从国产紫胶树脂中分离鉴定壳脑酸

本文利用紫胶树脂碱水解后,其链状与环状组份性质的差别,首次从国产紫胶树脂中分离得到一种无色透明的立方晶体,经光谱证实为壳脑酸二甲酯。     

大孔交联聚苯乙烯吸附树脂的合成及其对叶绿素铜的吸附…

通过改变苯乙烯－二乙烯苯共聚物的交联度和使用不同结构的二乙烯苯，合成了树脂Ｉ－Ⅵ，在工业二乙烯苯共聚体系中加入少量丙烯酸甲酯合成了树脂Ⅶ；交联聚苯乙烯经Ｆｒｉｅｄｅｌ－Ｇｒａｆｔｓ酰化反应在其苯环上引入乙酰基制备树了树脂Ⅷ，用物理技术和化学方法表征了树脂的结构。树脂对叶绿素铜的吸附量不仅与其二乙烯苯含量胶有关，还与二乙烯基的位置（间－，对－）异构有关，树脂骨架极性的增加，不利于树脂对叶绿素铜的吸附     

二—（2,4,4—三甲基戊基）膦酸浸渍树脂分离Tb^3＋,Dy^3＋,Ho^3＋,Er^3＋的研究

研究了大孔风状树脂ＸＡＤ－Ｒ,ＸＡＤ－７,ＸＡＤ－１１８０对二－（２,４,４－三甲基戊基）膦酸浸渍树脂的吸附及制备方法,并对Ｃｙａｎｅｘ５７１浸渍树脂分离稀土的性能进行了研究,发现在盐酸介质中Ｃｙａｎｅｘ５７１／ＸＡＤ－７具有最强的萃取能力,树脂中的萃取剂含量在０．３５－０．４５ｇ．ｇ＾－１时,其萃取性能最好,将上述浸渍树装入色层柱对稀土元素进行了分离,且降低负载量和流速分离效果量好。     

果汁中天然色素紫胶红的UPLC/TUV定量检测及UPLC - MS/MS结构确证

建立了天然色素紫胶红各组分的UPLC/TUV定量检测及UPLC - MS/MS结构确证方法,并将所建立的分析方法应用于果汁中紫胶红色素的定性定量检测.通过Oasis(R) HLB小柱固相萃取技术净化、提取果汁饮料样品中的紫胶红色素.使用Waters Acquity UPLC BEH Shield RP C18(1.7 ...     

“国产弱酸、弱碱离子交换树脂工艺性能试验”科研成果通过鉴定

继1986年10月由武汉水利电力学院完成的“国产强酸、强碱离子交换树脂工艺性能试验”科研成果通过总评审之后,该院又相继完成了国产弱酸和弱碱离子交换树脂的工艺性能试验。1989年10月11日在南京由能源部电力规划管理局主持的会议上,通过了对该项科研成果的鉴定。这项研究首次提出了国产D116弱酸和D354系列弱碱树脂的完整工艺性能数据,曲线和公式。这两种树脂在典型条件下的工作交换容量和出水水质特性曲线如图1、2所     

蒙旦树脂化学组成的研究

采用阴离子交换色谱和硅胶－氧化铝柱色谱对云南寻甸蒙旦树脂（ＸＤＳＺ）、潦浒蒙旦树脂（ＬＨＳＺ）、昭通蒙旦树脂（ＺＴＳＺ）和吉林舒兰蒙旦树脂（ＳＬＳＺ）进行了族组分的分离。树脂游离酸，树脂结合酸，树脂烃和树脂醇在各树脂中的百分含量分别为ＸＤＳＺ１１．８６，８．７６，１２．３０，４５．９９；ＬＨＳＺ１５．８９，１３．９１，４．９０，４５．９９；ＳＬＳＺ２５．４６，８．０７，１７．４０，３６．２２；ＺＴ     

固体超强酸研究的最新进展

简要介绍了近年来固体超强酸的发展。目前研究较多的固体超强酸有负载硫酸超强酸、Ｃｓ２．５盐、ＡｌＣｌ３／ＰＳ－ＤＶＢ磺酸树脂体系和全氟磺酸树脂（Ｎａｆｉｏｎ－Ｈ－Ｈ ＰＥＩＥＰ）四种。文章主要阐述了这几种固体超强酸的制备方法及它们的性质比较。     

