夏至乔车菊内酯的NMR研究

以一维核磁共振谱（Ｈ－ＮＭＲ，＾１３Ｃ－ＮＭＲ，ＤＥＰＴ）和二维核磁共振谱（Ｈ－ＨＣＯＳＹ，ＨＭＱＣ，ＨＭＢＣ，ＮＯＥＳＹ）为主要手段研究了从祁州漏芦地上部分上分离得到的夏至科车菊内酯（Ｉ），确认了其结构，圆满地归属了其Ｈ－ＮＭＲ和＾１３Ｃ－ＮＭＲ信号，并对其立体化学进行了研究。     

微生物来源的胆固醇生物合成酶抑制研究：Ⅲ.抗生素SIPI—891…

ＳＩＰＩ－８９１５经ＳＩＰＩ－１８６菌生物转化得１种转化产物，其结构经紫外，质谱（ＥＩ，ＨＲＭＳ），＾１Ｈ－ＮＭＲ，＾１Ｈ－＾１Ｈ ＣＯＳＹ，＾１３Ｃ－ＮＭＲ（ＤＥＰＴ），＾１３Ｃ－＾１Ｈ ＣＯＳＹ等光谱分析，证实该转化产物的结构与ｐｒａｖａｓｔａｔｉｎ相同。     

微生物来源的胆固醇生物合成酶抑制剂研究Ⅲ．抗生素SIPI─8915转化产物的研究

ＳＩＰＩ－８９１５（ｃｏｍｐａｃｔｉｎ）经ＳＩＰＩ－１８６菌株生物转化得１种转化产物，其结构经紫外、质谱（ＥＩ，ＨＲＭＳ）、１Ｈ－ＮＭＲ、１Ｈ－１ＨＣＯＳＹ、１３Ｃ－ＮＭＲ（ＤＥＰＴ）、１３Ｃ－１ＨＣＯＳＹ等光谱分析，证实该转化产物的结构与ｐｒａｖａｓｔａｔｉｎ相同     

微生物来源的胆固醇生物合成酶抑制剂研究Ⅱ．抗生素SIPI－8915的研究

菌株ＳＩＰＩ－８９１５经麦芽糖—蛋白胨培养基培养，发酵液于酸性条件下经乙酸乙酯萃取，硅胶柱层分离纯化、结晶和重结晶得一白色针晶，熔点１５０～１５２℃。分子式Ｃ２３Ｈ３４Ｏ５。其甲醇溶液在２３０，２３７、２４６ｎｍ处呈吸收高峰。高分辨质谱显示Ｍ＋（ｍ／ｚ）３９０．２３９２。经１Ｈ．ＮＭＲ、１Ｈ－ＨＣＯＳＹ谱以及１３Ｃ－ＮＭＲ（ＤＥＰＴ）和１３Ｃ－１ＨＣＯＳＹ谱等数据，证实ＳＩＰＩ－８９１５产生的物质与Ｃｏｍｐａｃｔｉｎ为同物。     

微生物来源的胆固醇生物合成酶抑制剂研究：Ⅱ.抗生素SIPI—891…

菌株ＳＩＰＩ－８９１５经麦芽糖－蛋白胨培养基培养，发酵液于酸性条件下经乙酸酯萃取，硅胶柱层分离纯化、结晶和重结晶得一白色针晶，熔点１５０～１５２℃。分子式Ｃ２３Ｈ３４Ｏ５。其甲醇溶液在２３０、２３７、２４６ｎｍ处呈吸收高峰。高分辨质谱显示Ｍ＾＋（ｍ／ｚ）３９０．２３９２。经＾１Ｈ－ＮＭＲ、＾１ｈ－＾１ＨＣＯＳＹ谱以及＾１３Ｃ－ＮＭＲ（ＤＥＰＴ）和＾１３Ｃ－＾１Ｈ ＣＯＳＹ谱等数据，证实ＳＩＰＩ－８     

