TBP碳糊修饰电极三元络合物体系测定痕量铅（Ⅱ）

研制了磷酸三丁酯（ＴＢＰ）碳糊修饰电极，在含１－苯基－３－甲基－４－苯甲酰基－５－吡唑酮（ＰＭＢＰ）的ＨＣｌ－ＫＣｌ底液中，通过电位富集，将三元络合物Ｐｂ（ＰＭＢＰ）２（ＴＢＰ）２中的铅富集在电极上，用２．５次微分阳极溶出伏安法测定铅．铅浓度在１．０×１０－９～２．５×１０－７ｍｏｌ·Ｌ－１范围内与峰高呈良好的线性关系．该电极用于铜合金和废水中铅的测定，获得满意结果．     

SLS存在下meso 四(对三甲胺基苯基)卟啉测定微量铜

研究了表面活性剂十二烷基苯磺酸钠（ＳＬＳ） 存在时,ｍｅｓｏ 四（ 对三甲胺基苯基） 卟啉［Ｔ（４ ＴＭＡＰ）Ｐ］ 与铜的显色反应。在ｐＨ＝ ３ ．７ 的ＨＡｃ ＮａＡｃ 介质中,在ＳＬＳ存在下,铜与［Ｔ（４ ＴＭＡＰ）Ｐ］ 形成１∶２ 的稳定配合物,至少在４ ．５ｈ 内吸光度无变化。最大吸收波长位于４１０ｎｍ ,ε＝ ３ ．７９ ×１０５Ｌ·ｍｏｌ－ １·ｃｍ － １ 。铜在０ ～１ ．４０μｇ／２５ｍＬ内有良好线性关系。用于自来水及湖水中铜的测定,相对标准偏差小于３ ％ ,加标回收率在９８ ％ ～１０３％ 之间     

邻菲啰啉和过氧化氢对锰－卟啉显色反应的影响

本文研究了在邻菲啰啉，过氧化氢存在下，Ｔ（４－ＭＰ）ＰＳ＿４、ＴＰＰＳ＿４、Ｔ（４－ＭＯＰ）ＰＳ＿４、Ｔ（４－ＨＰ）ＰＳ＿４、Ｔ（３－ＣＩＰ）ＰＳ＿４、Ｔ（３－ＢｒＰ）ＰＳ＿４等六种卟啉试剂与锰的显色反应。结果表明，当溶液ｐＨ为９．１５～９．３５时，邻菲啉和过氧化氢对锰与卟啉试剂显色反应协同增敏作用显著。加入表面活性剂ＣＴＭＡＢ，增强了配合物的稳定性和灵敏度。表观摩尔吸光系数高达１０￣７Ｌ·ｍｏｌ￣（－１）·ｃｍ￣（－１）。本法用于测定食品中的痕量锰，结果满意。     

（PSF—PDMS—PHS）n／PSF共混物的相容性及表面组成

利用ＤＳＣ、ＤＭＡ、ＴＥＭ和ＸＰＳ对［ＰＳＦ－ＰＤＭＳ－ＰＨＳ］ｎ／ＰＳＦ共混物的相容性及表面组成进行了研究．结果表明，ＰＤＭＳ在共混物表面的富集与ＰＳＦ均聚物和［ＰＳＦ－ＰＤＭＳ－ＰＨＳ］ｎ中硬段的相容性有关；ＰＤＭＳ在相容的共混物体系表面的富集与对应的多嵌段共聚物组成基本相近；不相容共混物体系表面ＰＤＭＳ的富集程度相对较高，当共混物本体中有机硅含量从１％增至５％，表面层ＰＤＭＳ的含量迅速增加，可达到嵌段共聚物中ＰＤＭＳ的含量．     