2—聚苯乙烯磺酰基乙醇树脂的合成及其在海因和脲固相合成中的应用

合成了一种新型的聚合物载体－－2－聚苯乙烯磺酰基乙醇，并研究其在固相有机合成中的应用。聚苯乙烯亚磺酸钠树脂（1）在相转移催化剂Bu4NI和助催化剂KI的作用下，与氯乙醇进行砜化反应，得到含羟基功能基的2－聚苯乙烯磺酰基乙醇树脂2。树脂2用Boc保护的氨基酸酯化，封闭树脂上未反应的羟基，用酸脱保护并用三乙胺中和，再与异（硫）氰酸苯酯反应生成聚合物支载的脲树脂6。树脂6用酸解脱得到了海因和硫代海因化合物。用碱处理树脂6时得到取代的脲和硫脲。优化了合成反应的全过程，探讨了树脂在酸性条件下的解脱方法。结果表明，2－聚苯乙烯磺酸基乙醇树脂易与羧工形成含酯键的连接桥，连接桥在强酸性和碱性条件下均可解脱得到产物。     

X—5树脂固相萃取血中四种局麻药的气相色谱分析

本文建立了以国产Ｘ－５树脂富集、净化血中局麻药的气相色谱测定法。本法洗脱回收率为７３．１％－８７．３％，变异系数为３．５－８．５％。     

交联聚苯乙烯固载聚乙二醇树脂（PEG）含量与活性的依赖关系研究

将具有不同ＰＥＧ含量的交联聚苯乙烯固载聚乙二醇树脂用于催化环已稀的二氯卡宾加成和乙酰苯胺的Ｎ－丁基化反应，发现树脂ＰＥＧ含量与催化剂活性之间存在的依赖关系。通过测定不同ＰＥＧ含量的树脂分别在水和甲苯中的溶胀系数，用树脂亲油－亲水性的变化规律，解释树脂活性与ＰＥＧ含量之间的依赖关系。     

Chemistry of lac resin—VII : Pure lac resin—3: Structure

It has been found that gas-liquid-chromatography of methyl esters of lac acids can be carried our after formylation of free OH groups. By this method, it has been found that pure lac resin is based on terpenic acids (essentially jalaric acid) and aleuritic acid in a 1:1 ratio and not in a 2:1 ratio as suspected earlier. This conclusion is clearly supported by a comparision of 220 MHz PMR spectra of pure lac resin derivatives with suitable reference samples. The PMR spectral data, taken along with the earlier results lead to the most plausible structure 11 for ‘pure lac resin’.     

Structural investigation of lac resin—II

The three fractions of lac rein viz., hard resin I, hard resin II and soft resin have been cleaved with hydriodic acid followed by deiodination. The products were separated into fatty acids and terpene acids. The former have been studied by GLC and data on the nature and distribution of the chain lengths and their relative amounts were thus obtained. Cleavage of the different fractions of the resin with hydrogen chloride followed by alkaline hydrolysis gave the total aleuritic acid quantitatively. Based on the above results, the possibility of the presence of alkali stable linkages in lac resin and the amount of aleuritic acid liberated only by acid cleavage have been determined.     

色谱-质谱联用技术在我国3种柚子组分鉴定及指纹图谱建立中的应用

利用色谱-质谱联用技术对我国主要的3个品种柚子果实的不同部位(外表皮、内表皮、内果皮、果肉、种子)的化学组分进行结构鉴定及种类和含量的差异性分析,结果表明,沙田柚、琯溪蜜柚、玉环柚果实5个部位共鉴定出68种不同化学组分物质,包括醇类19种、酯类15种、烯烃类9种、有机酸类8种、酮类7种、烷烃类4种、其他物质6种。其中3个品种柚子外表皮共有的化学组分有7种,含量最高的是柠檬烯(44.03%);内表皮共有的化学组分有6种,含量最高的是油酸酰胺(44.62%);内果皮共有的化学组分有10种,含量最高的是谷甾醇(30.75%);果肉共有的化学组分有11种,含量最高的是软脂酸(20.02%);种子中共有的化学组分有15种,含量最高的是亚油酸(45.83%)。化学组分差异性分析结果表明,沙田柚、琯溪蜜柚、玉环柚3种柚子的外表皮独有的化学组分分别有3种、6种、4种,内表皮分别有3种、4种、8种,内果皮分别有1种、4种、6种,果肉分别有4种、4种、2种,沙田柚、玉环柚种子独有的化学组分均为1种,并对化学组分进行聚类分析和相似度分析。研究结果说明不同品种柚子同一部位的化学组分种类和含量均存在相似性和差异性,特有物质较多,色谱指纹图谱特异性显著,这可为柚类品种鉴定、品质质量控制、原产地溯源等提出一种新的色谱指纹图谱思路。     

