甲醇-水流动相HPLC测定银杏萜内酯方法优化

优化了甲醇-水流动相HPLC测定银杏萜内酯的方法,建立了线性回归方程,并与药典正丙醇-四氢呋喃-水流动相方法进行比较。在此基础上,用两种方法对银杏叶、银杏外种皮、白果以及银杏叶提取物(EGB)样品中的萜内酯含量进行了对照分析。结果表明,甲醇-水梯度洗脱基线噪音小,柱效高,分离时间短。优化的洗脱条件为:甲醇-水为流动相,0～2 min,0～20%甲醇; 2～32 min,20%～60%甲醇,建立的方法在50～2 000 mg/L的浓度范围内具有良好的线性关系,检出限为0. 05～0. 09μg,不同浓度水平的加标回收率为92. 4%～101. 6%,相对标准偏差(RSD)值为2. 7%～5. 1%。两种方法测定银杏萜内酯没有明显差别,其中测定银杏叶中白果内酯、银杏内酯C、银杏内酯A、银杏内酯B的相对误差分别为0. 86、4. 2、1. 7、3. 9。     

分光光度法测定银杏萜内酯的含量

在弱碱性条件下,银杏萜内酯与Fe(Ⅲ)形成萜内酯-羟肟酸铁紫色环状配合物,最大吸收峰位于514nm处,分光光度法测定萜内酯含量在45~450μg/mL范围内服从比耳定律,标准曲线的回归方程为A=1.9316C 0.0129,相关系数r=0.9994,测定结果与HPLC法对比实验一致。方法简便、快速,可用于银杏样品中萜内酯含量的测定。     

双相深共熔溶剂提取的银杏果外种皮生物活性成分的分离回收

用双相深共熔溶剂（TP-DES）体系同时提取分离银杏果外种皮中亲水性成分萜内酯、黄酮、原花青素和疏水性成分银杏酚酸，分别利用EOPO（环氧乙烷-环氧丙烷共聚物）和大孔树脂对TP-DES中的亲水性和疏水性活性成分进行回收。萜内酯、黄酮和原花青素用分光光度法测定，银杏酚酸用HPLC测定，并根据回收过程中每一步的活性成分含量计算回收率。相对分子质量（简称分子量）为2650，质量分数为90%的EOPO进行回收萜内酯、黄酮和原花青素的回收率分别可达89.44%、53.27%和29.77%； HYA502B树脂静态吸附-解吸回收银杏酚酸回收率可达93.33%。     

高纯银杏萜内酯的超临界CO2提取研究

本文在分析银杏萜内酯重要的药效价值和广阔市场前景的基础上 ,将超临界 CO2 提取工艺与传统的有机溶剂提取法进行比较 ,结果发现超临界 CO2 法提取高纯银杏萜内酯是经济、合理的     

大孔树脂对银杏根皮中银杏内酯C富集工艺研究

目的:建立银杏根皮中银杏内酯C的大孔树脂分离纯化工艺。方法:以银杏根皮为原料,研究大孔树脂分离纯化银杏根皮中银杏内酯C工艺中树脂型号、树脂吸附及洗脱参数。结果:树脂选型为AB-8,其对银杏内酯C的最大静态吸附容量为15.81 mg/g;树脂径高比为1∶8;洗脱流速为3 m L/min;除杂用3 BV纯水;富集洗脱银杏内酯C用8 BV 30%乙醇,柱洗脱液浓缩得银杏根皮提取物,其银杏内酯C含量可从银杏根皮中的0.13%提高至5.24%。结论:本方法可有效地初步分离富集银杏根皮中的银杏内酯C。     

银杏萜内酯在反相高效液相色谱中保留行为

以水 -甲醇为流动相和InertsilODS3为固定相 ,系统地研究了银杏萜内酯的反相高效液相色谱上保留行为。研究表明 ,银杏萜内酯容量因子的对数和流动相中甲醇含量呈线形关系 ,其相关系数γ大于 0 .965。     