荧光分光光度法直接测定炎痢停片中的甲氧苄氨嘧啶和氟哌酸

应用荧光分光光度法通过更换溶剂,不经分离同时测定了炎痢停片中甲氧苄氨嘧啶（ＴＭＰ）和氟哌酸的含量。水相中直接测定了氟哌酸含量,乙醇相中测定ＴＭＰ时,引入光度分析中的Ｈ－点标准加入法求得ＴＭＰ的含量。该方法平均回收率：ＴＭＰ为１００．４４％（ＲＳＤ＝１．７６％,ｎ＝５）。氟哌酸为９９．９６％（ＲＳＤ＝１．６２％,ｎ＝５）。此法可作为样品的检测方法,也可应用于生产质量控制和药物代谢研究。     

TBP萃淋树脂色谱分离荧光分析法测定岩矿中痕量铟

本文研究了８—羟基喹啉—５—磺酸荧光法测定铟，在增效试剂ＣＴＭＡＢ存在下，提高了反应的灵敏度，铟在４—１２０ｎｇ／ｍＬ范围内与△Ｆ值呈良好的线性关系，检出下限为４ｎｇ／ｍＬ，其相对标准偏差为０．９４％，本法采用ＴＢＰ萃淋树脂色谱法分离和富集干扰后，可用于地质试样中铟的测定。     

磷酸三丁酯萃淋树脂富集水中痕量酚类化合物的研究

本文对磷酸三丁酯（ＴＢＰ）萃淋树脂为柱填料，研究了富集水中酚类化合物及其洗脱条件。结果表明，以ＴＢＰ萃淋树脂为富集剂，水样ｐＨ值为１－７，以３０ｍｌ／ｍｉｎ的流速通过吸附柱，用８ｍｌ０．１ｍｏｌ／Ｌ的ＮａＯＨ洗脱，多种酚类化合物回收率在９７％－１０３％。此外还试验了地面水中常见干扰物的影响，该方法富集倍数达１２５倍，最低检测限０．５μｇ／Ｌ。对实际样品１－１００μｇ／Ｌ范围内的测定相对标准偏差４．     

基于甲基丙烯酸（9蒽）甲基酯共聚物为敏感膜的土霉素荧光光纤传感器

将甲基丙烯酸（９蒽）甲基酯与甲基丙烯酸甲酯和丙烯酸乙酯共聚，制备了一种具有荧光的共聚物（ＰＡＭＢ）并基于土霉素（ＯＴＣ）对ＰＡＭＢ共聚物荧光的可逆熄灭作用，研制了一种测定ＯＴＣ的荧光光纤传感器，该传感器对ＯＴＣ的响应具有好的稳定性和可逆性。响应时间和回复时间均小于３０ｓ，在２．０×１０＾－７～２．０×１０＾－４ｍｏｌ／ＬＯＴＣ浓度范围内有良好的线性关系，碱金属，碱土金属离子及常用药物对ＯＴＣ测定没     

SLS存在下meso-四(对三甲胺基苯基)卟啉测定微量铜

研究了表面活性剂十二烷基苯磺酸钠存在时,ｍｅｓｏ－四（对三甲基苯基）卟啉「Ｔ（４－ＴＭＡＰ）Ｐ」与铜的显色反应。在ｐＨ＝３．７的ＨＡｃ－ＮＡａｃ介质中,在ＳＬＳ眄,铜与「Ｔ（４－ＴＭＡＰ）Ｐ」形成１：２的稳定配合物,至少在４．５ｈ内吸光度无变化。最大吸收波长位于４１０ｎｍ,ε＝３．７９×１０＾５Ｌ．ｍｏｌ＾０－１．ｃｍ＾－１。     

可变误差多面体法同时测定复方新诺明中二组分的含量

以可变误差多面体法处理多波长吸光光度数据同时测定了复方新诺明制剂模样和五个批号实际样品中磺胺甲恶唑（ＳＭＺ）,甲氧苯氨嘧啶（ＴＭＰ）的含量,１１份模拟样中ＳＭＺ、ＴＭＰ的回收率分别为９９．８％和１００．３％,复方新诺明片和注射液的测定结果与药典方法一致。     

Design of an Imipramine‐Selective Electrode Based on an Ion‐Pair and its Application to Pharmaceutical Analysis

