核壳复合材料NH2-MIL-125@TPA-COF用于高效液相色谱分离位置异构体

该文通过在金属－有机骨架材料（MOF）NH2－MIL－125表面原位生长共价有机骨架材料（COF）TPA－COF,制备了核壳复合材料（MOF@COF）NH2－MIL－125@TPA－COF,采用X-射线粉末衍射（PXRD）、红外光谱（FTIR）和扫描电镜（SEM）等手段对该复合材料进行表征,并将其作为固定相成功制备了NH2－MIL－125@TPA－COF色谱填充柱（25 cm long × 2.1 mm i.d.）。在正相（正己烷－异丙醇（9∶1））、反相（甲醇－水（9∶1））高效液相色谱（HPLC）条件下,考察了该柱对一系列位置异构体的分离性能。结果表明,该柱在较低的背景压力（60～100 kPa）下对9种位置异构体（溴硝基苯、硝基苯胺、氯苯酚、二硝基苯、碘苯胺、溴苯胺、苯二胺、甲苯胺和氯苯胺）表现出较好的分离能力,其中溴硝基苯、硝基苯胺和二硝基苯能达到基线分离,且最大分离度（Rs）为9.71。在反相HPLC条件下,邻-溴硝基苯、间-硝基苯胺和邻-氯苯酚的柱效分别为18 424、19 053、12 954 plates·m－1。以溴硝基苯为分析物,在正相HPLC条件下,考察了该柱的重现性和稳定性。该柱通过5次重复进样（第50次、第100次、第150次、第200次、第250次）,溴硝基苯保留时间和峰面积的相对标准偏差（RSD）分别为0.29%和0.89%,表明所制备的色谱柱具有较好的重现性和稳定性。核壳复合材料NH2－MIL－125@TPA－COF作为一种新型的HPLC固定相用于位置异构体分离具有良好的应用前景。     

用于放射性卤代药物合成的高速无载体固相标记法

本文研究了一种适合于卤素标记化合物的高分子氧化剂的合成及其性能, 研究了适合于某些卤代放射性药物合成的高速、无载体产物的固相标记法和固相反应。 用于肿瘤探针的药物带电诺丹明和肾功能显像剂胆固醇在固定化后, 将这两种药物进行固相法碘标记并对产物进行了鉴定, 得到了放射化学纯度大于95%, 放射性回收率高于96%的标记化合物, 实现了5分钟内完成放射性标记药物无需分离就可得到极高放化纯产物的高速标记法。本文还对其它能生成有机汞化合物的固相标记法进行了讨论。     

荧光标记反相高效液相色谱法测定蚕蛹体内痕量前列腺素的组成

利用荧光标记法在反相高效液相色谱上对蚕蛹体内痕量前列腺素的分离、鉴定进行了研究，并对不同蛹期蛹体中前列腺素的组成和分 进行了测定。７种前列腺素在所选择的实验下都能得到很好的分离，色谱柱为Ｃ８－键合柱；     

烷基磷酸酯盐分离技术的研究及波谱表征

通过对常压硅胶柱色谱分离条件的研究,实现了对工业合成烷基磷酸酯盐的分离。对两种分离产物进行IR、^1H-NMR、^31P-NMR和原子发射光谱分析,确定出其结构,验证了用常压硅胶柱色谱分离烷基磷酸单酯和双酯盐的可行性,并对硅胶柱色谱分离烷基磷酸酯盐进行了初步探讨。     