半合成新抗生素——抗生素89—07的合成和结构测定

以庆大霉素Ｃ１８为母核，采用保护合成法，将其二脱氧链霉胺（２－ＤＯＳ）１－Ｎ位上的１个氢原子用１个乙基取代，得到半合成新抗生素８９－０７，经ＩＲ、ＵＶ、ＭＳ、＾１Ｈ－ＮＭＲ、＾１３Ｃ－ＮＭＲ、ＤＥＰＴ、＾１Ｈ－＾１Ｈ－ＣＯＳＹ、＾１３Ｃ－＾１Ｈ－ＣＯＳＹ等测试证实抗生素和中间体的分别与１－Ｎ－乙基ＣＭＣ１ａ和３，２，６，－三－Ｎ－乙酰基ＧＭＣ１ａ（Ｐ１），３，２，６，－三－乙酰基１－Ｎ－乙基ＧＭＣ     

Na^＋—K^＋／ATP酶抑制剂的研究Ⅲ.SIPI—90—653菌株中小组份的研究

从ＳＩＰＩ－９０－６５３菌株中分离得到２个小组份，经ＵＶ、ＥＩ、ＦＡＢ、１Ｈ－ＮＭＲ、１３Ｃ－ＮＭＲ、１Ｈ－１ＨＣＯＳＹ、１３Ｃ－１ＨＣＯＳＹ及化学分析证实其结构分别为芦他霉素和ｖｕｌｇａｍｙｃｉｎ。两个化合物有较强的抗虫活性。     

菊淀粉型低聚糖类的^1HNMR及^13CNMR研究

本文应用二量子滤波＾１Ｈ－＾１Ｈ ＣＯＳＹ，＾１Ｈ－＾１３Ｃ ＣＯＳＹ及远程＾１Ｈ－＾１３Ｃ ＣＯＳＹ等二维核磁共振技术，结合与类似物的化学位移值比较，分析归属了菊淀粉型低聚糖（１￣４）的＾ＨＮＭＲ及＾１３ＣＮＭＲ信号。     

SHISEN-1,a novel phenazine antibiotic from Streptoplanospora viridis Ⅱ.Physico-chemical properties and structure elucidation

在筛选ＭＲＳＡ抑制剂的过程中，从稀有放线菌Ｓｔｒｅｐｔｏｐｌａｎｏｓｐｏｒａｖｉｒｉｄｉｓ的次级代谢产物中，得到活性化合物ＳＨＩＳＥＮ－１，该化合物为黄色粉末，于２５４及３６４ｎｍ处有最大的紫外吸收峰，经理化性质和光谱分析（ＩＲ、ＵＶ、ＦＡＢ－ＭＳ、ＥＩ－ＭＳ、１Ｈ－ＮＭＲ、１３Ｃ－ＮＭＲ、ＤＥＰＴ、ＨＭＱＣ、ＨＭＢＣ、１Ｈ－１ＨＣＯＳＹ），得知它为一个新的酚嗪类抗生素，分子式为Ｃ２２Ｈ１６Ｎ２Ｏ４。     

半合成新抗生素──抗生素89－07的合成和结构测定

以庆大霉素Ｃ１ａ为母核，采用保护合成法，将其二脱氧链霉胺（２－ＤＯＳ）１－Ｎ位上的１个氢原子用１个乙基取代，得到半合成新抗生素８９－０７。经ＩＲ、ＵＶ、ＭＳ、１Ｈ－ＮＭＲ、１３Ｃ－ＮＭＲ、ＤＥＰＴ、１Ｈ－１Ｈ－ＣＯＳＹ、１３Ｃ－１Ｈ－ＣＯＳＹ等测试证实该抗生素和中间体的结构分别与１－Ｎ－乙基ＧＭＣ１ａ和３．２’，６’－三－Ｎ－乙酰基ＧＭＣ１ａ（Ｐ１）、３，２’，６’－三－Ｎ－乙酰基－１－Ｎ－乙基ＧＭＣ１ａ（Ｐ２）相一致。     

Neue Guajanolide aus Centaurea imperialis

The aerial parts of CENTAUREA IMPERIALIS afforded three new guaianolides, 3-desoxysolstitialin A and two derivatives of centaurepensin.     