Ion‐selective electrodes play an important role in pharmaceutical analysis due to their simplicity, rapidity and accuracy over some other analytical methods. This research introduces the design of an ion‐pair of imipramine‐tetraphenyl borate (IMP‐TPB) based PVC membrane sensor for IMP hydrochloride determination. Effect of the membrane composition, the pH influence and the effect of lipophilic anionic additives on the response characteristics of the electrode were investigated. After a series of experiments, the best electrode performance was accomplished with a membrane composition of 30% PVC, 63% DBP, 5% (IMP‐TPB) and 2% (NaTPB). This electrode illustrated a fast (15 s), stable and Nernstian response across a relatively wide IMP hydrochloride concentration range (10^?5 to 10^?5 M), in the pH range of (3.0–8.0), and it can be used for at least two months without any measurable change in sensitivity. Additionally, the interference between IMP and several drugs and common inorganic anions was negligible as shown by the potentiometric selectivity coefficient data. The membrane sensor was successfully applied to the determination of IMP in tablets and human urine samples, and very good recovery results were obtained.     

Preparation of polyurethane dispersions by miniemulsion polymerization

With a two‐step miniemulsion polymerization, hydrophobic polyurethane (PU) dispersions were prepared with a cosurfactant, the costabilizer hexadecane (HD) in the oil phase, and sodium dodecyl sulfate (SDS) in the water phase. The first step involved the formation of NCO‐terminated prepolymers between isophorone diisocyanate and poly(propylene glycol) oligomer in toluene. Next, PU dispersions were produced by a miniemulsion method in which an oil phase containing NCO‐terminated prepolymers, HD, the chain extender 1,4‐butanediol (BD), the crosslinking agent trimethylol propane (TMP), and the catalyst dibutyltin dilaurate was dispersed in the water phase containing SDS. The influence of experimental parameters, such as the ultrasonication time, concentrations of SDS and HD, and TMP/BD and NCO/OH equivalent ratios, on the sizes of the miniemulsion droplets and polymer particles, as well as the molecular weights and thermal properties of the PU polymer, was examined. The chemical structure of the produced PU polymer was identified with a Fourier transform infrared spectrometer. The molecular weight distribution and average particle size were measured through gel permeation chromatography and dynamic light scattering, respectively. The thermal stability of the PU polymer was characterized with thermogravimetric analysis. © 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 43: 4870–4881, 2005     

线性扫描极谱法测定药物中的甲氧苄啶含量

研究了用线性扫描极谱法测定药物制剂中甲氧苄啶含量的新方法.在pH=4.5的HAc NaAc缓冲溶液中,甲氧苄啶在 1424mV(vs.SCE)处有一灵敏的极谱还原峰,在一定浓度范围内峰电流与溶质浓度具有良好的线性关系,相对标准偏差为1.21%.测定了药物片剂中的甲氧苄啶含量,与药典方法进行了对照,结果基本一致.     

Preparation of uniformly sized molecularly imprinted polymers for phenolic compounds and their application to the assay of bisphenol A in river water.

Uniformly sized molecularly imprinted polymers, which can recognize bisphenol A (BPA), have been prepared by a multi-step swelling and polymerization method using BPA or a structurally related analogue of BPA [p-t-octylphenol (OP) or p-t-butylphenol (BP)] as the template molecule, 4-vinylpyridine as the functional monomer, and ethylene glycol dimethacrylate as the cross-linker. The BP-imprinted polymer showed higher molecular recognition ability for BPA than the OP-imprinted polymer. The BPA- and BP-imprinted polymers were applied for the assay of a trace amount of BPA in river water using column-switching HPLC with fluorescence detection: A BPA-imprinted polymer was used for removal of BPA from the pretreatment eluent as the trap column, and a BP-imprinted polymer was used for selective pretreatment and enrichment of BPA in river water as the pretreatment column. The calibration graph, constructed from peak area data plotted versus BPA concentration, was linear with a correlation coefficient of >0.999 in the concentration ranges of 25-1000 ppt. The limit of quantitation was 25 ppt with a 5-ml injection. The column-switching HPLC system was successfully applied for the assay of BPA in river water.     

