新型尾式硫代苯并噻唑基卟啉化合物的合成与表征

通过不对称的单羟基卟啉化合物、溴代烷烃和巯基苯并噻唑合成了一系列新型硫代苯并噻唑基尾式卟啉化合物, 并采用核磁共振氢谱、碳谱、红外光谱、质谱和元素分析对卟啉化合物的结构进行了表征.     

Computer interactive identification system for polycyclic aromatic hydrocarbons in reversed-phase microcolumn liquid chromatography

Summary A computer interactive identification system is proposed which is based on the relationship between retention and molecular properties such as the size and shape of polycyclic aromatic hydrocarbons (PAHs). This system offers an automatic analytical process for liquid chromatography, providing a reliable identification of the separated components. The identification can be further enhanced by the use of multiple detectors such as a multichannel UV detector. The system can be used for optimization procedures, resulting in a highly automatic complex analytical system.     

傅里叶变换红外光谱和傅里叶变换拉曼光谱法无损鉴别药材的真伪

利用傅里叶变换红外（FT-IR）和近红外傅里叶变换拉曼（NIR FT-aman）光谱法对大黄（西宁大黄）与伪品大黄（华北大黄、山大黄、水根大黄）进行了无损快速的鉴别。结果表明：尽管正品大黄与伪品大黄差别较小，有大部分的化学成分有很大的相同之处，但在红外、拉曼谱图中各自的特征峰较突出，根据谱峰的强度和位置可容易地将它们区别开来。红外和拉曼光谱法相互印证，相互补充，具有快速、准确、操作简单、重复性好、不需对样品进行分离提取，可直接鉴别等特点。     

皱叶香茶菜化学成分的研究

从采自西藏的皱叶香茶菜中分离鉴定了3对B-闭联对映贝壳杉烯型二萜化合物:二萜化合物皱叶香茶菜素(Ⅰ)和二氢皱叶香茶菜素(Ⅱ);isodocarpin(Ⅲ)和dihydroisodocarpin(Ⅳ)及Carpalasionin(Ⅴ)和dihydrocarpalasionin(Ⅵ)。(Ⅰ)、(Ⅲ)和(Ⅴ)分别与对应的二氢化合物(Ⅱ)、(Ⅳ)和(Ⅵ)以混合物的形式被分离和鉴定。化合物(Ⅱ)为新化合物,(Ⅰ)、(Ⅳ)和(Ⅵ)首次在自然界发现,(Ⅲ)和(Ⅴ)为已知化合物。     

钳蝎毒中抗癫痫肽、镇痛肽和抗肿瘤肽的快速同时分离和鉴定

采用Shim-Pack WCX-1型阳离子交换高压色谱柱对中国东亚钳蝎全蝎毒进行了分离，在鉴定了其中的抗癫痫肽、镇痛肽和抗肿瘤肽活性峰的基础上，应用Shim-Pack DIOL-300型凝胶排阻高压色谱柱对它们进行了进一步分离和鉴定，可以得到较纯的3种多肽。在高压色谱所提供的全蝎毒分离信息的基础上，应用与Shim-Pack WCX-1色谱柱具有相同交换基团的、具有较大吸附容量的CM Sepharose CL-6B软胶介质在低压色谱上对全蝎毒进行了分离，并分别对其中的抗癫痫肽、镇痛肽和抗肿瘤肽进行了鉴定。     

大鼠体内复方清开灵代谢物的分析

建立了复方中药清开灵代谢物的液相色谱-质谱/质谱分析方法。采用Phenomenex Luna C18色谱柱,以0.1%甲酸(A)及V(甲醇)∶和V(乙腈)=4∶1混合液(B)作流动相,采用梯度洗脱(0 min,B为0%;33min,B为60%;66 min,B为88%;75 min,B为100%),流速:0.5 mL/min,离子阱质谱负离子模式进行检测。通过差谱方法对可能的代谢物进行快速搜索。对发现的重要的代谢物根据分子量以及多级质谱的碎片离子数据,结合体内代谢反应规律,进行指认和结构鉴定。共鉴定了3个主要的代谢物,其中一个为黄芩苷的代谢物,另两个为绿原酸的代谢物,后两个代谢物未见文献报道。本实验为研究复方中药复杂体系体内的代谢产物提供了一个有效而且快捷的模式。     

A New Technique of Synthesizing 10—Hydroxy—5—methyl—5,10—dihydrophenophosphazine 10—Oxide

10-Hydroxy-5-methyl-5,10-dihydrophenophosphazine 10-oxide(1)was prepared by a new technique of treating 10-methoxy-5,10-dihydrophenophosphazine 10-oxide(2)with an equivalent of NaH in anhydrous DMF,and then at 120℃ for 3-4h,which not only avoided poisonous and expensive methyl iodide used in literature,but made the consumption of NaH greatly decrease as well.The possible reaction mechanism was also described.The chemical structure of 1 was confiremed by IR,NMR,and mass spectroscopy.     

新型除草剂丙酯草醚A环14C均标记合成和鉴定

以U-¹⁴C-对氨基苯甲酸为前体, 通过酯化、缩合、还原和取代四步反应获得了A环¹⁴C均标记的丙酯草醚, 用PHPLC对其进行纯化. 采用HPLC-MS(ESI), MS(EI)和¹H NMR验证了其结构, 通过HPLC(外标法)确定其化学纯度大于98%; HPLC-LSC和TLC-IIA两种方法分析表明, 其放射化学纯度大于98%, 其比活度为1.089±0.011 mCi/mmol. 合成的化学收率和放化收率均为53%.     

Analysis of polynuclear aromatic hydrocarbons by glass capillary gas chromatography using simultaneous flame ionization and electron capture detection

The possibility of simultaneous application of an electron capture (ECD) and a flame ionization detector (FID) connected to a glass capillary column for analyzing polynuclear aromatic hydrocarbons (PNA) has been investigated. The ECD/FID ratio is determined for 46 PNA compounds. The ratios vary from 0.02 to 117 with relative standard deviations better than 20 percent determined from 10 replicate analyses. The results suggest that the method may be used for obtaining additional evidence in identifying PNA in environmental samples. Impurities and transformation products in the standard were identified by computerized glass capillary gas chromatography/mass spectrometry. Quinones and diones are responsible for the high EC-response determined in some trace components in the standard. An application of the method is shown for PNA from particulates in urban atmospheres.