制备液相色谱法分离纯化碘帕醇

基于制备液相色谱法,开发与优化了碘帕醇的分离纯化工艺,制备得到高纯度碘帕醇样品。实验首先在分析水平发展碘帕醇的反相分离方法,考察了两种不同键合量的反相C18固定相、柱温和上样量对碘帕醇的保留、分离度和峰形等的影响。结果表明,碘帕醇在键合量为13.7%的反相C18-1分析柱（250 mm×4.6 mm,10 μm）上保留较好,且可与杂质有效分离;柱温升高,碘帕醇保留变弱,和杂质之间的分离度降低,最终选用20~25℃作为分离纯化的温度;上样量增加,碘帕醇出峰时间提前,不利于前杂的去除。在制备水平上,以水和甲醇为洗脱剂,在20℃条件下使用装填C18-1固定相的制备柱（270 mm×50 mm,10 μm）对碘帕醇进行分离纯化,制备的碘帕醇样品的色谱纯度可达98.97%,回收率为93.44%,各项有关物质均符合限量规定。该方法可以在保证高回收率的条件下有效降低杂质水平,为碘帕醇分离纯化生产工艺的开发提供新方法。     

五加成C60氮杂丙酸衍生物的合成

Ｃ６０和β－叠氮丙酸在氰苯中回流，产物经柱色谱分离、ＦＤ－ＭＳ证实为五加成Ｃ６０衍生物，＾１３Ｃ ＮＭＲ、ＦＴ－ＩＲ和ＵＶ光谱对产物结构进行了表征。     

氨基酸对映体的芯片毛细管电泳拆分

在毛细管电泳芯片上，采用CD－SDS－MEKC模式，对FITC标记的3种氨基酸对映体进行了手性分离研究。CD种类、浓度、SDS浓度以及各种添加剂对氨基酸对映体拆分有影响，认定γ－CD对FITC标记的氨基酸手性识别能力较强，在含有5mmol/L γ-CD和30mmol/L SDSr 10mmol/L,pH10.0的硼砂缓冲溶液中，3种氨基酸对映体得到了较好的分离。     

反相离子对高效液相色谱分析~(125)Ⅰ-甲状腺激素

甲状腺激素3,5,3′,5′-四碘甲腺原氨酸(T_4),3,5,3′-三碘甲腺原氨酸(T_3)及3,3′,5′-三碘甲腺原氨酸(γT_3)为甲状腺碘代氨基酸。它们的~(125)I标记化合物分别为T_3、T_4、γT_3的碘-125标记药盒的主要组成。这些药盒分别用于测定血清中T_3,T_4,γT_3的浓度,以判断甲状腺对组织的成熟、生长、代谢活动和功能,诊断甲状腺疾病。     

脂肪醇在OV-1和Superox 0.6柱上的色谱行为

Ｓｕｐｅｒｏｘ系列固定相是性能优良的氢键型固定相，适用地脂肪醇分析，非级性固定相ＯＶ－１柱，经减活处理后亦适宜醇类异构体分离，考察了Ｃ１－Ｃ２异构醇的３６个组分在分离效能。ＯＶ－１柱和Ｓｕｐｅｒｏｘ０．６柱上的保留行为，柱效和极限温度，结果表明，两种柱对醇都有很好的分离效能。ＯＶ－１柱柱效及柱温极限高，除了戊醇－３和戊醇－２是重叠峰外，其余组分间有一定分离度，其分离顺序基本上是根据组分的沸点，包括     

混合烷基开管电色谱柱的制备和评价

利用溶胶－凝胶（Sol-Gel）技术制备了混合烷基开管毛细管电色谱柱（C8－C13OT－CEC），并考察了其电渗流行为和电色谱性能。研究了流动相中甲醇含量对芳香族中性化合物保留的影响。发现C8－C18OT－CEC柱体现反相分配机理。5种芳香族化合物和4种苯同系物在C8－C13OT－CEC柱上分离良好，同时还考察了分离电压和柱内径对柱效的影响，结果表明高的电压和较小的柱内径能提高柱效。     

Radioiodination of C60 Derivative C60(OH)xOy

In this paper water-soluble fullerene derivative C₆₀(OH)_xO_y was radioiodinated with the iodogen method. The labeling yield was determined by radio-TLC. The effects of pH value, reaction time, temperature and amount of the iodogen on the labeling yield were studied. The labeled product was purified by Sephadex G-25 column chromatography and then the stability of ¹²⁵I-C₆₀(OH)_xO_y was examined . The results showed that the radiochemical purity of ¹²⁵I-C₆₀(OH)_xO_y solution with benzylalcohol remained 82.7% after 43 hours.     