罗汉果皂苷Ⅳa碳氢NMR信号的归属

目的　研究传统中药罗汉果的皂苷类化学成分罗汉果皂苷IVa的结构 ,总结其结构的NMR特点。方法　采用常法提取、分离、纯化罗汉果皂苷IVa ,应用NMR方法 ( 1 HNMR、1 3CNMR、DEPT、1 H 1 HCOSY、HSQC、HMBC和NOESY)和计算机分子模拟研究其结构。结果　对罗汉果皂苷IVa的1 H和1 3C信号进行了归属 ,并为该类型化合物的结构确定提供了波谱学依据。结论　包括1 H 1 HCOSY、HSQC、HMBC、NOESY的一维和二维核磁共振波谱技术是对结构进行无创伤性分析的有力工具。NMR方法确定的结构与计算机分子模拟的最优构象一致。     

Characterisation of the 1H and 13C NMR spectra of N-acetylaspartylglutamate and its detection in urine from patients with Canavan disease

1H and 13C NMR spectra of N-acetylaspartylglutamate (NAAG) have been recorded and interpreted. The values of the 1H chemical shifts and 1H-(1)H coupling constants at different pH were obtained by iterative computer fitting of 1-D 1H NMR spectra. This provided information on the solution conformation of the investigated molecule. Proton-decoupled high resolution 13C NMR spectra of NAAG have been measured in a series of dilute water solution of various acidity. These data have provided a basis for unequivocal determination of the presence of NAAG in the urine sample of a patient suffering from Canavan disease. NMR spectroscopy provides a possibility of detecting NAAG in body fluids.     

连翘中的新化合物

从连翘果实中分离得到一个新化合物,用ＩＲ、ＭＳ、１Ｈ ＮＭＲ、１３Ｃ ＮＭＲ、１３Ｃ １ＨＣＯＳＹ及１Ｈ １ＨＣＯＳＹ光谱进行测定,鉴定其结构为８ 对羟基苯乙酰连翘醇酯,命名为连翘醇酯（ｒｅｎｇｙｏｌｅｓｔｅｒ）．     

维库溴铵的核磁共振谱研究

目的选择适合的实验条件,用核磁共振方法鉴定维库溴铵的结构。方法应用1H1、3C、DEPT、COSY、HSQC、HMBC等核磁共振技术,对维库溴铵的1H-NMR和13C-NMR谱进行测定,研究了使用不同温度、不同溶剂对13C-NMR谱信号的影响。结果对维库溴铵的1H-NMR和13C-NMR谱的信号进行了全归属。结论通过二维核磁共振技术确证了维库溴铵的结构。     

醌霉素A,C的^1H,^13C核磁共振谱归属的修正

以“精原细胞”法为筛选模型，从云南土壤的一株链霉菌１７２５０的菌丝和发酵液中分离得到２个抗肿瘤抗生素１７２５０－Ｚ１和１７２５０－Ｚ２。经对其理化性质和光谱数据的分析，确证１７２５０－Ｚ１为醌霉素Ｃ，１７２５０－Ｚ２为醌霉素Ａ，并对醌霉素Ａ、Ｃ的１３Ｃ核磁共振谱的个别归属进行了补充和修正     

NMR and pattern recognition studies on liver extracts and intact livers from rats treated with alpha-naphthylisothiocyanate

