SPE电极上Pt单组分及Pt-Au双组分还原态CO_2阳极剥离电化学氧化行为研究

采用循环伏安法，对ＳＰＥＰｔ电极以及ＳＰＥＡｕ－Ｐｔ电极上还原态ＣＯ２的电化学氧化行为研究表明，此类电极的电化学特性与光滑Ｐｔ电极一致：ＣＯ２在氢原子吸附电位区０～２５０ｍＶ（ｖｓ．ＲＨＥ）处，可与电极上化学吸附的氢反应，生成还原态的ＣＯ２，通过线性扫描，还原态ＣＯ２即发生一不可逆电化学氧化过程（阳极剥离）．在ＳＰＥＰｔ系列及ＳＰＥＡｕ－Ｐｔ系列上ＣＯ２的电化学行为表明，当ＳＰＥＰｔ系列上Ｐｔ的载量为２．５ｍＬ的０．０１ｍｏｌ·Ｌ－１Ｈ２ＰｔＣｌ６的Ｐｔ时，对还原态ＣＯ２的电催化活性最好，当Ｐｔ的载量相同时，在ＳＰＥＡｕ－Ｐｔ上，催化剂对还原态ＣＯ２的电化学氧化行为比ＳＰＥＰｔ电极更强，这是由于预先沉积的Ａｕ对后沉积的Ｐｔ有调制作用．     

高效液相色谱-串联质谱法同时测定表层水体中5类40种抗生素

建立了固相萃取-高效液相色谱-串联质谱（SPE-HPLC-MS/MS）同时检测表层水中5类40种抗生素的分析方法。水样经过滤、固相萃取柱富集净化后，以乙腈-0.2%（v/v）甲酸水溶液为流动相进行梯度洗脱，采用电喷雾电离源，在多反应监测、正离子模式进行定性定量分析。结果显示，40种抗生素在1~200 μg/L水平下线性关系良好，平均加标回收率为41.3%~112.6%。采用该方法对长江南京段表层水体进行检测，共检出13种抗生素，含量为13.4~780.5 ng/L，其中喹诺酮类抗生素恩诺沙星检出率达100%，大环内酯类抗生素克林霉素最高检出水平达739.4 ng/L。该法高效、灵敏、可靠，可用于实际水样中多种抗生素的分析。     

Preconcentration of copper with multi-walled carbon nanotubes pretreated by potassium permanganate cartridge for solid phase extraction prior to flame atomic absorption spectrometry

A procedure for the preconcentration of copper was described in this paper using multi-walled carbon nanotubes (MWCNTs) oxidized by potassium permanganate as the adsorbent for the enrichment of trace copper in water samples. Important parameters, such as the sample pH, the concentration and volume of eluent, sample flow rate and volume, and interference of coexisting ions, were investigated. The obtained results indicated that proposed method possessed an excellent analytical performance. The linear range, the detection limit, and precison (RSD) were 1-100 ng/mL (R2 = 0.9993), 0.32 ng/mL and 2.88%, respectively. The results showed that copper could be adsorbed quantitatively on the pretreated MWCNTs with potassium permanganate, and proposed method was very useful in the monitoring of copper in the environment.     

Optimization and validation of an enzyme immunoassay for the insect growth regulator fenoxycarb

A competitive enzyme-linked immunosorbent assay (ELISA) was developed for the quantitative detection of the insect growth regulator fenoxycarb. Polyclonal rabbit antisera, raised against protein conjugates of four haptenic derivatives of fenoxycarb, were utilized in immobilized antigen-based, competitive immunoassays. With ELISA systems that were both hapten- and carrier-heterologous, most antiserum titers fell in the range of 1:1000-1:30,000. Assay conditions, including concentrations of antisera and coating antigens, were optimized. The effect of pH, organic solvents, and various blocking agents was also investigated. A hapten-homologous and two hapten-heterologous indirect ELISAs allowed fenoxycarb determination in the range of 0.1-85 ng ml⁻¹ with apparent IC₅₀ values of 1.2-2.8 ng ml⁻¹. Cross-reactivities with a number of compounds (e.g. pesticides of related structure, hapten synthesis intermediates, fenoxycarb metabolite, photodegradation products) were determined, and the assay proved highly selective for fenoxycarb. In particular, no significant interference was found with selected pyrethroid and juvenile hormone analog insecticides, phenoxyacetic acid herbicides, and photodegradation products of fenoxycarb. Using spiked water samples, assay performance was validated by SPME/GC-MS.     

Development of an HPLC method with electrochemical detection of femtomoles of 8-oxo-7,8-dihydroguanine and 8-oxo-7,8-dihydro-2'-deoxyguanosine in the presence of uric acid

A selective method based on high performance liquid chromatography with electrochemical detection (HPLC-ECD) was developed to enable simultaneous detection of 8-oxo-7,8-dihydroguanine (8-oxoGua) and 8-oxo-7,8-dihydro-2′-deoxyguanosine (8-oxodGuo), products of DNA oxidative damage, in the presence of uric acid (UA), a strong interferent in their electrochemical detection. The method developed consists of HPLC isocratic elution with amperometric detection on a glassy carbon electrode, enabling a detection limit for 8-oxoGua and 8-oxodGuo lower than 1 nM in standard mixtures. Detection of low concentrations up to 25 nM of 8-oxoGua and 8-oxodGuo in the presence of UA in a 10⁴-fold higher concentration was achieved after one-step solid phase extraction (SPE). The method was tested with urine samples and it was possible to detect and quantify the presence of 8-oxoGua, and to confirm that UA was eliminated after uricase degradation and SPE. The LOD found in urine samples was about 80 nM, a value higher than in standard mixtures, due to the increase of background current in the urine matrix. The results presented here contribute to the development of a methodological approach to simultaneous determination of 8-oxoGua and 8-oxodGuo in urine samples.     