Preparation of 125I-Lanreotide and its biodistribution in murine model of melanoma

Lanreotide, a somatostatin analogue, was radioiodinated with ¹²⁵I to explore the possibility of using ¹²³I labeled lanreotide as a diagnostic radiopharmaceutical for tumors overexpressing somatostatin (SST) receptors. Radioiodination was carried out with ¹²⁵I using chloramine T as the oxidant. The labeling yield was >90%. Characterization of ¹²⁵I-Lanreotide was carried out by paper electrophoresis as well as HPLC. ¹²⁵I-Lanreotide was purified by chromatography using a C18 Sep-Pak column. Radiochemical purity of the purified ¹²⁵I-Lanreotide thus obtained was >99%. Significant tumor uptake of ¹²⁵I-Lanreotide was observed in C57BL/6 mice bearing melanoma.     

羧甲基牛膝多糖的制备、结构及生物活性研究

在NaOH水溶液中,以ClCH_2COOH为羧甲基化试剂,对牛膝多糖(AbPS)进行了羧 甲基化,粗产物经DEAE-Cellulose及Sephadex G-25两次柱层析纯化,得到羧甲基 牛膝多糖(CM-AbPS)纯品,经高效液相法（HPLC）及毛细管电泳法（CE）检测表明 具有较好的均一性,并通过样品甲基化和GC-MS分析,对羧甲基牛膝多糖链中羧甲 基的分布进行了研究,结果表明羧甲基牛膝多糖中羧甲基主要取代的糖链中呋喃果 糖的4-位上。该产物具有抗肿瘤活性。     

Radiolabeling of EGCG with 125I and its biodistribution in mice

The aim of the present study was to label EGCG with ¹²⁵I and to determine its radiopharmaceutical potential in mice. EGCG was labeled with ¹²⁵I using the iodogen method. The labeling yield and the radiochemical purity of ¹²⁵I–EGCG were determined by radio thin-layer chromatography (RTLC). The Labeling yield was approximately 89.4 %. The radiochemical purity was approximately 96.4 %. The biodistribution studies of the labeled compound (specific activity; 0.47 TBq/μg) were performed in male Kunming mice. The uptakes of ¹²⁵I–EGCG in some organs were determined at different time after injection to the mice. The radioactivity in each organ was counted and the percentage of injected activity per gram of tissue weight (%ID/g) for each organ and blood was calculated. Incorporation of radioactivity in the various tissue/organ was confirmed by microautoradiography. ¹²⁵I–EGCG uptake in the stomach and salivary gland was higher than other organ/tissue. The black silver grains was concentrated in the nucleus, cytoplasm, intercellular substance and capillaries of that various organs, and its unevenly distributed. Thus, ¹²⁵I–EGCG may be radiopharmaceutical for the imaging of the stomach and salivary gland.     

Application of preparative reversed-phase high-performance liquid chromatography to the isolation of insulin-like growth factor II from human serum

Substantially purified insulin-like growth factor II (IGF-II) was prepared from human serum. Initial enrichment using ion-exchange chromatography on DEAE Sephadex A50, followed by gel permeation chromatography on Sephadex G-75 in 1% formic acid produced material suitable for application to a preparative reversed-phase high-performance liquid chromatographic (HPLC) column containing LiChroprep RP-18. The latter step gave about 90-fold purification with a recovery of about 70% IGF-II bio-activity. Finally, a small reversed-phase HPLC column achieved a 17-fold purification with similar yield of activity. Overall, the four steps gave IGF-II of about 90% purity in yield of 12%.     

