巴戟天中一种多糖的分离与结构表征

以巴戟天的根为原料, 经热水浸提、Sevag法除蛋白、乙醇沉淀和DEAE-Sepharose CL-6B离子交换柱层析, 得到一种水溶性的巴戟天多糖(MOPI-3). 通过UV、IR、NMR、GC-MS、高碘酸氧化、Smith降解和甲基化等物理化学方法对MOPI-3的纯度、理化性质和组成结构进行表征. 结果表明, MOPI-3分子量为36061, 是一种由阿拉伯糖、半乳糖和葡萄糖组成的杂多糖, 以α-1,3-吡喃葡萄糖和α-1,4-吡喃半乳糖为主链, 平均每5个葡萄糖连接一个半乳糖, 每个重复单元具有一个支链, 支链由3个呋喃阿拉伯糖以α-1,3-键型组成, 连接在主链葡萄糖的6位碳上, MOPI-3含有乙酰基, 连接在主链半乳糖的2位碳原子上.     

不同预处理方法对巴戟中砷限量检查的影响

采用５种不同预处理方法对巴戟药材进行处理，并用古蔡氏砷斑法检测其含量，发现不同处理方法的检测结果相差甚大，为中药砷限量检查中正确选择样品预处理方法提供了参考。     

不同提取方法对巴戟天中金属元素含量影响的初步探讨

采用了水提、醇提及模拟胃酸浓度的酸提法对巴戟天药材进行提取,并用火焰原子吸收分光光度法分别对其中的金属元素含量进行了测定。实验结果表明,三种提取方法中,醇提法金属溶出量最少,对于有害重金属含量较高的中药,可以在中药提取的工艺当中,利用不同的提取方法除去有害重金属。通过对三种提取方法所得的提取液中Pb、Cd的存在形态研究表明,Cd在工艺过程除去相对较容易,而Pb较困难,所以应在种植巴戟天时注意避免土壤及水源的Pb污染。     

南药巴戟天中十二种无机元素的初步研究

采用火焰原子吸收光谱法测定了不同产地和生长期的巴戟天中Mn．Fe．Cu．Zn、Ca、Mg、K、Na、Cr、Co、Ni、Pb等十二种无机元素的含量及其灰化率,为研究巴戟天的药效及栽培技术提供了实验数据．     

南药巴戟天中十二种无机元素与药效关系的进一步研究

在初步研究的基础上，进一步研究了不同产地巴戟天的无机元素含量差异，通过对比各元素含量、相关系数及TE图谱，说明地道药材与非地道药材的巴戟天，其特征元素的含量存在非常明显的差异，要使大面积扩种的药材提高药效，建议根据当地土壤含Mn、Fe、Cr、Co、Ni的含量，以旋微量元素肥料的方法来补充这些元素在土壤中的不足。但在微量元素肥料配方中，应注意巴戟天吸收土壤中的元素时的协同作用和拮抗作用。     

中药材巴戟天及其水煎液微量元素的分布模式

模拟传统煎药方式,制备巴戟天水煎液。用电感耦合等离子体质谱法(ICP-MS)测定了药材及其水煎液中11种微量元素Cr、Mn、Co、Ni、Cu、Zn、As、Se、Cd、Sn、Pb含量,用火焰原子吸收光谱法(FAAS)测定了微量元素Fe含量。根据微量元素含量,得到了药材及水煎液微量元素的分布模式。结果表明,巴戟天药材样品富含人体必需元素Fe、Mn、Zn,含量分别是1086.3、393.8、15.1μg.g-1;巴戟天药材与水煎液微量元素的分布模式图清晰地显示了其微量元素的分布特征,且药材与水煎液微量元素的分布模式以及不同煎制时间下水煎液微量元素的分布模式均存在明显差异,进而表明这种微量元素分布模式对中药微量元素的研究和临床应用具有参考价值。     

Surfactant self-assembling in gas phase: electrospray ionization- and matrix-assisted laser desorption/ionization-mass spectrometry of singly charged AOT clusters

The self-assembling of sodium bis (2-ethylhexyl) sulfosuccinate (AOT) in gas phase has been investigated by electrospray ionization- and matrix-assisted laser desorption/ionization mass spectrometry. Large surfactant clusters with an aggregation number close to that found in apolar media have been observed either as positive or negative ions. Moreover, the marked predominance of singly charged species as well as preliminary theoretical calculations strongly suggest an aggregate structure characterized by an internal hydrophilic core hosting the extra charge surrounded by an apolar shell constituted by the surfactant alkyl chains. This structure is similar to that of the more familiar reversed micelles formed when an appropriate surfactant is solubilized in apolar solvents. Finally, similar trends are observed independently either on the ionization technique or the polarity of the solvent used. This, together with the large dependence of the aggregation number on the flow rates, strongly indicates that self-assembling of the surfactant molecules occurs during the evaporation step.     

