中空纤维膜液相微萃取-高效液相色谱法测定醋酸氯己定痔疮栓中的醋酸氯己定

建立了中空纤维膜液相微萃取-高效液相色谱（HPLC）测定醋酸氯己定痔疮栓中醋酸氯己定含量的方法。将样品用醋酸水溶液萃取5次,配成样品溶液,然后用装有正辛醇的中空纤维膜进行液相微萃取,萃取液用高效液相色谱测定。醋酸氯己定的质量浓度为0.5 ～ 16 mg/L时与其峰面积呈良好的线性关系,加样回收率大于98.0%,相对标准偏差低于4.0%。该方法样品处理简单、快速,灵敏度与不经过液相微萃取的HPLC方法相比提高了约24倍,醋酸氯己定痔疮栓中的其他物质对测定无干扰。     

间苯二胺、间氨基酚与间苯二酚混合液的萃取分离

在不同的酸碱条件下,分别以正丁醇(BuOH)、醋酸正丁酯(BuAc)及甲基异丁基甲酮(MIBK)作为萃取剂,对间苯二胺、间氨基酚及间苯二酚的水溶液混合体系进行萃取分离研究.HPLC分析实验结果表明:随着混合水溶液中H+浓度的增加,分离出间苯二酚的效果增强;而随着混合水溶液中OH-浓度的增加,分离间苯二胺的效果将大大增强;作为萃取剂,醋酸正丁酯和甲基异丁基甲酮优于正丁醇,能对水溶液混合体系中的三组分进行完全有效的分离,其中以甲基异丁基甲酮萃取效果最好.实验得到的最佳分离条件是:萃取剂为甲基异丁基甲酮,混合溶液中n(H+)/n(-NH2)≥1.32∶1时,萃取相中仅有间苯二酚;混合溶液中n(OH-)/n(-OH)≥1.11∶1时,萃取相中仅有间苯二胺.     

甲基绿光度法测定电镀废水中洗涤剂的方法

摘要：本发明涉及一种甲基绿光度法测定电镀废水中洗涤剂的方法,包括以下步骤：（1）准备2．5g／L的甲基绿水溶液、缓冲溶液、三氯甲烷、振荡器、紫外／可见分光光度计、分液漏斗和容量瓶;（2）利用三氯甲烷进行一次萃取;（3）利用三氯甲烷进行二次萃取;（4）利用紫外／可见分光光度计测定洗涤剂含量。本发明通过利用甲基绿水溶液来进行电镀废水中洗涤剂含量的测定,使得测定的偏差小于6％,样液加标回收率在92．9％至103％之间,且方法简便,准确可靠。     

聚酰胺微胶囊的制备及其在处理低浓度含铬废水中的应用研究

如何处理低浓度的含铬废水一直是工业生产中亟待解决的问题之一 ,作者就这一问题进行了大量的基础研究 .首先采用界面缩聚法制备了聚酰胺微胶囊 ,将制得的微胶囊经表面处理后使其具有主动输送功能 ,具有这一特性的微胶囊可以高效、快速提取低浓度废水中的铬 .作者还讨论了微胶囊处理含铬废水的机理、提取速率 .实验证明 ,用微胶囊处理低浓度的含铬废水是行之有效的新技术     

以醋酸纤维素吸水胶囊为载体制备固定化脲酶

把高吸水材料封在具超滤功能的醋酸纤维素（CA）皮膜中，制成胶囊。此胶囊浸泡在脲酶水溶液中，水分受高吸水材料的吸引透过皮膜进入胶囊中，脲酶被截留在CA皮膜上，并且与CA上的活性基团相结合，形成CA胶囊固定化脲酶。     

Separation and analysis of the degradation products of two coals in aqueous NaOC1 solution

两种煤于温和条件下在次氯酸钠水溶液中进行降解,所得水溶液经酸化后,水溶物依次用乙醚、CS2、石油醚、乙酸乙酯和苯进行分级萃取,萃取物经重氮甲烷酯化后用GC/MS分析.结果发现氯代物、脂肪酸和芳酸是煤的NaOCl水溶液降解的典型化合物,不同极性溶剂分级萃取可以实现产物的初步族组分分离.通过该研究建立煤的次氯酸钠氧化反应混合物有效分离和分析的方法,为煤的高附加值利用提供有效的途径.     