Complexation behavior of gelatin with amphiphilic drug imipramine hydrochloride as studied by conductimetry,surface tensiometry and circular dichroism studies

Herein we report our studies carried out on the interaction between IMP and gelatin in aqueous medium at 25 °C using conductimetry, surface tensiometry and circular dichroism (CD) techniques. Both surface tensiometry and conductimetry results indicate that the drug interacts with the gelatin in a surfactant-like manner, i.e., both critical aggregation (cac) and polymer saturation points (psp) were observed. The interaction starts with the formation of a highly surface-active complex as revealed by the lowering of surface tension on the addition of drug to the macromolecule. The decrease in cac on increasing gelatin concentration is an indication of the strong interaction between gelatin and IMP. However, at low concentration of gelatin the interaction was not much strong as exposed by surface tension study, i.e., the cac was not very clear (as with higher gelatin concentrations). As usual, the psp increased on increasing the gelatin concentration and was always higher than the critical micelle concentration of the drug in pure aqueous medium. Using CD measurements the influence of IMP on the secondary structure of gelatin in aqueous solutions was also investigated. CD studies (performed at very low drug concentrations) illustrated that the random coil content of gelatin increases with increasing drug concentration. Free energies of aggregation (ΔG_agg) and micellization (ΔG_mic) were computed with the help of degrees of micelle ionization obtained from the specific conductivity – [IMP] plots.     

Effect of a Set of Acids and Polymerization Conditions on the Architecture of Polycarbonates Obtained via Ring Opening Polymerization

Polycarbonate‐based polymers with a well‐defined architecture have become interesting materials due to their large range of applications. Ring opening polymerization (ROP) has been largely applied to make branched polycarbonates. The polymer architectures obtained via this method are strictly related with the polymerization mechanisms involved which depend on the polymerization conditions chosen. Hereby, we evaluate the catalytic activity of three acids, fumaric, trifluoroacetic, and methanesulfonic on the Cationic ROP of trimethylene carbonate (TMC) over a trifunctional initiator, trimethylol propane (TMP), under different reaction conditions. In‐detail characterization of the polymers showed the co‐existence of two polymerization mechanisms: the activated monomer (AM), which produces a tri‐armed branched polycarbonate with inclusion of the TMP initiator (TMP‐PTMC), and a combined AM/Activated Chain End (ACE) mechanism, which produces a linear polycarbonate (L‐PTMC). Such mixtures were identified for nearly all the reaction variables investigated, together with other side reactions. Upon optimization of the synthesis, the polymerizations in toluene with TFA at 35 °C and equimolar acid/initiator ratio were optimal, avoiding side reactions, but still resulting in a polymer mixture composed of ～69% TMP‐PTMC and 31% of a polycarbonate linear polymer. The occurrence of such mixed polymer architectures is commonly overlooked in literature regarding CROP of branched polycarbonates. We demonstrate the importance of performing a full characterization for a successful detection of polymer mixtures having different (number of) end‐functionalities, which are critical for further use in advanced applications, such as in the biomedical or pharmaceutical filed. © 2017 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2017 , 55, 1502–1511     

Photodamaging Effects of Porphyrin in a Human Carcinoma Cell Line

A convenient procedure to visualize the photodynamic effect of porphyrins on cell lines is shown. 5,10,15,20-Tetra(4-methoxyphenyl)porphyrin (TMP) was used as photosensitizer. The culture flasks bearing a Hep-2 cell line were incubated for 24 h with 1 M of TMP. Under these conditions saturation of the TMP intracellular concentration is obtained. The irradiation of cell cultures for 30 min produces 90% cell mortality, while no toxicity was observed under dark conditions or under irradiation without TMP. This methodology can be used to demonstrate the photodynamic therapy (PDT) process in a laboratory experiment.     

