Separation Membranes Constructed from Inorganic Nanofibers by Filtration Technique

Nanofibrous materials have been extensively investigated and used as building blocks for various nanodevices, due to their unique one‐dimensional structures. Recently, novel membranes constructed by using nanofibers have been reported by various techniques. Here, we will give a critical review of our recent research on the general solution processed unique sub‐3 nm thin metal hydroxide nanofibers and their application for constructing ultrathin separation membranes via filtration technique. The superior separation performances of these membranes hold the promising future for pressure‐driven membrane separation processes.     

Rapid and Sensitive Hplc Determination of Ranitidine in Plasma. Application to Pharmacokinetics Study

Abstract

A rapid and sensitive reversed-phase high-performance liquid chrormatography (RP-HPLC) method for the separation and quantification of the H₂-receptor antagonist drug ranitidine in human plasma is described.

The extraction of ranitidine from plasma by an organic solvent was eliminated in this method. Instead, the pre-chromatography isolation of the drug was done by adding approximately 50 mg of zinc sulfate and 200 μL of acetonitrile in 1.0 mL of plasma. A short column packed with pH-stable (1–13) reversed phase PLRP-S^TM particles was used with an isocratic elution of 5.0mM dibasic potassium phosphate plus 0.50mM tetraethyl ammonium hydroxide/ acetonitrile, 80:20 (v/v). The ranitidine was monitored at 315 nm and 0.20 to 0.002 absorption units full scale (AUFS). The completion time of the assay was less than 15 minutes and had a limit of detection of 1.0 ng/mL for a 100-μL injection volume.

After an oral dose of 150 mg of ranitidine, plasma samples were collected at several time points and were analyzed by using this method to determine various pharmacokinetic parameters.     

Rapid detection and quantification of 35 benzodiazepines in urine by GC-TOF-MS

A rapid and sensitive method for the screening and quantification of 35 benzodiazepines in human urine by gas chromatography/time-of-flight mass spectrometry was developed and validated. Target analytes were isolated from 1 ml urine by solid-phase extraction using Oasis MCX extraction columns (extraction recovery between 35 and 99%). With a supported liquid-liquid extraction method, a new modification of conventional liquid-liquid-extraction, a less time intensive alternative for benzodiazepine extraction is presented. The sample pretreatment entails the derivatization of the benzodiazepines with N,O-bis(trimethylsilyl)trifluoroacetamide plus 1% trimethylchlorosilane. Separation of all benzodiazepines was done within 9.5 min, and detection was based on full mass spectra for each analyte. A deconvolution algorithm was used for unresolved chromatographic peaks to identify coeluted substances. The subsequent quantification was done using significant masses. The limit of quantification is 10 ng/ml for most of the compounds. Linearity is in the range between 10 and 350 ng/ml. Reproducibility was observed with coefficients of variation below 2% at concentrations of 50 and 200 ng/ml. The accuracy is between 88 and 108% depending on the respective analyte and the concentration.     

离子排斥色谱法分析有机酸和无机弱酸

用非抑制型电导检测的离子排斥色谱法,以对甲苯磺酸为淋洗液,研究了柠檬酸、苹果酸、抗坏血酸、乙醇酸、甲酸、乙酸、丙酸及氢氟酸和碳酸的色谱分离及定量检测条件。     

微流体芯片电泳技术对人血清蛋白的快速分离

通过微流体芯片电泳技术分离人血清蛋白,探讨了常见十字形微流体芯片上样品的电动进样与分离过程,分析了在十字芯片上的进样时间和电压设置对后续样品检测和定量的影响。采用的缓冲体系为:100mmol/L H3BO3,50mmol/L NaCl,5%Dextran(以NaOH调至pH 8.3),该缓冲液能够有效分离人血清蛋白中的白蛋白(Albumin)和4种球蛋白(α1-,α2-,β-,和γ-globulin),并且给出了它们在该缓冲体系中的淌度估算范围为5.15×10-5～47.2×10-5 cm2/(V.s)。在芯片上2min之内可以完成进样和分离,相比于常用的毛细管区带电泳,提高了分析速度。     

用聚丙烯酰胺交联涂层毛细管电泳柱分离无机阴离子

研究了用涂层柱分离Ｉ＾－，ＮＯ＾－２，ＮＯ＾－３，ＳＣＮ＾－，ＭｏＯ＾２－４等５种具有紫外吸收的阴离了的毛细管电泳方法。采用涂层柱可以有效地抑制电渗流，因此无需在载体电解质溶液中加入电流改性剂。其优越性在于改善了由于电渗流改性剂与体积较大的阴离子发生离子对相互作用所导致的峰形拖尾现象，有助于准确定理。     