HPLC-ESI-MS/MS检测典型废水与活性污泥中4种大环内酯类抗生素

应用超声波辅助萃取技术,联合固相萃取及高效液相色谱-电喷雾串联质谱(HPLC-ESI-MS/MS)技术建立了典型废水和活性污泥中4种大环内酯类抗生素(MLs)的高灵敏分析方法。水样经Oasis HLB萃取小柱富集、净化后以甲醇洗脱;活性污泥样品以乙腈-磷酸盐缓冲溶液为溶剂超声萃取、富集、净化。采用HPLC-ESI-MS/MS进行定量分析;流动相为乙腈-乙酸铵水溶液,采用电喷雾正电离源和选择性反应监测模式进行检测。结果表明,4种抗生素的线性范围为0.1～100μg·L-1,相关系数均大于0.99,方法检出限为0.002～0.019 pg,废水和活性污泥样品中MLs的平均回收率分别为70.2%～90.6%和75.6%～88.7%,方法检出限分别为0.013～0.025 ng·L-1和0.09～0.22 ng.g-1。将建立的方法应用于新疆石河子市可能的抗生素污染源典型废水和活性污泥样品中4种MLs的检测,结果表明,MLs普遍存在于各废水(未检出～308.23ng·L-1)和活性污泥(未检出～120.46 ng.g-1)样品中。     

固态萃取搅拌棒技术/气相色谱联用分析废水中的痕量爆炸物

制备了以聚醚砜酮(PPESK)为萃取相的新型固态萃取搅拌棒, 建立了一种固态萃取搅拌棒/热解吸器直接热解吸/气相色谱联用分析水样品中痕量爆炸物的新方法. 将萃取搅拌棒放入水样品中完成萃取后, 再直接放入热解吸器中于250 ℃热解吸, 将萃取到搅拌棒上的分析物一次性全部导入气相色谱柱中. 对于硝基苯类爆炸物, PPESK固态萃取搅拌棒的萃取容量比萃取纤维针提高1个数量级以上; 其萃取效率比PDMS固态萃取搅拌棒高2个数量级. 对所测定的7种爆炸物的最低检出限为0.008~0.022 μg/L, 方法的重复性误差(RSD)为6.9%~16%, 在线性浓度范围0.06~10.0 μg/L(除TNT)内, 线性相关系数r为0.9962~0.9998. 在优化的条件下对硝基苯类炸药生产过程中产生的废水进行了分析, 结果表明, 方法的回收率分别为88%~100%(低浓度样品)和61%~88%(高浓度样品), 该方法的重复性误差(RSD)小于11%.     

稀醋酸/水溶液中单个醋酸与水分子的氢键结构

在醋酸/水体系的工业分离中,溶液中的氢键对分离效率有很大影响.本文采用两种第一性原理方法,即从头算分子动力学模拟(AIMD)和量子化学计算(QCC),对由单个醋酸和不同水分子所组成聚合体的氢键相互作用进行了研究,采用极化统一模型和自洽反应场模型计算得到了聚合体在水溶液中的热力学数据.从QCC计算的气相和水溶液中的聚合自由能表明六元环在两种状态下都为最优结构,热力学数据反映出的各种结构的相对稳定性与AIMD模拟的环分布符合得相当一致.研究表明,由于存在醋酸和水分子间的氢键作用,稀醋酸/水溶液中的醋酸分离要比在浓醋酸溶液中困难得多.     

“液-液萃取”实验教学内容的选择与拓展

从学生实验能力培养出发,以"液-液萃取"实验内容为例,对较为常见的教学内容"乙醚萃取醋酸水溶液中醋酸"和"四氯化碳萃取碘水中碘"进行比较,提出选用"四氯化碳萃取碘水中碘"作为"液-液萃取"教学内容。并在此基础上,增加"四氯化碳回收"和"碘水中碘的含量测定"为拓展教学内容。教学实践表明:重组的"液-液萃取"项目,不仅丰富了教学内容,增强了实验项目的趣味性和综合性,更重要的是增加了学生课堂动手训练机会,同时对于培养学生化学实验素养、提高对环境保护的意识和自主探究学习精神起到了积极推进作用。     

不同方法提取菟丝子微量元素Fe，Mn和Mg的比较研究

为比较不同提取方法对菟丝子中微量元素含量的影响,采用酸式提取法、碱式提取法、沸水提取法及超声提取法对中药菟丝子中的微量元素进行提取,用原子吸收分光光度法测定了提取液中微量元素铁、锰和镁的含量并进行了比较。结果表明,4种提取方法对微量元素的溶出率由高到低顺序为：铁-酸提,超提,碱提,沸提;锰-酸提,超提,沸提,碱提。镁酸提,沸提,超提,碱提。     

Multiple solid-phase microextraction

Theoretical aspects of multiple solid-phase microextraction are described and the principle is illustrated with the extraction of lidocaine from aqueous solutions. With multiple extraction under non-equilibrium conditions considerably less time is required in order to obtain an extraction yield that is equal to that of one extraction at equilibrium. On the other side, the extraction yield can be increased if multiple extraction is performed with the same total time as is needed for one extraction at equilibrium time. The effect of multiple extraction is strongly dependent on the value of the partition constant and for practical use the length of the desorption time is important. A good agreement between theoretical and experimental data has been obtained. Chromatograms are presented showing the potential of multiple solid-phase microextraction.     

