痕量砷流动注射在线还原氢化物发生原子吸收测定

方法采用流动注射停流技术使水及土壤浸出液中Ａｓ（Ｖ）在线还原为Ａｓ（Ⅲ），不经手工还原，用氢化物发生原子吸收光谱法直接测定砷的含量。含４ｍｏｌ／Ｌ ＨＣｌ的样品溶液与３０％碘化钾溶液在编结式反应器中混合，并在采样环中停流４０ｓ，达完全还原后注入到载流中与硼氢化钠反应，采样速度５５次／ｈ，检出限（３δ）０．１μｇ／Ｌ，对自来水和土壤浸出液的加标回收结果满意。     

miR-9 and let-7g enhance the sensitivity to ionizing radiation by suppression of NFκB1

The activation of nuclear factor-kappa B1 (NFkB1) in cancer cells may confer resistance to ionizing radiation (IR). To enhance the therapeutic efficiency of IR in lung cancer, we screened for microRNAs (miRNAs) that suppress NFkB1 and observed their effects on radiosensitivity in a human lung cancer cell line. From time series data of miRNA expression in γ-irradiated H1299 human lung cancer cells, we found that the expression of miR-9 was inversely correlated with that of NFκB1. Overexpression of miR-9 down-regulated the level of NFκB1 in H1299 cells, and the surviving fraction of γ-irradiated cells was decreased. Interestingly, let-7g also suppressed the expression of NFκB1, although there was no canonical target site for let-7g in the NFκB1 3' untranslated region. From these results, we conclude that the expression of miR-9 and let-7g could enhance the efficiency of radiotherapy for lung cancer treatment through the inhibition of NFκB1.     

Synthesis and characterization of κ‐carrageenan/poly(N,N‐diethylacrylamide) semi‐interpenetrating polymer network hydrogels with rapid response to temperature

In this study, a novel classical thermo‐ and salt‐sensitive semi‐interpenetrating polymer network (semi‐IPN) hydrogel composed of poly(N,N‐diethylacrylamide) (PDEAm) and κ‐carrageenan (KC) was synthesized by free radical polymerization. The structure of the hydrogels was studied by Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). FTIR and SEM revealed that the semi‐IPN hydrogels possessed the structure of H‐bonds and larger number of pores in the network. Compared to the PDEAm hydrogel, the prepared semi‐IPN hydrogels exhibited a much faster response rate to temperature changes and had larger equilibrium swelling ratios at temperatures below the lower critical solution temperature (LCST). The salt‐sensitive behavior of the semi‐IPN hydrogels was dependent on the content of KC. In addition, during the reswelling process, semi‐IPN hydrogels showed a non‐sigmoidal swelling pattern. Copyright © 2008 John Wiley & Sons, Ltd.     

Direct detection of nanoparticles and components in smoke by time-of-flight mass spectrometry with soft plasma ionization

A new system combining a soft plasma ionization (SPI) source with a time-of-flight mass spectrometer (TOFMS) has been successfully developed and applied to direct and on-line analysis of nanoparticles in smoke generated during combustion of mosquito coils with no sample preparation. The mass spectra of nanoparticles in smoke were examined in conjunction with the effects of species, pressure and current of the SPI discharge on fragmentation. The results indicated that a maximum mass of m/z 1576 was detectable when the following optima SPI conditions were satisfied: a He gas pressure of 1000 Pa with an air pressure of 1600 Pa and a discharge current of 110 mA. Furthermore, considering the results for emission spectra we suppose an ionization mechanism of SPI in which excitation and ionization of nitrogen molecule is promoted by the presence of He gas, leading to promote the smoke sample ionization. The mass spectrum of nanoparticles showed specific patterns of a peak interval of 74 which were assigned to triacetylene (1,3,5-hexatriyne). The most abundant peak in the mass spectrum, at m/z 452, was assigned to triacontanoic acid.     

微波辅助快速制备核-壳型尿苷印迹聚合物及其在线富集应用研究

采用微波辅助加热,以尿苷为模板分子,丙烯酰胺(AA)为功能单体,乙二醇二甲基丙烯酸酯(EGDMA)为交联剂,快速制备尿苷印迹聚合物,聚合时间大大缩短,仅为传统加热的1/8.采用红外光谱和扫描电镜对印迹聚合物进行表征,结果表明二氧化硅表面成功包覆尿苷印迹壳层;该印迹聚合物颗粒分散均匀,印迹壳层厚度约为100 nm.将该印...     

