平对映体的拆分方法。方法 考察了手性选择剂浓度、运行缓冲液pH值、毛细管温度、工作电压和多糖分子量等因素对手性分离的影响。结果 马来酸氨氯地平两对映体得到了完全分离，分离度为2.20，并研究了多聚乙酰神经氨糖酸对马来酸氨氯地平的手性识别机理。结论 本法操作简便，可用于该新药对映体的分离分析。

本文建立了对羧基偶氮羧分光光度法测定微量钙的方法，研究了试剂与钙的B型显色反应的条件、影响因素及形成机理。在柠檬酸介质中，钙与该试剂只发生灵敏的13型显色反应，络合物最大吸收波长为718nm（△λ=157nm），表观摩尔吸光系数ε=1.51×105L·mor-1·cm-1，反应完全后，吸光度可保持4h不变。方法用于直接测定复方氯化钠注射液中的钙，回收率在99.20%～103.5%之间，结果与标准方法一致，相对标准偏差小于1.5%。

基于间抓偶氮安替比林可与钙在碱性介质中形成灵敏的兰色络合物这一显色反应，本文在自行组装的带微型计算机的流动注射分析仪上，以分光光度计作检测器，建立了测定微量钙的流动注射分光光度法。最佳显色反应条件：0.08mol/L NaOH-0.012%显色剂一三乙醇胺溶液，测定波长为630nm。以三乙醇胺为掩蔽剂，方法选择性较高。钙的线性范围为1.0～15.0μg/ml。检测限0.5μg/ml。进样频率可达55样次/h。方法可不经分离直接测定药物和水中的钙，回收率及情密度均良好

以阴离子聚合物聚丙烯酸为涂层材料，研制了一种新型的阴离子型毛细管电泳Polybrene/聚丙烯酸双涂层柱。此法不但操作方便，而且毛细管涂层重现性好，柱寿命超过100次电泳分析，经1mol/LHC1、0.1mol/LNaOH、CH3OH和CH3CN 等冲洗15min 后，涂层未发生变化，化学稳定性强。将该双涂层柱用于以新型多糖作手性选择剂的碱性药物手性拆分中，毛细管内壁对碱性药物的吸附作用大大降低，样品色谱峰对称性显著改善，手性分离的效果良好。