PHOTOCHEMICAL INTERACTION OF FUROCOUMARINS WITH BROMODEOXYURIDINE AND POLYDEOXY-NUCLEOTIDES CONTAINING BROMODEOXYURIDINE: ITS BIOLOGICAL IMPLICATIONS

Abstract— The photoreaction of 5-bromodeoxyuridine (BUdR) exposed to 360 nm light in the presence of the furocoumarins, 4,5',8-trimethylpsoralen (TMP) and 8-methoxypsoralen (&MOP), was studied and compared to those of thymidine. BUdR reacted with furocoumarins, producing cyclobutane-containing adducts, as does thymidine. Furocoumarins reacted also with BUdR-containing polymer, poly(dA-BUdR) in the double stranded form, at a rate similar to that of thymidine-containing polymer, poly(dA-dT). Polyamines, which slow the photoreactions of TMP with DNA, had no effect on its binding to the two former polynucleotides. It is suggested that because of the similar photoreactions of BUdR and thymidine with furocoumarins, this combination could be used to elucidate the mechanism by which BUdR sensitizes biological systems. In Escherichia coli some sensitization by BUdR of TMP plus 360 nm light killing was observed. It is therefore concluded that at least part of the sensitization of bacteria by BUdR to UV and ionizing radiation is caused by interference with the repair processes. Since no such sensitization was observed in a uvr B mutant, BUdR apparently impairs the efficiency of the excision resynthesis pathway of repair.     

Optimization of an Electrochemical Sensor for Determination of Imidacloprid Based on β‐cyclodextrin Electropolymerization on Glassy Carbon Electrode

An electrochemical sensor based on electropolymerization of β‐cyclodextrin (β‐CD) on a glassy carbon electrode (GCE) was developed for the determination of imidacloprid (IMP). That insecticide is the most commonly used insecticides globally and has been related to the death of bee colonies around the world are imperative. So the development of a simple, cheap and sensitive method for IMP determination is essential. This work aims the modification of a GCE by β‐CD film. The analytical response obtained with GCCE/β‐CD in the presence of the IMP showed an increase in the peak current variation of 947 % in relation to the bare GCE, indicating that the analyte was encapsulated in the β‐CD increasing the detection sensitivity. The followed experimental conditions were optimized: potential range (−1.3 to 0.9 V), presence or absence of dissolved oxygen (presence) and stirring during the electropolymerization (with agitation), number of cycles (5 scans), electrolyte pH (pH=5.0), scan rate (100 mV s⁻¹) and concentration of β‐CD (6 mol L⁻¹). The optimization promoted a peak current variation increase of 57 %, developing a more sensitivity methodology.     

钇离子及其阳离子卟啉配合物与金黄色葡萄球菌的相互作用

用LKB-2277生物活性检测系统考察了Y~(3+)，TMP及其阳离子型钇卟啉配合物 {[Y(TMP)(H_2O)_3]Cl, TMP = 5, 10, 15, 20-四（4-甲氧基苯基）卟啉}对金黄色 葡萄球菌全程代谢作用的影响，测定了Y~(3+)，TMP和[Y(TMP)(H_2O)_3]Cl对金黄 色葡萄球菌作用的产热曲线，根据产热曲线求算了金黄色葡萄球菌在Y~(3+)，TMP ，[Y(TMP)(H_2O)_3]Cl作用下生长代谢的速率常数k_1，k_2，抑制率I_1，I_2，和 半抑制浓度IC_(50)~1，IC_(50)~2等热动力学参数。实验结果表明：Y~(3+)，[Y (TMP)(H_2O)_3]Cl对金黄色葡萄球菌的生长代谢有双向调节作用，在低浓度下表现 为刺激作用，高浓度为抑制作用，而TMP对金黄色葡萄球菌的生长代谢主要为抑制 作用，在低浓度下表现为刺激作用，高浓度为抑制作用，而TMP对金黄色葡萄球菌 的生长代谢主要为抑制作用，对金黄色葡萄球菌的抑制作用[Y(TMP)(H_2O)_3]Cl > TMP > Y~(3+)。