The metabolite profiles from livers of toxin-treated rats were investigated using high resolution 1H NMR spectroscopy of aqueous (acetonitrile/water), lipidic (chloroform/methanol) extracts and magic angle spinning (MAS)-NMR spectroscopy of intact tissue. Rats were treated with the model cholestatic hepatotoxin, alpha-naphthylisothiocyanate (ANIT, 150 mg/kg) and NMR spectra of liver were analysed using principal components analysis (PCA) to extract novel toxicity biomarker information. 1H NMR spectra of control aqueous extracts showed signals from a range of organic acids and bases, amino acids, sugars, and glycogen. Chloroform/methanol extracts showed signals from a range of saturated and unsaturated triglycerides, phospholipids and cholesterol. The MAS 1H NMR spectra of livers showed a composite of signals found in both aqueous and lipophilic extracts. Following ANIT treatment, 1H NMR-PCA of aqueous extracts indicated a progressive reduction in glucose and glycogen, together with increases in bile acid, choline, and phosphocholine signals. 1H NMR-PCA of chloroform/methanol extracts showed elevated triglyceride levels. The 1H MAS-NMR-PCA analysis allowed direct detection of all of the ANIT-induced tissue perturbations revealed by 1H NMR of extracts, enabling metabolic characterisation of the lesion, which included steatosis, bile duct obstruction and altered glucose/glycogen metabolism. MAS-NMR spectroscopy requires minimal sample preparation and, unlike 1H NMR spectroscopy of tissue extracts, does not discriminate metabolites based on their solubility in a particular solvent and so this is a particularly useful exploratory tool in biochemical toxicology.     

Further structural analysis of rat liver microsomal metabolites of 2-methylnaphthalene

The oxidative metabolites of 2-methylnaphthalene (2-MN) were extracted from rat liver microsome suspensions. One monohydroxylated and three isomeric dihydrodiol metabolites of 2-MN were isolated and purified by HPLC. The metabolites were characterized by GC-MS together with 1H Fourier transform (1HFT) NMR. The identification of a 2-MN-monohydroxylated product as 2-hydroxymethylnaphthalene was confirmed by comparison of its HPLC retention time and NMR spectrum with that of a synthetic standard. The three isomeric dihydrodiol metabolites had different HPLC retention times, fragmentation patterns, ultraviolet, and 1H NMR spectra. GC-MS of the silylated dihydrodiols revealed the consistent presence of an ion peak at m/z 320, indicative of a disilylated dihydrodiol. Analysis of the 1H FT NMR spectra revealed the metabolites to be the 3,4-dihydrodiol, 5,6-dihydrodiol, and 7,8-dihydrodiol of 2-methylnaphthalene.     

微生物来源白细胞介素1受体拮抗剂的研究Ⅱ．链霉菌660代谢产物的化学研究

从活性链霉菌660的发酵液中,经溶媒萃取,硅胶制备薄层层析及ODS等分离得到化合物4和化合物6,通过理化性质研究和UV、IR、MS、^1H-NMR、^13C-NMR、DEPT、^1H-^1H COSY、^1H-^13C COSY、HMBC等光谱分析确定化合物4为N－乙酰基酪胺（N-acetyltyramine),化合物6为3－丙基－7－甲基－六氢吡咯[1,2-a]并吡嗪－1,4－二酮（3－propyl-7-methyl-hexahydropyrrolo[1,2-a]pyrazine-1,4-dione)。并对其活性进行研究。     

免疫抑制剂SIIA9268A的研究.Ⅱ.结构鉴定

在筛选免疫抑制剂的过程中，得到具有免疫抑制剂活性的化合物ＳＩＩＡ９２６８Ａ，经理化性质和光谱分析（ＩＲ、ＵＶ、１Ｈ－ＮＭＲ、１３Ｃ－ＮＭＲ、ＡＰＴ、１Ｈ－１ＨＣＯＳＹＮＭＲ、１３Ｃ－１ＨＣＯＳＹＮＭＲ、ＥＩ－ＭＳ），得知该化合物属于新型大环内酯类，与ｒａｐａｍｙｃｉｎ同质。