在线净化液相色谱-串联质谱法快速测定牛奶中的6种孕激素

建立了在线净化液相色谱-串联质谱同时测定牛奶中炔诺酮、17α-羟基孕酮、甲羟孕酮、乙酸甲地孕酮、孕酮和醋酸美伦孕酮6种孕激素的方法。本方法采用乙腈为提取溶剂提取目标化合物。提取液经在线净化柱Cyclone-P净化,经Phenyl-Hexyl色谱柱分离,流动相采用0.5%（v/v）甲酸水溶液-乙腈,在电喷雾正离子模式下以多反应监测（MRM）方式测定,内标法定量。方法在0.1~50 μg/L范围内呈线性关系,线性相关系数均大于0.999。6种分析物的测定低限为0.5 μg/kg,在牛奶中3个水平的添加回收率在90.8%~107.5%之间,相对标准偏差在6.3%~11.8%之间。该方法快速简便,灵敏度高,选择性好,可用于牛奶样品中孕激素的快速定性定量分析。     

在线富集离子色谱-质谱联用法同时测定饲料添加剂中的16种有机酸

建立了在线富集方式结合离子色谱-质谱(IC-MS)快速分离分析16种有机酸的方法。离子色谱配备自制富集柱和分离柱对有机酸进行在线富集和分离;质谱采用大气压化学电离源负离子电离方式(APCI^-),在选择离子监控(SIM)模式下对有机酸进行定性和定量分析。采用200 μL大体积进样,在线富集时间为3 min,以NaOH溶液作为淋洗液,梯度洗脱。结果表明,富集柱和分离柱对有机酸有很好的富集分离能力;16种有机酸在30 min内完全洗脱,并在一定浓度范围内线性关系良好;方法检出限(LODs)为0.01~0.22 mg/L;加标回收率为70.6%~110.8%,相对标准偏差(RSD)≤6.3%。该方法样品前处理简单,分离速度快,有机酸检测灵敏度高,适用于多种饲料添加剂样品中有机酸添加剂的检测。     

On-line preconcentration and determination of Au(III) in various environmental/industrial samples by flame atomic absorption spectrometry

A rapid and simple on-line method is described for the determination of Au(III) in various samples. The method is based on the sorption of gold(III) on Lewatit MonoPlus TP207 chelating resin including the iminodiacetate group, which is used as sorbent material and packed in a minicolumn. The chemical variables such as the pH of the sample solution, eluent type, interfering ions and concentrations of reagents, and instrumental variables such as sample loading volume, reagents flow rates, and tubing length, which affect the efficiency of the method were studied and optimised. Au(III) was sorbed on the chelating resin, from which it could be eluted with 3 mol L^?1 HCl, and then introduced directly to the nebuliser-burner system of FAAS. The limit of detection of the method was 0.2 µg L^?1 while the relative standard deviation was <4.0% for 20 µg L^?1 Au(III) concentration. The preconcentration factor was found to be 106 while the optimised sample volume was 15.3 mL. The accuracy of the method was verified by analysing the certified reference material. The developed method was applied successfully for the determination of gold in different samples with satisfactory results.     

在线质谱仪在车内VOCs现场快速监测中的应用

挥发性有机物(VOCs)影响车内空气质量和驾乘者的身心健康。自主研发的在线挥发性有机物质谱仪(SPI-MS 2000),实现了有机物分子的单光子电离,产生无碎片的分子离子,可实现秒级响应,仪器的质量分辨率优于800 FWHM,质量精度优于0.02 amu,对甲苯的测定限优于3μg/m^3,且在3~8000μg/m^3范围内有良好的线性关系。将该仪器应用于某客车车内空气的在线检测:在5 s内检测到20多种微克~毫克每立方米量级的有机物。该仪器在车内VOCs现场快速监测方面有广泛的应用前景。     

On-line extraction and determination of uranium in aqueous samples using multi-walled carbon nanotubes-coated cellulose acetate membrane

In this work, multi-walled carbon nanotubes (MWCNTs)-coated cellulose acetate membrane was used for on-line extraction and pre-concentration of uranium from aqueous samples prior to inductively coupled plasma optical emission spectrometry (ICP-OES) determination. Sample solutions containing the U(VI)-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (Br-PADAP) complex were passed through the membrane. The adsorbed analyte was subsequently eluted from the membrane with acid, which was directly introduced into the ICP-OES nebuliser. The main variables affecting the pre-concentration and determination steps of uranium were studied and optimised. Under the optimised conditions, the enrichment factor of 150 and the detection limit of 0.16 μg L^–1 were obtained. This method was successfully used for determination of uranium in environmental water samples.