Synthesis of tricolorin F

A hetero-trisaccharide resin glycoside of jalapinolic acid known as tricolorin F has been synthesized. The approach involved the preparation of intermediate 5 and a subsequent coupling reaction with imidate 6 to produce disaccharide 7, which after deacetylation generated intermediate 8. A further coupling between this glycosyl acceptor and the quinovose glycosyl donor 9 resulted in the formation of the tricoloric acid C derivative 10. Basic hydrolysis afforded the intermediate 11, which was subsequently lactonized under Yamaguchi conditions to produce protected macrolactone 12. Removal of acetonide and benzyl protecting groups afforded pure tricolorin F (1).     

三七水煎液中还原型谷胱甘肽及腺嘌呤的分离与鉴定

三七经水煎提取,阴、阳离子交换树脂分离以及RP-HPLC分离获得多种含肽类化合物组分,采用游离及酸水解后氨基酸组成及含量对照分析的方法预示了提取液中肽类化合物的存在,经氨基酸组成分析、聚丙烯酰胺薄膜双向层析、羧肽酶C-末端序列分析、质谱测定等方法分析,将YN-3H12组分鉴定为还原型谷胱甘肽,YN-3H11组分鉴定为腺嘌呤,本研究方法可为植物中水溶性肽类化合物等活性成分的研究提供参考。     

Chemistry of lac resin-VIII: Synthesis of jalaric ester-I,possible key compound in the elaboration of lac resin by laccifer lacca kerr

Preparation of (E)- and (Z)-16-hydroxy-9-hexadecenoic acids and erythro-aleuritic acid starting from naturally occurring aleuritic acid, is described. 16-Hydroxy-(Z)-9-hexadecenoic acid and jalaric acid have been selectively condensed to furnish the naturally occurring jalaric xxxter-I. The possible importance of this compound in the elaboration of lac resin by the insect is pointed out.     

The isolation and structure elucidation of a new sesquiterpene lactone from the poisonous plant Coriaria japonica (Coriariaceae)

A new sesquiterpene lactone named coriarin was isolated from achenes (seeds) of Coriaria japonica (Coriariaceae) along with known constituents tutin, dihydrotutin and corianin, and its structure was deduced on a spectroscopic basis. The structure of coriarin was finally confirmed by the base-catalized chemical conversion of tutin into coriarin, in which the lactone ring linkage was transposed from C-3 to C-2. Chemical investigation of sarcocarps was also undertaken in parallel, but neither sesquiterpene lactones nor related constituents were obtained. The results indicate that sesquiterpene lactones occur only in achenes of C. japonica berry, as is the case in other Coriaria species.     

Botanical Source Differentiation of Podophyllum Resin by HPLC

Abstract

A high-performance liquid chromatographic method to determine botanical sources of Podophyllum resin via approximate podophyllotoxin content is described. North American resin contains about 10% podophyllotoxin, the Indian variety about 40%. Samples are dissolved in mobile phase solution and analyzed by HPLC using normal-phase chromatography with detection at 280 nm. Estimates of podophyllotoxin content were made using commercially available references.     

大孔树脂分离纯化丹酚酸的研究

比较了D301R、D392、D380大孔阴离子交换树脂和X-5.AB-8、NKA-9、SP825大孔吸附树脂对丹参水溶性成分的吸附和解吸能力,筛选出效果较好的SP825进行分离纯化丹酚酸的研究.实验表明,大孔吸附树脂SP825能分离出纯度为95.32%的丹参素,在梯度洗脱条件下可得到以丹参素(水洗脱)和丹酚酸B(乙醇洗脱)为主的产品.在最佳吸附与解吸工艺参数下,丹参素、紫草酸、迷迭香酸、丹酚酸A和丹酚酸B的收率分别为:36.92%、80.39%、82.45%、43.07%和41.03%.