中性人乳寡糖的分离及结构鉴定

以脱脂、除蛋白后的人乳为原料,联合运用阴离子交换色谱(AEC)、凝胶渗透色谱(GPC)和多孔石墨化碳色谱(PGC)等多种分离纯化技术制备了18种中性人乳寡糖,并采用电喷雾碰撞诱导串联质谱(ESI-CIDMS/MS)技术对其结构进行了鉴定.结果表明,所制备的中性人乳寡糖主要为三至九糖,含有半乳糖(Gal)、葡萄糖(Glc)、N-乙酰葡萄糖胺(GlcNAc)和岩藻糖(Fuc).所有寡糖的还原端均含有乳糖核心(Galβ1-4Glc),非还原端均含有乳糖胺(Galβ1-3/4GlcNAc),并且Fuc以α1-2,α1-3和α1-4连接于主链的Gal,Glc和GlcNAc上.     

Quantitative determination of perfluorinated surfactants in water by LC-ESI-MS/MS

The surfactants perfluorooctanoate (PFOA), perfluorooctane sulfonate (PFOS), and derivatives of the latter have emerged as globally distributed persistent environmental contaminants. Methods for their reliable quantitative determination at ppt-levels (ng/L) are needed in order to detect their main sources, to elucidate their environmental fate, and to identify potential sinks. The common method for water analysis involves preconcentration by SPE followed by LC coupled to ESI MS/MS (LC-ESI-MS/ MS). All sample preparation steps must be carefully optimized in order to arrive at reliable quantitative data. Two major aspects are important: (i) during SPE, contaminations may arise from materials containing traces of PFOA/S; (ii) during LC-ESI-MS/ MS, ionization yields are suppressed by matrix components and depend upon the analyte concentrations in the extracts. The levels of PFOA/S in the river Roter Main near Bayreuth have been determined using the optimized method.     

Rapid Determination of Coumatetralyl in Human Serum by High‐Performance Liquid Chromatography Coupled with Electrospray Ionization Tandem Mass Spectrometry

Abstract

A rapid, sensitive, and selective high‐performance liquid chromatography‐tandem mass spectrometric method (HPLC‐MS‐MS) for the determination of coumatetralyl in human serum using warfarin as an internal standard has been developed and validated. Coumatetralyl and the internal standard were extracted from the human serum samples by liquid‐liquid extraction with ethyl acetate, followed by separation on a XDB C₁₈ reversed‐phase column (150 mm×2.1 mm i.d., 5 µm) using a mobile phase consisting of acetic acid‐ammonium acetate (5 mmol/L, pH=4.5)/methanol (20:80, v/v) at a constant flow rate of 0.40 mL/min. Coumatetralyl and the internal standard were ionized by negative ion pneumatically assisted electrospray and detected in the multiple‐reaction monitoring mode using precursor→product ion combinations at m/z 291→247 and 307→161, respectively. The calibration curve was linear (r²=0.9945) in the concentration range of 0.5～100.0 ng/mL, with a lower limit of quantification of 0.5 ng/mL in human serum. Intra‐ and inter‐day relative standard deviations were less than 6.3 and 11.0%, respectively. The mean extraction recovery was 87.9% for coumatetralyl and 90.1% for the internal standard. This method is found to be able to determine trace coumatetralyl in human serum and can be used for the diagnosis of poisoned human beings.     

Liquid Chromatography–Electrospray Ionization–Mass Spectrometric Method for the Determination of Hydrochlorothiazide in Human Plasma: Application to a Pharmacokinetic Study

Abstract

A rapid, convenient, and sensitive liquid chromatography–electrospray ionization–mass spectrometry method was developed and validated for the quantification of hydrochlorothiazide in human plasma. The samples were first spiked with the internal standard, and the analyte was then extracted with ethyl acetate. The chromatographic separation was achieved on a C₁₈ column by using water–acetonitrile (68:32, v/v) as mobile phase. The method was linear within the range of 2.5–200 ng/ml. The lower limit of quantification was 1.0 ng/ml. Finally, the validated method was successfully applied for the evaluation of the pharmacokinetic profiles of hydrochlorothiazide in healthy male Chinese volunteers.