萃取银杏内酯动态变化的研究

以银杏叶为材料,研究了超临界CO₂萃取过程中银杏内酯A、B、C在不同时间段内即时质量分数与总获得量的动态变化。采用液相色谱与蒸发光检测器联用检测银杏内酯。结果表明,银杏萃取物的质量随萃取时间的延长而越来越少,前40 min萃取物质量占总量的55.9%。银杏内酯质量分数随萃取时间的延长先增加后减少。银杏内酯A的即时质量分数最高值出现在60～80 min时间段内,为0.403%,银杏内酯B、C即时质量分数最高值在40～60 min时间段内,分别为0.289%、0.246%。银杏内酯A、B、C总获得量随萃取时间的延长而减少,0～20 min时间段内是最高的,分别占整个180 min获得量的33.6%、33.3%、35.4%。     

吸附树脂提取分离银杏叶提取物的研究进展

银杏叶中含有具有药理作用的黄酮类化合物和银杏内酯类化合物,吸附树脂是提取分离银杏叶提取物（GBE）－银杏黄酮化合物和银杏内酯化合物的有效试,本文综述了树提取分离GBE的机理,比较了用不同树脂提取分离GBE的分离效果,并总结了影响吸附树脂分离提取GBE的多种因素,为树脂提取分离银杏黄酮提供了较为全面的科学信息。     

银杏叶超临界CO_2萃取银杏内酯动态变化的研究

以银杏叶为材料,研究了超临界CO2萃取过程中银杏内酯A、B、C在不同时间段内即时质量分数与总获得量的动态变化。采用液相色谱与蒸发光检测器联用检测银杏内酯。结果表明,银杏萃取物的质量随萃取时间的延长而越来越少,前40 min萃取物质量占总量的55.9%。银杏内酯质量分数随萃取时间的延长先增加后减少。银杏内酯A的即时质量分数最高值出现在60~80 min时间段内,为0.403%,银杏内酯B、C即时质量分数最高值在40~60 min时间段内,分别为0.289%、0.246%。银杏内酯A、B、C总获得量随萃取时间的延长而减少,0~20 min时间段内是最高的,分别占整个180 min获得量的33.6%、33.3%、35.4%。     

银杏叶中4种活性成分含量分布规律研究

采用HPLC法对不同树龄及不同年生长月份银杏叶中总黄酮、总萜内酯、莽草酸、绿原酸4种成分含量进行检测,发现树龄对银杏叶中绿原酸、总黄酮、总萜内酯含量有影响,莽草酸含量受树龄影响较小。不同树龄中,1～10年银杏叶中总黄酮、总萜内酯均达到药典要求,而上100年的银杏叶中总萜内酯含量低于0.25%,质量达不到药典要求。4月至9月银杏叶中总黄酮、绿原酸含量随采摘月份增加而下降,而总萜内酯则随叶子年生长月份变大而升高,含量8～9月达到最高,莽草酸含量随月份变化影响较小。研究了不同树龄及不同年生长月份对银杏叶中总黄酮、总萜内酯、莽草酸和绿原酸4种活性成分含量的影响规律,为银杏叶中4种活性成分进行综合利用提供了参考数据。     

C.I.颜料红122在有机溶剂中的溶解行为研究

测试了C.I.颜料红122（PR122）在DMF、DMSO、乙酸乙酯、丙酮、乙醇、甲苯、正己烷和四氯乙烯等八种有机溶剂中的溶解行为,结果表明,PR122在DMF和DMSO中有可观的溶解度,它的最大吸收波长随溶剂极性的增大而增长,它在这两种溶剂中的摩尔吸光系数要比偶氮染料小1个数量级.PR122在乙酸乙酯、丙酮和乙醇中微溶,在甲苯、正己烷和四氯乙烯中几乎不溶.采用国家标准（GB/T5211.5-2008）方法测定该颜料在上述有机溶剂中的溶解度并不科学,原因在于该方法没有考虑到细小的颜料颗粒会穿过普通滤纸的孔径.在DMF中,PR122的溶解度标准曲线服从Y=136.5X＋ 0.156,该回归方程的相关系数为0.9835,标准方差为0.1155;在DMSO中PR122的溶解度曲线服从下列数学式：y=96.5X＋ 0.594,该方程的相关系数为0.9805,标准方差为0.0804.     

