双水相气浮浮选光度法分离/测定废水中痕量土霉素

利用自制的浮选装置,选择四氢呋喃作溶剂,氯化钠作分相剂,NaOH溶液调节酸度,将Zn(II)与OTC形成的疏水性缔合物浮选至有机相,浮选完毕后经分光光度法分析,方法线性回归方程为A=2.038×105c(mol/L)+0.005,相关系数r=0.9996,线性范围：1.1×10-7~9.7×10-5 mol/L;检出限7.36×10-8 mol/L;回收率99.8~100.4%;表观摩尔吸光系数ε=2.038×105 L/(mol•cm),适用于废水中痕量土霉素的分离/富集及分析测定。     

Development and validation of a generic RP‐HPLC PDA method for the simultaneous separation and quantification of active ingredients in cold and cough medicines

A novel generic reverse phase high performance liquid chromatography (RP‐HPLC) method is developed and validated for simultaneous determination of seven pharmaceutically active ingredients, namely, acetaminophen, dextromethorphan, doxylamine, phenylephrine, guaifenesin, caffeine and aspirin. All seven ingredients were quantified in soft gel, syrup and tablet formulations of the over‐the‐counter US‐marketed products, as per the guidelines of the International Conference on Harmonization. The separation was achieved in a 16 min run time on an Agilent Zorbax Phenyl column using a gradient method with two mobile phases. Mobile phase A was 0.15% trifluoro acetic acid in purified water and while mobile phase B was a mixture of acetonitrile and methanol (750:250 v/v) with 0.02% trifluoro acetic acid. The flow rate was 1.0 mL min^?1 and injection volume was 10 μL. Detection was performed at 280 nm using a photodiode array detector. As part of the method validation, specificity, linearity, precision and recovery parameters were verified. The concentration and area relationships were linear (R² > 0.999), over the concentration ranges 20–120 μg mL^?1 for acetaminophen, 75–450 μg mL^?1 for dextromethorphan, 31.25–187.5 μg mL^?1 for doxylamine, 25–150 μg mL^?1 for phenylephrine, 25–150 μg mL^?1 for aspirin, 6.5–39 μg mL^?1 for caffeine and 12–72 μg mL^?1 for guaifenesin. The relative standard deviations for precision and intermediate precision were <1.5%. The proposed RP‐HPLC generic method is applicable for routine analysis of cold and cough over‐the‐counter products.     

土霉素(OTC)在东北典型黑土上的吸附行为及其影响因素

采用批量平衡法研究了东北地区典型黑土对四环素类抗生素土霉素(OTC)的吸附动力学特征,以及离子强度、温度和腐熟牛粪DOM对黑土吸附OTC的热力学影响。结果表明:OTC在黑土上的吸附动力学过程包括快速吸附和慢速吸附2个阶段,而且可以较好地被准二级动力学方程拟合。黑土对OTC的吸附过程为吸热熵增反应,属熵增控制过程,且黑土对DOM的吸附以化学吸附为主。Freundlich模型对不同因素影响下DOM在黑土上的吸附热力学过程均能进行较好地描述。离子强度的增加抑制了OTC在黑土上的吸附,不同离子强度作用下黑土对OTC的吸附能力顺序为0.001 mol/L0.01 mol/L0.1 mol/L。温度的增加促进了OTC在黑土上的吸附,不同温度作用下黑土对OTC的吸附能力顺序为35℃25℃15℃。DOM的存在抑制了黑土对OTC的吸附,而且抑制作用随着DOM浓度的增大而增大。黑土对OTC的吸附能力随着OTC添加顺序的不同而改变,符合以下规律:T_s(DOM与OTC同时加入)T_O(先加入OTC)T_D(先加入DOM)。     

纳米级二氧化钛对水中土霉素的光降解实验研究

采用纳米级二氧化钛作为吸附和光催化降解材料,对水中土霉素进行吸附和光催化降解实验,实验过程中考察了反应时间、pH以及二氧化钛投加量对二氧化钛去除土霉素的影响,并分析并判断反应作用机制.结果表明,二氧化钛去除水中土霉素需在紫外灯光的照射下才能发生降解,比较pH和二氧化钛投加量对结果的影响之后发现,二氧化钛的投加量对去除水...     

基于不确定性推理与Fuzzy评判模型的智能选药系统

针对目前非处方药使用中用药不对症、药品种类多难以选出最满意药品的问题,提出了开发非处方药智能选择系统,用计算机实现常见轻微疾病的专家级诊断,获得对症的非处方药,然后根据用户购药时关注药品的不同角度和不同程度,采用二级模糊综合评判模型对对症的非处方药进行满意度评价,按满意度高低依次推荐。智能选药系统可以帮助公众方便地获得最满意的对症药品,指导公众安全、合理使用非处方药。     

Supercritical fluid chromatography as a tool for enantioselective separation; A review

Supercritical fluid chromatography (SFC) has become popular in the field of enantioselective separations. Many works have been reported during the last years. This review covers the period from 2000 till August 2013. The article is divided into three main chapters. The first one comprises a basic introduction to SFC. The authors provide a brief explanation of general principles and possibilities of this method. The advantages and drawbacks are also listed. Next part deals with chiral separation systems available in SFC, namely with the commonly used chiral stationary phases. Properties and interaction possibilities of the chiral separation systems are described. Recent theoretical papers are emphasized in this chapter. The last part of the paper gives an overview of applications of enantioselective SFC in analytical chemistry, in both analytical and preparative scales. Separation systems and conditions are summed up in tables so that they provide a helpful tool for analysts who search for a particular method of analysis.     

