在线柱浓缩-超高效液相色谱法测定水体中的痕量甲萘威和呋喃丹

采用在线柱浓缩-超高效液相色谱联用技术测定水体中痕量甲萘威和呋喃丹。水样过滤后直接进样,采用固相萃取小柱富集待测物,梯度洗脱后,利用阀切换技术将待测物反冲至分析柱Acclaim RSLC C18(100 mm×2.1 mm, 2.2 μm)上进行色谱分离,以10 mmol/L醋酸铵缓冲溶液(pH 5.0,用醋酸调节)和乙腈分别为流动相A和B,梯度洗脱,泵流速为0.8 mL/min,检测波长为280 nm,二极管阵列检测器检测。甲萘威和呋喃丹在1.0～100 μg/L范围内线性良好(相关系数r2 ＞ 0.9999),检出限(S/N=3)分别为0.5和0.25 μg/L,加标回收率为76.0%～120.0%。用所建立的方法测定了水中痕量的甲萘威与呋喃丹的含量,结果令人满意。     

亲水改性C18填料的制备及其在萃取水中酚类化合物中的应用

通过在甲基丙烯酸十八酯(SMA)中加入亲水性单体甲氧基聚乙二醇甲基丙烯酸酯(PEGMEA),以1-正丙醇/1,4-丁二醇为致孔剂,热聚合得到具有一定亲水性的新型C18填料,并将该填料应用于固相萃取(SPE)富集水中的酚类化合物。实验优化了致孔剂的配比、SPE过程中上样溶液pH值、洗脱剂种类等参数。在上样溶液pH为6.0,以5.0 mL乙腈为洗脱剂的优化条件下,5种酚类化合物在0.5～10 mg/L范围内呈良好的线性关系,检出限为0.16～0.47 mg/L。所制备的亲水改性C18材料已成功用于大辽河水样中酚的检测,平均加标回收率为64.33%～92.14%, 相对标准偏差为4.2%～6.4%(n=3),证明了该填料对环境水样中痕量酚类化合物富集的可靠性。     

小尺度4-巯基苯硼酸修饰纳米金粒子用于大鼠肝脏糖蛋白选择性富集和质谱鉴定研究

报道了利用硼氢化钠还原一步法合成小尺度巯基苯硼酸修饰的纳米金材料（尺寸约为3 nm）,合成方法简便快捷.利用纳米金表面的硼酸基团与糖蛋白/糖肽中顺式邻二羟基的酯化反应,成功实现了糖肽和糖蛋白的选择性富集.利用该材料对糖蛋白HRP酶解产物进行富集,经富集后糖肽质谱峰的信号强度提高近百倍;将该材料用于大鼠肝脏中糖蛋白的富集...     

Determination of relative sensitivity factors for trace element analysis of solar cell silicon by fast-flow glow discharge mass spectrometry

A commercially available Element GD, the latest generation of glow discharge mass spectrometry (GDMS), has been used for quantitative analysis of impurities in silicon for photovoltaic applications (PV silicon). In order to be able to accurately measure impurities in silicon, relative sensitivity factors (RSFs) need to be determined. These factors are, currently, given only for steel matrices. In this study, standard silicon materials with known levels of impurities have been produced and independent analytical methods have been used for determining the RSFs for silicon matrices. It has been found that the tuning parameters of the Element GD, mainly the discharge gas flow rate, influence the RSF values. In addition, it has been found that RSF values are matrix specific; RSFs for a silicon matrix differ significantly from those for metallic conductor matrices even under identical instrumental parameters. A study of the relative reproducibility in the quantitative analysis of impurities in solar cells silicon has shown variations between 5% and 12%.     

电感耦合等离子体原子发射光谱法测定氧化铁粉中微量组分

提出了电感耦合等离子体原子发射光谱法(ICP-AES)测定氧化铁粉中二氧化硅、氧化锰、五氧化二磷、三氧化二铝、氧化镍、氧化钙、三氧化二硼、氧化钠、氧化钾、二氧化钛、氧化镁、氧化铜、氧化铬等含量的方法。使用盐酸直接分解氧化铁粉样品,采用基体匹配法消除基体干扰。方法中各元素的测定下限在7×10-4%~5×10-3%范围内。按所提出方法测定了样品6次,各元素测定值的相对标准偏差(n=6)在1.7%~8.5%之间。     

微波消解-电感耦合等离子体质谱同时测定普里兹湾沉积物中微量元素

以HNO3-H2O2为消解体系,采用微波对沉积物进行消解,建立了普里兹湾沉积物中微量元素的电感耦合等离子体质谱(ICP-MS)测定方法。从样品分析数据可以看出:8个站位10种元素总量变化范围为493.41～1481.02μg/g,总量最大值是最小值的3.00倍。元素Ba、Mn在总量中占了很大比例,V次之,而As、Mo、Ag、Cd的含量很少。大部分元素检出限可达ng/L,仅Co、Mo 2种元素的检出限稍高;各元素线性良好,相关系数r2≥0.9997。方法的RSD<5.0%,适用于普里兹湾沉积物中微量元素的定量分析。     