银杏内酯的提取纯化与分离

以银杏叶标准化提取物为原料 ,经乙酸乙酯提取纯化得高纯度的银杏内酯混合物 ,方法简单 ,银杏内酯含量达 95 1% ;再以其混合物经硅胶柱层析 ,得到银杏内酯A、银杏内酯B及银杏内酯C的单体化合物     

Chemical analysis of environmental samples collected in Iraq: Analysis for the presence of chemical warfare agents

Nineteen samples from the United Nations Special Commission 65 on Iraq (UNSCOM 65) were analyzed for chemical warfare (CW) related compounds using a variety of spectroscopic and chromatographic techniques including multinuclear NMR, GC (phosphorus, sulfur and atomic emission detection), GC/MS (electron impact and chemical ionization), tandem MS, HPLC/ion chromatography, HPLC/thermospray/MS, FTIR, ICP and GFAA. The samples consisted of one piece of cloth, one piece of wood, six waters, six soils, two vegetation samples and two mortar shell crosscut sections. No intact CW agents were detected; however, diethyl phosphoric acid was unambiguously identified in three of the water samples and ethyl phosphoric acid was tentatively identified, at lower levels, in one of the water samples. Diethyl phosphoric acid and ethyl phosphoric acid are degradation products of munitions-grade Tabun (GA), an organophosphorus nerve agent. However, these compounds are also degradation products of the Chemical Weapons Convention (CWC) scheduled compound Amiton as well as many commercially available pesticides.     

Preparation and Application of Bauxite-based Sintered Mullite Homogenized Grog in Ladle Castable

Preparation of bauxite-based sintered mullite homogenized grog was introduced and its application in ladle castable was studied.Two kinds of bauxite-based sintered mullite homogenized grogs were used,named as GA and GB,respectively.The results show that bauxitebased sintered homogenized grog with uniform components,stable microstructure and mullite as main crystal phase can be prepared using joint process of three-step homogenization,automatic component batching,wet cogrinding,high-temperature calcinations.It also indicates that carbon steel ladle castables with GA or composite aggregate of GA and GB as main materials have the same excellent general performance indicators,great erosion resistance,anti-strip performance and longer service life in field applications,and compared with castables with single aggregate of GA,the castables with aggregate of GA and GB as main materials had higher cost performance because of lower bulk density of GB.     

二甲基环硅氧烷混合物中杂质的分析

利用气相色谱仪和气相色谱-质谱联用仪对二甲基硅氧烷混合环体进行了分析,推测其中一种杂质为含乙基的环硅氧烷。     

仿生催化环己烷空气氧化联产环己醇、环己酮和己二酸工艺的产物分离与分析

针对仿生催化环己烷空气氧化联产环己醇（ROH）、环己酮（RO）和己二酸（AA）工艺的复杂混合物体系,建立了产物分离和分析方法。通过过滤和分液过程将反应产物体系分成油相、水相和固相混合物．然后分别建立定量分析方法。油相采用GC分析环己醇和环己酮含量;水相联合采用GC分析环己醇、环己酮和己二酸环己酯（CHA）,HPLC分析丁二酸（SA）、戊二酸（GA）、己二酸、戊酸（VA）和6-醛基己酸（OCA）含量,水相总有机碳含量由总有机碳分析仪（TOC）测定;固体采用HPLC分析丁二酸、戊二酸、已二酸和6-醛基己酸含量,固相总有机碳含量由元素分析仪测定。该方法可准确给出环己烷的转化率以及环己醇、环己酮和己二酸的选择性。对混合样品的判别分析表明,产物的回收率为99．83％-100．30％．相对标准偏差（RSD）为0．115％～0．631％。     

