黄芩-栀子配伍治疗糖尿病肾病大鼠的尿液代谢组学研究

采用基于超高效液相色谱与串联四极杆飞行时间质谱仪(Ultra-high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry,UHPLC-Q-TOF MS)联用的代谢组学方法,通过分析大鼠尿液内源性代谢物的变化,研究黄芩-栀子药对治疗糖尿病肾病的作用机制。利用高脂高糖饲料喂养并腹腔注射链脲佐菌素(STZ)建立糖尿病大鼠模型。给药12周后,采用UHPLC-Q-TOF MS对正常对照组、模型组、黄芩-栀子药对治疗组的尿液样品进行代谢轮廓分析。利用正交偏最小二乘判别分析(Orthogonal partial least squares discriminant analysis,OPLS-DA)对实验数据进行分析,挑选出对各组分分离贡献较大(VIP>1,p<0.05)的化合物在Human Metabolome Database(HMDB)等数据库进行质谱信息匹配,共鉴定出糖尿病肾病潜在生物标记物31个,给药后回调生物标记物16个。研究结果表明,黄芩-栀子药对通过影响胆汁酸的合成与代谢、尿毒素代谢、能量代谢、色氨酸代谢、苯丙氨酸代谢、酪氨酸代谢等通路对糖尿病肾病起到治疗作用,其中胆汁酸的合成与代谢、尿毒素代谢和能量代谢可能是黄芩-栀子药对发挥治疗作用的主要途径。与单味药相比,配伍后的药对具有了新的药理作用。     

半制备色谱柱的装填及其在中草药分离中的应用

对填料颗粒的尺寸和不同装填方法,即干法和匀浆法填充的半制备柱的柱效和分离效果进行了研究,并应用于中草药的分离。实验结果表明,粒径小的填料装填的柱效及其分离效果要远远优于粒径大的,匀浆法装填的分离结果好于干法且重现性好;对于芍药和银杏提取物使用自装填半制备色谱柱进行分离,可以得到满意的分离结果。     

International comparison of the determination of cadmium and lead in herb: the Comité Consultatif pour la Quantité de Matière (CCQM) pilot study CCQM-P97

A Comité Consultatif pour la Quantité de Matière (CCQM) inter-laboratory comparison program, CCQM-P97, for the analysis of cadmium and lead in Herba Demodii Styracifolii was organized by the Hong Kong Government Laboratory. The objective of the program was to establish comparability of trace metals analysis in herbal matrices amongst the participating national metrology institutes. The arithmetic mean values of the 13 participants were 0.3186 mg kg⁻¹ (RSD = 11.3%) and 1.650 mg kg⁻¹ (RSD = 11.0%) for cadmium and lead, respectively. The participants using double-isotope dilution mass spectrometry technique for their quantification were found to provide similar mean values to those of non-isotope dilution mass spectrometry users. The observation indicated that trace metal analysis in herbal matrices was not method-dependent, but the use of the highest metrological IDMS approach gave a better precision than other routine calibration methods.     

Calderón Couples of Lorentz Spaces

We present some sufficient conditions under which pairs of Banach function lattices are Calderón couples with special attention to the case of classical Lorentz spaces.     

X射线荧光光谱法测定花草茶中22种元素

采用粉末压片法制样,应用X射线荧光光谱法对花草茶中N,Na,Mg,Al,Si,P,S,Cl,K,Ca,Ti,Cr,Mn,Fe,Ni,Cu,Zn,Br,Rb,Sr,Ba,Pb共22种元素进行了分析。讨论了测量条件的选择,对于22种目标元素的分析线,除Ba,Pb采用L线外,其余都选择K_α线,在对Rh靶K_α线的康普顿散射进行测量时,应适当降低管电压,选择合适的管电流。采用经验系数法和3条散射谱线(Rh靶L_α线的瑞利散射、0.1876nm处的散射线、Rh靶K_α线的康普顿散射)作内标进行基体效应校正,并对N,Na,Ca,Ti,Mn,Sr,Ba等部分元素进行了谱线重叠干扰校正。实验结果表明,该方法对N,Na,Mg,Al,Si,P,S,Cl,K,Ca,Ti,Cr,Mn,Fe,Ni,Cu,Zn,Br,Rb,Sr,Ba,Pb各目标元素的检出限较低,且准确度较好,精密度较高。采用该方法对花草茶中元素的种类和含量信息进行分析发现,花草茶元素组成较为丰富,不同种类花草茶元素种类和含量有差异,且同一种类不同来源花草茶略有差异,但元素组成含量特征大体相似。综上可知,该方法操作简单,能够实现花草茶的低成本、快速、准确、多元素测定。     