肌钙蛋白Ⅰ提取纯化新方法的研究

兔骨骼肌匀浆液经离心后,依次经DEAE－SephadexA25,SephadexG75及ButylSepharoseF.F柱层析,得到了兔骨骼肌肌钙蛋白C(sTnC)纯品.将其与Sepharose4B凝胶偶联,制成sTnC亲和层析凝胶.人心肌或骨骼肌经匀浆、离心后上sTnC亲和层析柱,一步分离可获得人心肌肌钙蛋白Ⅰ(cTnI)或人骨骼肌肌钙蛋白Ⅰ(sTnI)纯品.HPLC分析出现单一峰.SDS－PAGE分析得到一条电泳带,其分子量分别为25000及21000.用20gsTnC亲和凝胶处理40g人心肌时,相当于每100g心肌可得到82.6mgcTnI.     

Optimization of the separation of the Rp and Sp diastereomers of phosphate-methylated DNA and RNA dinucleotides.

The separation by reversed-phase high-performance liquid chromatography of Rp and Sp diastereomers of phosphate-methylated DNA and RNA dinucleotides was studied with respect to pH, organic modifier type and concentration and reversed-phase packing material. Drylab G was used to deduce optimum conditions. On the basis of the observed discrepancies between the computer predictions and experimental results, the gradient operation procedure with volatile buffers was improved. By repetitive chromatography on a 250 x 22 mm I.D. reversed-phase column, fourteen diastereomeric pairs were obtained in at least 97% purity and 60% yield, in amounts of 10-100 mg.     

Preparative isolation of angiotensin-converting enzyme from human lung.

Angiotensin-converting enzyme from human lung was purified to apparent homogeneity using a five-step purification procedure consisting of ammonium sulfate precipitation, ion-exchange chromatography on DEAE Sephadex A-50, gel permeation on Sephadex G-200, chromatofocusing on a polybuffer exchange (PBE 94) column and high-performance liquid chromatographic gel permeation on a Bio-Sil TSK-250 column. This procedure gave an approximately 700-fold purification with a 20% yield compared to a 550-fold purification and a 1% yield with an affinity chromatography-based procedure. The 20-fold greater yield of the five-step procedure offers a major advantage for preparative use in the structural characterization of angiotensin-converting enzyme.     

Radioiodination and biodistribution of NBNPQD (2-benzyl-1-oxo-1,2-dihydropyrido[4,3-b]quinoxaline 5,10-dioxide) in tumor bearing mice

NBNPQD (2-benzyl-1-oxo-1,2-dihydropyrido[4,3-b]quinoxaline 5,10-dioxide) is a new synthesized quinoxaline derivative. It could be labeled with auger emitter ¹²⁵I successfully with yield about 90 %. The labeled product was evaluated by electrophoresis and thin layer chromatography. Factors affected labeling yield were studied. ¹²⁵I-NBNPQD was stable up to 48 h post labeling. Biodistribution study of ¹²⁵I-NBPQD in normal and tumor bearing mice was also conducted. The biodistribution data revealed that ¹²⁵I-NBNPQD diffused rapidly to tumor sites in both ascites and solid tumor bearing mice. ¹²⁵I-NBNPQD was declined rapidly from most of organs but slowly from tumor sites. In vitro radiotoxicity of ¹²⁵I-NBNPQD increased with the increase of its radioactivity. This study encourages the possible use of ¹²⁵I-NBNPQD in tumor imaging and treatment. It also encourages further studies on the chemotherapeutic activity of NBNPQD hoping to get a new potent antitumor agent.     

CHROMATOGRAPHIC SEPERATION AND PURIFICATION OF HUMAN CHORIONIC GONADOTROPIN

Separation and purification of human chorionic gonadotropion(HCG) in the urine sample of early pregnant women by D3520 resin adsorption chromatography is reported.The crude product obtained by DEAE-Cellulose 23 and DEAE-Sephadex A50 column chromatography showed a high activity of HCG. Further purification of the sample by gel filtration chromatography on a Sephadex G75 column gives a final preparation of 6000-6500 IU/mg.The preparation meets the requirements of the pyrogn test in Chinese Law of Pharmacopeia.