Phosphate adsorption ability of granular gibbsite and cerium hydroxide

In the present study, the phosphate adsorption abilities of granular materials, gibbsite (GB) and cerium hydroxide (CE), granulated with ethyl cellulose and ethanol, were investigated. For suitable granular conditions using GB or CE, the percentage of binder and amount of solvent were 10% and 3.25 mL/5 g for GB and 7.5% and 2.50 mL/5 g for CE. The amount of phosphate adsorbed by granular GB or CE was similar to that adsorbed by powdered GB or CE. The adsorption isotherms of phosphate were also similar for the granular and powdered materials. The results of a column experiment showed that when GB was used, the suitable concentration of sodium hydroxide as the desorption solution was 2 mmol/L. In these experiments, the amount of phosphate adsorbed was 31.4 mg/g, the amount of phosphate desorbed was 25.3 mg/g, and the recovery percentage was 80.5%. In contrast, when CE was used, the suitable concentration of sodium hydroxide was 500 mmol/L; the amount of phosphate adsorbed was 77.7 mg/g, the amount of phosphate desorbed was 57.8 mg/g, and the recovery percentage was 74.4%. Results also indicate that granular GB and CE could be used at least five times in a column without loss of absorption or desorption abilities. Moreover, granulation of GB and CE is possible using ethyl cellulose and ethanol.     

高良姜挥发油提取工艺研究

目的比较不同方法提取高良姜挥发油的效果,为高良姜挥发油化学成分分析提供参考依据。方法采用水蒸气蒸馏法、溶剂提取法和超声波辅助提取法提取高良姜挥发油,用气一质谱联用仪（GC／MS）对高良姜挥发油成分进行鉴定,采用峰面积归一化法确定各成分的相对含量。结果不同方法提取的挥发油外观性状和产率不同,其挥发油样品的峰的数目也有明显差别。结论水蒸气蒸馏法存在不足之处,索式回流提取和超声波辅助提取可作为有效的补充方法。     

单塔连续制备乙酸乙酯工艺研究

采用反应精馏技术,连续合成乙酸乙酯,通过加入带水剂,使反应生成的水完全带出。在选择的实验条件下,塔顶粗酯产品中乙酸乙酯含量达到91％以上,基本不含酸。塔顶粗酯直接用盐液萃取,可获得符合GB3728—91合格品要求的乙酸乙酯产品。     

Rapid quantitation of fish oil fatty acids and their ethyl esters by FT‐NIR models

Consumption of fish oil and dietary supplements containing eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) has steadily increased because of their reported health benefits. A rapid procedure based on Fourier Transform Near Infrared Spectroscopy (FT‐NIR) models was developed for analysis of fish oil and their ethyl ester derivatives to replace the time consuming GC method. Inclusion of fish oil or ethyl esters containing varied concentrations of OA, EPA, and DHA into the FT‐NIR classification models made possible their classification and quantification. Accurate GC analysis is essential in developing reliable quantitative models since FT‐NIR is matrix dependent. Development of FT‐NIR models based on 30 m PEG capillary GC column results, as recommended by the official GC method for analysis of marine oils, proved problematic, since these columns did not resolve many geometric isomers compared to 100 m highly polar cyanopropyl polysiloxane columns. Depending on the content of geometric isomers in fish oils and ethyl esters, the levels of long‐chain n‐3 PUFA would be overestimated if the model used were based on the results from a 30 m column. The FT‐NIR method was found to be applicable to all fish oil and ethyl ester samples, except when fatty acids were outside the range examined, or contaminants were present. The FT‐NIR method was applicable to analysis of in‐plant intermediates provided contaminants were absent, or identified so they could be incorporated into the model. The FT‐NIR method was suitable to evaluate the shelf life of n‐3 PUFA concentrates.