快速溶剂萃取柚皮中的黄酮类化合物

采用快速溶剂萃取法从柚子皮中提取出黄酮类化合物,考察了不同的提取溶剂、提取时间、提取温度、循环次数等提取条件下的提取效果,并与微波法、超声波法及索氏提取法进行了对比.结果表明,快速溶剂萃取法提取柚子皮中的黄酮类化合物,在提取溶剂用量、提取时间和提取效率等方面,均优于传统的提取方法,且自动化程度高,为进一步开发利用柚子皮的药用价值提供了参考.     

盐碱法提取酵母核酸的工艺研究

对盐碱法提取酵母核酸进行了研究。结果表明,最佳提取条件为提取温度85℃,提取pH为7.5,NaCl的含量为6.5%,提取时间180 min,对酵母核酸的平均提取率达到5.70%。     

花生油提取工艺研究

以花生为原料,研究回流法,索式提取法和超声波辅助提取花生粗油脂的工艺条件,结果显示超声波提取在低温短时间内提取率有优势。通过单因素试验和正交试验优化了超声波辅助提取花生粗油脂的工艺条件。结果表明：超声波辅助提取花生粗油脂工艺的最佳条件是：石油醚作为溶剂,料液比1：12（g/mL）,提取温度35℃,提取时间25min,超...     

Pressurized liquid extraction in environmental analysis

A critical evaluation of recent literature utilizing pressurized liquid extraction (PLE) for environmental analysis is presented by compound class. Overall, the extraction efficiency of PLE, using the appropriate solvent, temperature and pressure for extraction, is similar to that of Soxhlet extraction. PLE has been used for some classes of compounds that are thermally labile (e.g., explosives) and may require acidic conditions for extraction (e.g., organometallic compounds). References to recent applications are presented emphasizing studies which utilize unspiked, natural matrices and studies that compare PLE to alternate extraction techniques.     

微波辅助提取-HPLC测定决明子中的5种蒽醌类化合物

通过微波辅助提取法与索氏提取法、超声提取法的比较研究和优化,确定提取决明子中蒽醌类化合物的最佳工艺.采用HPLC测定决明子提取液中芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚5种蒽醌类化合物的含量.结果显示微波辅助提取法效率最高,在乙醇浓度为80%,料液比为1∶50,升温速率8℃/min,于100℃提取15 min时5种蒽醌类化合物的平均回收率为97.0%,RSD均小于1.8%.     

Pressurised liquid extraction of polycyclic aromatic hydrocarbons from contaminated soils

The reliability and efficiency of the pressurised liquid extraction technique (PLE) for extracting polycyclic aromatic hydrocarbons (PAHs) from contaminated soil has been investigated. Experimental design was used to study the influence of seven extraction variables (sample load, solvents used, solvent ratios, pressure, temperature, extraction time, and rinse volume). The results show that large sample loads in combination with small solvent volumes may result in low extraction efficiency. They also indicate that the recovery of low-molecular-mass PAHs is reduced by low extraction temperatures. The exact settings of the other variables are, however, less significant for the extraction efficiency. Repeated extractions at optimised settings of the tested variables show that PLE is an exhaustive extraction technique that generally results in high yields. In addition, extraction of a certified reference material (CRM 103-100) revealed that the method is both accurate and precise. Another finding was that adding the internal standard on top of the soil in the extraction cell causes considerable over-estimation of the concentrations when large samples are extracted with small solvent volumes. This is because the PLE-cell resembles a chromatographic column, so compounds added to the top of the soil layer have a longer distance to travel through the soil compared to the average distance of the native compounds, which are distributed evenly throughout the column. We therefore recommend that the internal standard should be added to the extract immediately after the extraction or, alternatively, carefully mixed with the sample prior to extraction.     

A reinterpretation of C5-BTBP extraction data, performed in various alcohols

The separation of trivalent actinides from trivalent lanthanides present in used nuclear fuel can be achieved by using solvent extraction and the BTBP class of ligands. This separation is relevant for the advanced reprocessing of the used fuel. The choice of diluents in such BTBP based systems has shown to affect the extraction as well as the separation. Long chained alcohols have previously been investigated as such diluents, showing that the americium extraction is higher into alcohols having shorter chains (hexanol, and heptanol) than in longer chained ones (nonanol and decanol). In this work it is shown that not only the distribution ratio, but also the contact time needed before reaching extraction equilibrium is shorter when using shorter chain length of the alcohol diluent. It is also shown that the rate of extraction can be correlated to the interfacial tension between the diluent and the aqueous phase. A low interfacial tension gives a fast extraction while an extraction system with higher interfacial tension needs a longer time of phase contact in order to reach extraction equilibrium.     

中药大黄中蒽醌的微波辅助流动萃取研究

利用微波辅助流动萃取法提取大黄中的蒽醌类化合物，考察了微波提取条件(包括溶剂浓度、微波辐射功率、溶剂提升量)对大黄中葸醌提取率的影响，采用分光光度法测定提取液中蒽醌的含量．结果表明溶剂为60%乙醇，提升量为4mL／min，微波功率为80％时，提取效率最佳．微波辅助流动萃取法与超声波法和索氏提取法相比，具有提取效率高，时间短且节能的良好特点．