微波消解样品-火焰原子吸收光谱法测定淡竹叶中痕量元素

产自3个不同地区的淡竹叶样品用硝酸经微波辅助消解,采用火焰原子吸收光谱法测定所得样品溶液中锌、铁、铜、锰、钾、钙、钠、镁、镍、铅、铬、钴、铝和硒等14种痕量元素的含量。14种元素的质量浓度在一定的范围内均与其吸光度呈线性关系。以1#样品为基体,加入适量9种痕量元素的标准溶液做方法的回收试验,测得回收率在98.1%～108.0%之间,测定值的相对标准偏差(n=5)均小于8%。     

仿生消化-单层脂质体萃取在蕨类植物微量金属形态分析和生物可给性评价中的应用

依据化学仿生原理,将整体药物研究与分子药物研究法(以微量元素为指标)相结合,设计体外仿生消化法用于蕨类植物分析前处理。以单层脂质体为细胞膜模型,萃取分离食糜中微量元素形态(单层脂质体亲合态、水溶态);根据单层脂质体亲合态含量对微量元素的生物可给性和危险性进行评价。比较单层脂质体结合亲和态金属在胃、肠中浓度,可得金属主要吸收部位。沙椤茎、叶和蜈蚣草茎、叶成年人摄入安全剂量分别为210.4、153.5、828.2、367.5 g/day,最大摄入剂量分别为864.1、1208.8、2067.1、1977.3 g/day。     

Submicro Determination of Copper and Zinc in Needle Biopsy-Sized Cardiac and Skeletal Muscles by Atomic Absorption Spectroscopy Using Stoichiometric Air-Acetylene Flame

Abstract

A highly sensitive and rapid procedure is described for submicro quantitation of copper and zinc contents from the nitric acid extract of fat free-dry-tissue (FFDT) by a double beam atomic absorption spectrophotometer using stoichiometric air-acetylene flame. Simultaneous background correction was afforded with a deuterium lamp for Zn analysis to eliminate interferences from non-atomic absorption at 213.9 nm. Cu and Zn standards, as well as the muscle extracts, were prepared in an aqueous medium containing 0.75 M Ultrex quality HNO₃ for spectral analysis which did not quench or enhance the relevant absorbance signals. Inherent mineral constituents of muscle such as Ca, Mg, Na, K, and P, when added upto ～10-60 fold greater than the physiological concentration, did not cause either analytical or chemical interferences. Muscle specimens weighing between 0.8-12.0 mg FFDT were extracted in 5 ml of 0.75 M HNO₃ and directly aspirated into the flame. Muscle Cu and Zn contents were expressed in mg/kg FFDT. The smallest sample size confidently analyzed using this technique was ～0.4 mg FFDT which corresponds to 2.0 mg of fresh tissue and can be safely obtained from a patient by muscle needle biopsy. Recovery studies from the inherent muscle matrix revealed 100.01 ± 0.399 and 99.64 ± 0.13% precisions for Cu and Zn respectively.     

Novel Screen-Printed Gold Nano Film Electrode for Trace Mercury(II) Determination Using Anodic Stripping Voltammetry

Integrating the screen printing technique with the vacuum evaporation method, we developed a novel and disposable screen-printed gold film electrode (SPGFE) in the present work. First, a conductive silver layer, a connection graphite-carbon layer, and an insulating polymer layer were successively printed onto a flexible polyethylene terephthalate (PET) substrate. Then, a gold thin film was achieved on the scheduled vacant site by use of the vacuum evaporation method. In order to enhance the electroanalytical performance of the SPGFE, the thickness of the gold film was controlled in the range of 70–80 nm under optimum conditions. The fabricated SPGFE was applied to detect trace mercury(II) based on the square-wave anodic stripping voltammetry (SWASV). The results indicated that the proposed SPGFE exhibited higher sensitivity to trace mercury(II) than the gold disc electrode. The stripping current was linearly related to the concentration of mercury(II) in the range of 16–280 µg/L (R² = 0.9919) and 1.2–8.0 µg/L (R² = 0.9977), with a detection limit of 0.8 µg/L (S/N = 3) under 180 s accumulation. The SPGFE was further used to detect mercury in real samples, and the obtained results revealed a good agreement with those of inductively coupled plasma atomic emission spectrometry (ICP-AES) and atomic absorption spectroscopy (AAS). The highly sensitive and environmental friendly electrode, as another type of “mercury-free” electrode, holds great promise in stripping measurements.