新型反相限进材料及其性能

以溴代硅胶为引发剂,CuBr/2,2-联吡啶为催化体系,在改性硅胶上经二步表面引发原子转移自由基聚合(SIATRP)制备内表面接枝甲基丙烯酸十八烷基酯(C18)、外表面接枝甲基丙烯酸环氧丙酯(GMA)、水解得到表面含大量二醇基的新型反相限进材料。使用傅里叶变换红外光谱(FT-IR)、元素分析和热重分析(TGA)对其表征,采用静态吸附实验研究反相限进材料的吸附性能,其对磺胺二甲氧嘧啶和土霉素的最大吸附量分别为18.02和4.80mg/g。结合固相萃取(SPE)评价其对大分子蛋白质的排阻性能,以牛血清白蛋白(BSA)作为排阻大分子模型,排阻能力达90%。将其用于牛奶中土霉素的分离富集,经高效液相色谱(HPLC)检测,土霉素的平均加标回收率为89.19%,相对标准偏差为3.03%。有望将新型反相限进材料和HPLC或液相色谱-质谱(LC-MS)等分析系统结合应用于生物样品的处理和检测。     

融合点测量信息的光学层析方法

光学计算机层析术的困难在于不能得到足够的信息以完全确定探测目标,理论上,将先验知识融入层析术可以在一定程度上降低病态程度,而实际中场的一组孤立点的测量值是一种更为直接的可得信息。利用ＡＲＴ３算法对于含噪声、甚至部分的投影数据具有很好的鲁棒性,并且能友好地融合来自其他测量系统的信息的特点,提出一种利用点测量信息的自适应方法,避免了对重建过程引入原本不存在的高频信息,以及在迭代过程中对预期的低频分量的     

Determination of organotin compounds (OTC) at low levels in seawater by solid-phase extraction (SPE) and gas chromatography-pulsed flame photometric detection (GC-PFPD)

In this work, a simple, sensitive and affordable analytical method for the simultaneous determination of nine organotin compounds (butyltins, phenyltins and methyltins) in seawater using solid-phase extraction (SPE) and gas chromatography-pulsed flame photometric detection was developed and validated. The performance of three different SPE cartridges (Envi C₁₈, Oasis HLB and Oasis MCX) and three elution solvents of different polarity (hexane, methanol and acetonitrile) was evaluated. The extraction parameters, such as solvent volume, presence of complexing and ion-pairing reagents, sample volume and pH and breakthrough volume, were also investigated. Tributyltin, as the organotin compound of special interest, was efficiently extracted using any of the cartridges and solvents tested. However, the simultaneous extraction of all nine organotin compounds was the most efficient using reversed-phase Envi C₁₈ cartridge and 0.1% (w/v) tropolone in methanol as eluent. The optimised method resulted in good recovery, precision and linearity for all compounds, particularly for tri- and disubstituted species. Method detection limits ranged from 0.22 to 1.27 ng(Sn) L^?1 for butyltins, 0.37 to 4.91 ng(Sn) L^?1 for phenyltins and 0.45 to 1.16 ng(Sn) L^?1 for methyltins. The accuracy of butyltins determination was further verified by the comparison with purchased derivatised standards. The developed method was successfully applied to the environmental samples.     

滨海围垦湿地芦苇凋落物分解对模拟增温的响应

采用开顶式生长室(Open-top chambers,OTC)模拟增温,结合网袋法,研究了空气增温(1.984±0.7)℃对崇明东滩滨海围垦湿地代表植物——芦苇(Phragmites australis)不同凋落物组分(茎和叶)分解速率的影响,并分析增温和非增温条件下凋落物分解速率与1.2 m高度的空气温度、0～5 cm土壤温度及0～5 cm土壤湿度3种主要环境因子的相关性及其变化.结果表明:①增温与不增温处理下,OTC组和对照(CG)组芦苇茎的年分解率分别为49.20%和45.11%,而叶的年分解率分别为63.52%和58.53%,增温对叶的分解促进作用更加显著;②增温增大了湿地芦苇凋落物分解常数K值,OTC组和CG组茎的平均K值分别为0.028和0.027,叶的平均K值分别为0.093和0.080,叶的增幅显著大于茎的增幅;③3种主要环境因子与滨海围垦湿地芦苇凋落物的分解速率相关性由大到小依次是1.2 m空气温度>0～5 cm土层温度>0～5 cm土层湿度,且增温使分解速率与3种环境因子相关性程度均增大,其中,叶分解速率与土壤温度的相关性变化最显著,增大6.43%.综上所述,气温是影响滨海围垦湿地芦苇凋落物分解的关键环境因子,增温不仅会增大滨海围垦湿地芦苇凋落物的分解速率,同时也会改变芦苇凋落物分解速率与主要环境因子的相关性.