Phase identification in Ti/TiN diffusion couples with the Kossel technique

A Ti/TiN diffusion couple, which had been prepared by isothermal annealing of a Ti sheet in nitrogen atmosphere at 1091 °C and quenched in water, was investigated by Kossel microdiffraction. Kossel patterns were obtained from all phases present in the diffusion couple (-Ti(N), -Ti₃N_2–x, -Ti₄N_3–x and -TiN_1-x)It could be shown that the Kossel technique has a superior lateral resolution (10 m) compared to commercially used X-ray microdiffraction methods, especially in the case of weak X-ray radiation.     

Quality assessment of traditional Chinese medicine herb couple by high‐performance liquid chromatography and mass spectrometry combined with chemometrics

This study was designed to develop a simple, specific and reliable method to overall analyze the chemical constituents in clematidis radix et rhizome/notopterygii rhizome et radix herb couple using high‐performance liquid chromatography coupled with tandem mass spectrometry and multiple chemometric analysis. First, the separation and qualitative analysis of herb couple was achieved on an Agilent Zorbax Eclipse Plus C₁₈ column (250 mm × 4.6 mm, 5 μm), and 69 compounds were unambiguously or tentatively identified. Moreover, in quantitative analysis, eight ingredients including six coumarins and two triterpenoid sapogenins were quantified by high‐performance liquid chromatography coupled with tandem mass spectrometry. In terms of good linearity (r² ≥ 0.9995) with a relatively wide concentration range, recovery (85.40–102.50%) and repeatability (0.99–4.45%), the validation results suggested the proposed method was reliable, and successfully used to analyze ten batches of herb couple samples. Then, hierarchical cluster analysis and principal component analysis were used to classify samples and search significant ingredients. The results showed that ten batches of herb couple samples were classified into three groups, and six compounds were found for its better quality control.     

纸基质室温磷光法快速测定中药材中西维因的研究

以快速定量滤纸为基质,用KI作为重原子微扰剂,建立了快速测定中药材中西维因的固体基质室温磷光(SS-RTP)分析法。其最大激发和发射波长分别为284nm与520nm。在优化的实验条件下,西维因在4×10-6~2×10-4mol/L浓度范围内呈现良好的线性关系。在样品体积为10μL时,方法的检出限为0.89ng/斑点。所建立的方法用于中草药中西维因残留量的测定。     

中药川芎和赤芍配伍规律的方法研究

提出应用HPLC-PAD-MS研究中药配伍多种化学成分的基本思路,指出应用色谱保留时间、紫外光谱及质谱等多信息、综合对照的方法确定合煎液中各峰的归属,从而进一步研究了中药的配伍规律.首先建立了一套稳定、重复而可靠的液相色谱分析方法进行分离,再用统一的分析方法对分离的色谱图进行数据处理.在HPLC-PAD-MS分析中可得到各成分的保留时间、紫外光谱和分子量信息.通过比较合煎液和单煎液中各成分的保留时间及分子量信息可确定合煎液各峰的归属,最后比较了单煎液和合煎液的化学成分变化.结果表明,川芎和赤芍配伍后有一新峰产生,同时有两个成分含量发生变化.     

液流电池研究进展

和通常熟悉的以固体或气体材料作电极的化学电源不同,液流电池的活性物质是流动着的电解质溶液,是一种可实现规模化储能的电化学装置.本文简要综述液流电池的发展历史及其研究现状,瞻望发展前景,并提出它存在的主要问题.