IR光谱分析PEO/V2O5纳米复合材料结构

聚合物溶液直接嵌入法制备 PEO/ V2 O5纳米复合材料。由红外光谱 (IR)表征了 PEO与氧化物层之间的相互作用。V2 O5干凝胶的钒氧双键 (V=O)主要与层间聚合物 PEO中的醚氧键 (Oet)发生作用 ,以Oet…V=O形式存在     

纹党参与白条党参红外光谱的SIMCA聚类鉴别方法研究

以纹党参和白条党参的红外光谱为聚类分析的对象,研究了红外光谱结合SIMCA聚类分析法对纹党参和白条党参进行识别与分类的可行性.选取400 ～2 000 cm~(-1)范围内的光谱,通过基线补偿(Offset)和散射校正(MSC)等预处理后,采用SIMCA聚类分析法建立识别模型.结果表明,所建模型对纹党参和白条党参的识别率分别达92%和96%,拒绝率均为100%.用盲样对所建模型进行了测试,测试结果全部正确.该法可实现对纹党参和白条党参的快速鉴别.     

Rapid quantification of iridoid glycosides analogues in the formulated Chinese medicine Longdan Xiegan Decoction using high-performance liquid chromatography coupled with mass spectrometry [corrected

Longdan Xiegan Decoction (LXD) is a formulated preparation composed of 10 ingredient herbs, with iridoids as the main bioactive components. In this study, a rapid, simple and reliable method of simultaneous determination of four iridoid glycosides in LXD using high-performance liquid chromatography (HPLC) coupled with electrospray ionization mass spectrometry (MS) was first developed and validated. The four iridoid glycosides references were isolated from LXD extract and purified using a preparative HPLC chromatography. The sample preparation for quantification comprised of a simple ultrasonic extraction and the satisfactory chromatographic separation of the four structurally similar iridoid glycosides was effected in less than three minutes on a CAPCELL PAK C(18) MGII column (3 microm, 100 mm x 2.0 mm), using an elution system of 10% methanol and their concentrations in different batches of LXD and ingredient herbs were simultaneously determined by HPLC-MS/MS using a multiple reaction monitoring (MRM) mode. The method was validated with respect to the overall intra- and inter-day variation (RSD less than 8%) and the limits of quantification for the four iridoid glycosides were 35, 20, 37 and 33 ng/mL, respectively.     

Studies on principal components and antioxidant activity of different Radix Astragali samples using high-performance liquid chromatography/electrospray ionization multiple-stage tandem mass spectrometry

The principal components, isoflavonoids and astragalosides, in the extract of Radix Astragali were detected by a high-performance liquid chromatography couple to electrospray ionization ion trap multiple-stage tandem mass spectrometry (HPLC-ESI-IT-MSⁿ) method. By comparing the retention time (t_R) of HPLC, the ESI-MSⁿ data and the structures of analyzed compounds with the data of reference compounds and in the literature, 17 isoflavonoids and 12 astragalosides have been identified or tentatively deduced. By virtue of the extracted ion chromatogram (EIC) mode, simultaneous determination of isoflavonoids and astragalosides could be achieved when the different components formed overlapped peaks. And this method has been utilized to analyze the constituents in extracts of Radix Astragali from Helong City and of different growth years. Then the antioxidant activity of different samples has been successfully investigated by HPLC-ESI-MS method in multiple selected ion monitoring (MIM) mode, applying the spin trapping technology, and the Ferric Reducing Antioxidant Power (FRAP) assay was applied to support the result. The correlations of the isoflavonoids and astragalosides components and the antioxidant activities of Radix Astragali were summarized. The present paper demonstrates that HPLC-ESI-MSⁿ is a powerful method for the characterization of the principal components and evaluation of the antioxidant activity of Chinese medicinal herbs.     

Determination and quantification of astragalosides in Radix Astragali and its medicinal products using LC–MS

In the present study, a liquid chromatography–tandem mass spectrometry method was developed for the separation and simultaneous quantification of astragalosides I–IV in samples of Radix Astragali and a medicinal product thereof (Jinqi Jiangtang tablets). Chromatographic separation was achieved on an Agilent Eclipse XDB (ODS)‐C18 column with a mobile phase consisting of acetonitrile and 0.05% formic acid aqueous solution by use of an efficient 17‐min program. A triple quadrupole mass spectrometer was operated in positive ionization mode with multiple reaction monitoring for the detection of four astragalosides. The saponin ginsenoside Rg1 (similar structure to astralagosides) was used as an internal standard. All calibration curves showed excellent linear regressions (r² ? 0.9912) within the range of tested concentrations. The intra‐ and inter‐day variations were below 4.57% in terms of RSD. The recoveries were 94.38–103.53% with RSD of 1.39–3.58% for spiked Radix Astragali samples. The method was successfully used for the analysis of samples of Radix Astragali and Jinqi Jiangtang tablets. In conclusion, we have developed a rapid, efficient, and accurate LC–MS/MS method for the detection of astragalosides, which can be applied for quality control of Radix Astragali and related medicinal products.     