阴离子交换柱分离不同价态砷的研究及其应用

利用醋酸型AG 1-X8阴离子交换树脂和氯化物型AG 1-X8阴离子交换树脂对As(Ⅴ)和As(Ⅲ)吸附的差异,实现As(Ⅲ)和As(Ⅴ)的有效分离。过滤和酸化后的水样流经树脂交换柱(75mm×5.3mm i.d.)时,醋酸型AG 1-X8阴离子交换树脂可吸附As(Ⅴ);而As(Ⅲ)可通过树脂柱。被吸附的As(Ⅴ)用0.12mol/L HCl淋洗出来,在此过程中醋酸型树脂转化为氯化物型树脂。该树脂交换柱可多次循环使用。本方法简单易行,适用于野外现场条件下高砷地下水中As(Ⅲ)和As(Ⅴ)的分离和准确测定;用于检测水铁矿除砷过程中砷价态变化。结果表明,缺氧条件下水铁矿对As(Ⅲ)和As(Ⅴ)的吸附动力学特征遵循假二级反应动力学模式,内扩散不是控制As(Ⅲ)和As(Ⅴ)吸附的因素。随着时间的推移,膜扩散对吸附的控制作用增强。     

Rapid Separation of Antioxidants in Food Samples by Coelectroosmotic CE

Rapid separation of a group of eight antioxidants by coelectroosmotic capillary electrophoresis and their preliminary determination in foods (cereal, wine, and beer) is described. The compounds studied were protocatechuic acid, salicylic acid, p-hydroxybenzoic acid, vanillic acid, syringic acid, p-coumaric acid, ferulic acid, and sinapic acid. The best separation was achieved by use of a running buffer consisting of 125 mM boric acid, 49 mM disodium hydrogen phosphate, 0.002% (w/v) hexadimethrine bromide, and 2.5 mM α-cyclodextrin, at pH 7.5; the analysis time was less than 3.5 min. Ligration time and peak area reproducibility, studied on the same day (n=4) and on three different days (n=12), showed the method is reproducible. A study of the antioxidant content of cereal, wine, and beer samples was conducted to evaluate the usefulness of the method. Antioxidants were extracted from cereal samples by sonication with methanol and from wine and beer samples by solid-phase extraction with C₁₈ cartridges. This preliminary study showed that seven of the eight compounds could be detected in wine and cereal samples whereas only five were detected in beer samples.     

The Use of Cationic Polymer for the Separation of Inorganic Anions by Capillary Electrophoresis

A capillary zone electrophoresis (CZE) method for the simultaneous assay of bromide, iodide, nitrite, nitrate, and thiocyanate using direct UV detection is reported. The method is based on the separation of anions in a capillary coated with a cationic polymer, polyethyleneimine (PEI). The minimum detection limits, reproducibility of peak areas, and migration times were determined at the optimal condition. The method was applied to the analysis of tap water and human urine. The changes in separation selectivity of the anions resulting from addition of the cationic polymer to the buffer were investigated.     

全波长扫描式多功能读数仪-分光光度法测定土壤中无机氮

快速准确测定土壤中铵态氮、硝态氮含量对监测土壤肥力水平和生态环境,指导作物氮肥施用非常重要。选择30份土样,利用全波长扫描式多功能读数仪(酶标仪)结合靛酚蓝分光光度法、硫酸肼还原法测定土壤中铵态氮和硝态氮含量,探讨利用酶标仪测定土壤无机氮含量的可行性。结果显示,利用酶标仪测定土壤铵态氮、硝态氮含量与连续流动分析仪测定结果之间无明显差异,彼此间呈显著线性相关。铵态氮回归直线方程为Y(连续流动分析仪-NH_4~+-N)=0.997 6 X(酶标仪-NH_4~+-N)-0.012 3,相关系数R=0.961 9(n=30,P<0.01);硝态氮回归方程为Y(连续流动分析仪-NO_3~--N)=0.959 3 X(酶标仪-NO_3~--N)+0.021 9,相关系数R=0.964 0(n=30,P<0.01)。酶标仪测定铵态氮回收率在96.2%～108%,相对标准偏差在10%以内;硝态氮测定回收率为94.9%～110%,且相对标准偏差在5%以内,酶标仪测定土壤铵态氮和硝态氮方法检出限分别为0.068mg/L和0.028mg/L。酶标仪测定土壤无机氮速度快,精密度、准确度较高,消耗试剂少,可用于大批量土壤浸提液中铵态氮和硝态氮含量的快速分析。     