Solid-phase extraction of iron(III) with an ion-imprinted functionalized silica gel sorbent prepared by a surface imprinting technique

A new Fe(III)-imprinted amino-functionalized silica gel sorbent was prepared by a surface imprinting technique for selective solid-phase extraction (SPE) of Fe(III) prior to its determination by inductively coupled plasma atomic emission spectrometry (ICP-AES). Compared with non-imprinted polymer particles, the ion-imprinted polymers (IIPs) had higher selectivity and adsorption capacity for Fe(III). The maximum static adsorption capacity of the ion-imprinted and non-imprinted sorbent for Fe(III) was 25.21 and 5.10 mg g⁻¹, respectively. The largest selectivity coefficient of the Fe(III)-imprinted sorbent for Fe(III) in the presence of Cr(III) was over 450. The relatively selective factor (α_r) values of Fe(III)/Cr(III) were 49.9 and 42.4, which were greater than 1. The distribution ratio (D) values of Fe(III)-imprinted polymers for Fe(III) were greatly larger than that for Cr(III). The detection limit (3σ) was 0.34 μg L⁻¹. The relative standard deviation of the method was 1.50% for eight replicate determinations. The method was validated by analyzing two certified reference materials (GBW 08301 and GBW 08303), the results obtained is in good agreement with standard values. The developed method was also successfully applied to the determination of trace iron in plants and water samples with satisfactory results.     

液相色谱-串联质谱法检测雄蜂蛹粉中50种抗生素残留

建立了液相色谱-串联质谱检测雄蜂蛹粉中50种抗生素残留（大环内酯类、喹诺酮类、磺胺类、四环素类、硝基咪唑类、林可霉素和氯霉素）的方法。样品经高氯酸溶液和醋酸铅溶液提取沉淀蛋白质，清液用磷酸氢二钾溶液调节pH值至8，经固相萃取净化后进行仪器分析。采用多反应监测正离子或负离子模式检测，可以一次完成对雄蜂蛹粉中50种目标化合物的定性和定量测定。50种抗生素的加标回收率为70.2%~118.3%，相对标准偏差（RSD）为1.8%~13.6%。该方法操作简便，灵敏度高，适用于雄蜂蛹粉中多种兽药残留的分析确证。     

Determination of Naphthalenesulfonate Isomers in Industrial Effluents and River Water by Solid‐Phase Extraction and Capillary Zone Electrophoresis

This work presents a method to separate polar naphthalenesulfonate (NS) isomers by capillary zone electrophoresis (CZE) with ultraviolet detection in industrial effluents and river water samples. The method involves extraction of samples by a polystyrene‐divinylbenzene copolymer (PS‐DVB) solid‐phase extraction (SPE) cartridge. The most effective CZE separation conditions were obtained in 20 mM borate buffer with 30% acetonitrile at pH 9.0 and 30 °C. The method proposed herein provides a high precision and sensitivity for NS isomers, to quantitation at ≤ 1.0 μg/L in 200 mL of the water samples. Recovery of the NS isomers in spiked water samples ranged from 73% to 87% while RSD ranging from 5.6 to 9.7%. The analysis of industrial effluents and river water samples was performed and naphthalene‐2‐sulfonate was found as a major pollutant. The difficulties in quantitating and identifying analytes in complex environmental samples can be resolved by using an internal standard response factor to calculate concentrations and relative migration times for peak confirmation.     

微孔型固体偏氟乙烯-六氟丙烯共聚物电解质

将固体聚合物电解质 (Ｓｏｌｉｄｐｏｌｙｍｅｒｅｌｅｃｔｒｏｌｙｔｅ)用于锂离子电池的研究已经有 3 0年的历史[1] ,从物理角度来看 ,研究过干态型 (ＤｒｙＳＰＥ)、凝胶型 (ＧｅｌｌｅｄＳＰＥ)和微孔型固体聚合物电解质 (ＰｏｒｏｕｓＳＰＥ)三大类型[2 ] ;从化学角度来看 ,研究过含氧、含氮、和含氟的等聚合物[1～ 6 ] .微孔型固体含氟聚合物电解质是近 1 0年来才开始研究并受到产业界很大关注的一种ＳＰＥ .固体聚合物电解质的应用可以解决液体电解质锂离子电池的漏液问题 ,并提高其安全性 ,还可以通过使用塑料包装来减小电池的重量…     

SPE – Microwave‐assisted extraction coupled system for the extraction of pesticides from water samples

SPE is a commonly applied technique for preconcentration of pesticides from water samples. Microwave‐assisted extraction (MAE) technique is the extraction applied for preconcentration of different compounds from solid samples. SPE coupled with MAE is capable of preconcentrating these compounds from water samples too. This investigation was aimed at improving the efficiency of atrazine, alachlor, and α‐cypermethrin pesticide extraction from the spiked water samples applying SPE followed by MAE. In this way, MAE served for elution of pesticides from C₁₈‐extraction disks with solvent heated by microwave energy. Various elution conditions were tested for their effects on the extraction efficiency of the SPE–MAE combined technique. Several parameters, such as elution solvent volume (mL), elution temperature (°C), and duration of elution (min), affect the extraction efficiency of the SPE–MAE coupled system and need to be optimized for the selected pesticides. In order to develop a mathematical model, 15 experiments were performed in the central composite design. The equation was then used to predict recoveries of the pesticides under specific experimental conditions. Optimization of microwave extraction was accomplished using the genetic algorithm approach. Best results were achieved using 20 mL of ethanol at 60°C. Optimal hold time was 5 min and 24 s. The SPE–MAE combination was also compared with the conventional SPE extraction technique with elution of a nonpolar or a moderately polar compound with nonpolar solvents.