离子液体分散液相微萃取对苯丙烯酸类化合物的浓缩及作用机制

研究了离子液体分散液相微萃取(ILDLPME)机理, 建立了简单、快速、灵敏的ILDLPME-HPLC(高效液相色谱)同时测定中药白附子中5种低丰度苯丙烯酸类化合物含量的方法, 对不同产地白附子的质量进行了比较和评价. 在最佳的ILDLPME-HPLC条件下, 测得咖啡酸的线性范围为1.28×10^-3~2.60 μg/mL, 对羟基桂皮酸及阿魏酸的线性范围为1.28×10^-4~2.60 μg/mL, 桂皮酸及对甲氧基桂皮酸的线性范围为1.28×10^-3~4.00 μg/mL, 检出限分别为0.13, 0.01, 0.01, 0.13和0.13 ng/mL, 日内精密度RSD<7.9%, 日间精密度RSD<9.7%, 药材中分析物的回收率在86.9%~112.6%之间, ILDLPME 对5种分析物的富集倍数分别在56.0~159.3倍之间. 结合5种苯丙烯酸类化合物ILDLPME萃取前后紫外光谱的变化, 提出了ILDLPME萃取苯丙烯酸羧基-离子液体电荷转移超分子(CTSMCIL)机理. 本研究为建立中药白附子的质量控制方法提供了理论依据和实验基础.     

中药黄芩中神经氨酸酶抑制剂的超滤质谱筛选研究

采用超滤质谱分析技术, 结合体外酶活性实验方法, 从传统中药黄芩提取物中筛选神经氨酸酶抑制剂. 研究结果表明, 中药黄芩提取物具有较强的神经氨酸酶抑制活性, 利用超滤质谱方法从中筛选并鉴定出了六种具有潜在神经氨酸酶抑制活性的化合物, 为开发神经氨酸酶抑制剂提供了实验依据.     

处方应用三种葛根水煎液的二维相关红外光谱分析

中药是复杂的化学体系,建立快速、有效的分析方法有助于中药水煎液的实时质量控制。葛根在处方中常用有三种,分别为粉葛、野葛和煨葛(葛根炮制品),且传统应用中多采用水煎煮的方式,因此,采用傅里叶变换红外光谱技术(FTIR),二阶导数光谱(SD-IR),结合二维相关红外光谱(2D-IR)对三种葛根水煎液进行快速分析。结果表明,通过FTIR和SD-IR光谱能够将粉葛水煎液明显区别于野葛和煨葛水煎液。经过2D-IR分析,发现野葛经过煨制后水煎液化学成分发生了变化,二者在主要的自动峰和交叉峰的位置和强度方面存在较大差异,在1 800~1 300 cm-1范围内,野葛水煎液中最强的自动峰为1 556 cm-1,次强峰为1 561 cm-1,而在煨葛水煎液中最强自动峰为1 563 cm-1,次强为1 572 cm-1,再次为1 556 cm-1。另外,在野葛水煎液中出现了明显的1 536和1 634 cm-1自动峰,二者的强度相当。野葛及煨葛水煎液的2D-IR光谱中,出现的自动峰1 448和1 518 cm-1的相对强度有较大的差异。在野葛水煎液的2D-IR光谱中,交叉峰(1 518,1 561)和(1 518,1 563) cm-1强于煨葛水煎液中相应峰。凭借2D-IR自动峰和交叉峰可以较直观地鉴别野葛和煨葛水煎液,并揭示二者相应各官能团的变化规律,能够为葛根在临床处方应用过程中,水煎液的快速质量控制提供依据。利用FTIR,SD-IR结合2D-IR的整体性和宏观指纹性,可以为中药等复杂体系的逐级鉴别提供快速、准确的方法和手段。     

树脂法分离纯化倒提壶生物碱的研究

采用阳离子交换树脂和大孔吸附树脂联用的方法,将倒提壶生物碱提取液依次经过阳离子交换树脂和两次大孔吸附树脂,对其中的天芥菜碱和毛果天芥菜碱进行分离纯化。结果表明,倒提壶生物碱溶液采用阳离子交换树脂经过水洗和NaCl洗脱与大孔吸附树脂两次经乙醚和50%乙醇洗脱后,毛果天芥菜碱与天芥菜碱的纯度分别从0.73%和2.2%提高至81.6%和79.2%,提取量分别由4.6 mg/g和10.7 mg/g提高至50.6mg/g和92.7 mg/g。该文所建立的分离纯化方法具有成本低、污染小、周期短、操作简便和分离纯化效率高等特点,适合工业化生产。     

Polymer phase separation in composite latex particles. 1. Considerations for the nucleation and growth mechanism

This study addresses the question of how polymer phase separation takes place during polymerization reactions within composite latex particles. Experiments resulted in acrylic/styrene latices with two-phase structures that were analyzed via TEM. Those that resulted from the use of semi-batch reactions allowed us to observe domains that likely did not undergo phase rearrangement after they were formed within the particles. We computed the critical size of the phase-separated domains by assuming that the nucleation and growth mechanism applied to such experiments. We also computed how much these domains would increase in size by subsequent polymerization within those domains. Comparisons of predicted and experimental domain sizes and distributions showed quite reasonable agreement. The domains formed in latex particles of about 350 nm were in the 30–50-nm range. Despite the close agreement between theory and experiment, we are not convinced that phase separation occurs by nucleation and growth, as it appears to us that given the relative rates of reaction and polymer diffusion, phase separation events will often be forced to occur within the spinodal region of the phase diagram. To cite this article: J.M. Stubbs, C. R. Chimie 6 (2003).