Rapid Separation of Prostaglandins by Linear High Performance Thin Layer Chromatography

Abstract

A continuous development technique using silica gel linear high performance TLC plates is described for the separation of prostaglandins 6-keto-F_1α, F_2α, E₂, 13,14-dihydro-15-keto-F_2α, 13–14-dihydro-15-keto-E₂, and thromboxane B₂. Complete separation of all six prostaglandins was achieved with a solvent system of ethyl acetate/acetone/acetic acid (90:5:1). The method is simple, rapid and provides excellent resolution of plasma prostaglandins prior to quantitation by gas chromatography-mass spectrometry.     

A Mild and Efficient Procedure for Dehydration of Primary Carboxamides to Nitriles by Silyl Sulphonyl Polyphosphates

A new dehydration procedure is described for the conversion of aryl, aralkyl and aliphatic carboxamides to nitriles in high yields under mild conditions using silyl sulphonyl polyphosphates.     

A Stability-Indicating Hplc Analysis of Famotidine and Its Application to Kinetic Studies

Abstract

A stability-indicating HPLC analytical method has been developed for the determination of the H₂-receptor antagonist, famotidine in the presence of its degradation products. the method utilizes reversed phase chromatography with UV detection and internal calibration techniques. the mobile phase was comprised of 84% ammonium acetate buffer (pH 2.9) and 16% acetonitrile and pumped at a flow rate of 1.5 ml/min. Quantitation was performed by measuring the peak height ratio of drug to internal standard (salicylic acid). the limit of famotidine detection was determined to be 10 ng (0.4 ug/ml) with a signal to noise ratio of 3:1. Within day coefficient of variation of the method was 2.22% (2.5 μg/ml) and 0.82% (10 μg/ml). Between day coefficient of variation based on the slopes of daily prepared standard curves was 4.70%. the developed method was used to determine the drug content of famotidine tablets. Further, it was used to investigate the kinetics of degradation of the drug in an acidic solution.     

毛细管电泳法快速分离和检测肠毒性大肠杆菌

 建立了快速分离和检测引起仔猪腹泻的肠毒性大肠杆菌K88、K99和 987P细菌细胞的毛细管区带电泳方法 ,并进行了腹泻仔猪粪便中肠毒性大肠杆菌的应用检测分析。结果表明 ,在电泳缓冲液为 0 0 5mol/LNa2 CO3 NaHCO3(pH 9 9)、分离电压为 1 4 1kV、检测波长为 2 1 0nm的电泳条件下 ,E coliK88、K99和 987P的细胞分别具有单一、稳定的特征谱峰 ,其保留时间的相对标准偏差RSD≤ 0 9% ;在确定的实验条件下 ,实现了腹泻仔猪粪便中肠毒性大肠杆菌的快速检测分析 ,发现将出生 5d～ 6d的腹泻仔猪粪便引入培养基中增殖后主要检出K88。     

Universal Janus Filters for the Rapid Separation of Oil from Emulsions Stabilized by Ionic or Nonionic Surfactants

Existing Janus filters cannot separate oil from emulsions stabilized by nonionic surfactants. Reported herein are universal Janus filters that separate oil from emulsions stabilized by not only ionic but also nonionic surfactants. To prepare such a filter, poly(dimethyl siloxane) (PDMS) is grafted onto one side of a fabric. The other side is then grafted with a copolymer polysoap bearing pendant oligo(ethylene glycol) monolaurate (EL) chains. Upon contact with an emulsion, the grafted polysoap competes with free surfactants, ionic or nonionic, for adsorption onto the emulsified droplets, drawing them to the surfaces of the fabric fibers, and causes them to coalesce locally. The coalesced oil then migrates to the PDMS‐coated side of the fabric and selectively permeates it. These novel filters possess enhanced versatility and showcase a new application for polysoaps.     

巯基葡聚糖凝胶分离富集-光度法测定微量有机锗和无机锗

研究了巯基葡聚糖凝胶分离富集 光度法测定微量有机锗和无机锗。在HCl介质中,在抗坏血酸(Vc)、溴化十六烷基三甲基胺存在下锗与2,4 二甲氧基苯基荧光酮形成有色络合物,其ε=1.12×105L·mol-1·cm-1,锗浓度在0～12μg/25mL范围内符合比耳定律。方法可用于多种样品中痕量有机锗和无机锗的测定,结果令人满意。