QuEChERS-超高效液相色谱-串联质谱法快速测定3种叶菜中矮壮素和丙环唑残留

建立了菜心、芥蓝和小白菜中矮壮素和丙环唑残留的分析方法.以QuEChERS法进行样品前处理,采用含1％ HAc的乙腈溶液提取,无水MgSO4、C18及PSA吸附剂净化,超高效液相色谱-串联质谱(UPLC-MS/MS)法测定.对提取溶剂、吸附剂和色谱柱的选择进行了研究探讨.结果表明矮壮素在1～1 000 μg/L、丙环唑在1～500 μg/L浓度范围内均有良好的线性关系.矮壮素和丙环唑的检出限分别为0.1 μg/kg和0.01 μg/kg;在0.010、0.10和0.50 mg/kg 3个添加浓度水平下,菜心、芥蓝和小白菜中矮壮素和丙环唑回收率为75.0％～96.2％;相对标准偏差为0.9％～8.3％;方法定量限为最低添加浓度0.010 mg/kg.该方法快速、简便、准确,满足叶菜中矮壮素和丙环唑残留分析的要求.     

石墨烯基复合材料去除和检测重金属离子的研究进展

石墨烯具有超大的比表面积、较快的载流子迁移速率和优异的电催化活性,广泛用于环境保护与检测领域。过去几年,基于石墨烯的大批高效吸附剂和传感器均被开发并应用于重金属离子的污染治理。本文详细阐述了石墨烯基复合材料在重金属离子去除和检测方面的研究进展,同时比较了不同方法的优缺点,最后对后续研究方向进行了展望。     

Ionic liquids as precursors for highly luminescent,surface-different nitrogen-doped carbon dots used for label-free detection of Cu/Fe and cell imaging

Carbon nanodots (C-Dots) have attracted much attention in recent years due to their low cost, ready scalability, excellent chemical stability, biocompatibility and multicolor luminescence. Here, we report a facile strategy for producing highly luminescent, surface-different nitrogen-doped carbon dots (C-Dots) by using different ionic liquids (ILs). Intriguingly, the surface-different C-Dots show different selectivity for Cu²⁺ and Fe³⁺. To the best of our knowledge, this is the first example which shows that ILs are excellent precursors for producing luminescent nanomaterial used for detection of different metal ions. The resultant nitrogen-doped C-Dots are highly photoluminescent and can be used for multicolor bioimaging. Most notable, by taking different ILs as precursors, we obtain surface-different C-Dots, which can be directly used for selective detection of Cu²⁺ and Fe³⁺ without any modification. These C-Dots based sensors exhibit high sensitivity and selectivity and the sensing process can be easily accomplished with one-step rapid operation. More importantly, compared with other method using QDs, organic dyes and organic solvent, this strategy is much more eco-friendly. This work may offer a new approach for developing low cost and sensitive C-Dots-based sensors for biological and environmental applications.     

Measurement techniques for mercury species in ambient air

This review critically evaluates the measurement methodologies most commonly employed for the analysis of the various forms of mercury (Hg) in air. Emphasis is given to the three most common forms of mercury in air [i.e. gaseous elemental mercury (GEM, Hg⁰), reactive gaseous mercury (RGM), and particle-bound mercury (Hg_p)]. Moreover, we also briefly describe methods dealing with gas-phase analysis of organic mercury species (e.g., mostly methyl mercury), as they are also reported to be present in air on rare occasions. To begin with, we describe the approaches to sampling airborne mercury species and associated sample-treatment strategies. We evaluate both conventional and emerging alternative detection techniques for different mercury forms with respect to their applicability in airborne mercury analysis. We also discuss the artifacts and the biases associated with analysis of different mercury species. Finally, the review summarizes current methodological developments for the determination of mercury in air and highlights future prospects for improvements.     

Detection of explosives in traces by laser induced breakdown spectroscopy: Differences from organic interferents and conditions for a correct classification

With the aim to study and to improve LIBS capability for detecting residues of energetic compounds in air surrounding, nine types of explosives and some potential interferents, placed in small quantities on a metallic support, were interrogated by a laser. Shot-to-shot behavior of the line intensities relative to the sample constituents was studied. The detected plasma was not stoichiometric and the line intensities, as well as their ratios, were changing even for an order of magnitude from one sampling point to another, particularly in the case of aromatic compounds. We explained some sources of such LIBS signal's behavior and this allowed us to establish a data processing procedure, which leads to a good linearization among the data sets. In this way, it was possible to determine some real differences between the LIBS spectra from explosives and interferents, and to correlate them with molecular formulas, with some known pathways for the molecule's decomposition and with successive chemical reactions in the plasma. Number spectral parameters, which distinguish the each studied explosive from other organic materials, were also determined and compared with previously published results relative to percentages of correct classifications for the same explosives. Experimental conditions for reliable recognition of the explosives by LIBS in air are also suggested, together with the parameters that should be considered or discarded from the classification procedure.     

液相色谱串联质谱法测定蔬菜中四聚乙醛残留量

建立了测定蔬菜中四聚乙醛残留量的液相色谱串联质谱方法.蔬菜样品经乙腈提取,盐析后吹干乙腈提取液,再用氟罗里硅土固相萃取小柱净化,用正已烷/丙酮(80:20,V/V)混合溶剂洗脱,氮吹后用乙腈-20mmol/L,乙酸铵溶液(70:30,V/V)溶解后进行仪器分析.分析采用XBridgeTM C18色谱柱分离,乙腈-20m...     

电化学免疫传感器在食品安全检测中的应用进展

介绍了3种电化学免疫传感器的组装、构建,着重评论了近十年来其在食品安全检测中的应用研究,并对其前景进行了展望(引用文献30篇)。     

Quantitative trace analysis of eight chloramphenicol isomers in urine by chiral liquid chromatography coupled to tandem mass spectrometry

Chloramphenicol is a broad-spectrum antibiotic with, apart from its human medicinal use, veterinary abuse in all major food-producing animals. Chloramphenicol occurs in four stereoisomers (all para-nitro substituted) and furthermore four meta-nitro analogs of chloramphenicol exist. In this paper these are referred to as eight chloramphenicol isomers. According to EU regulations an analytical method should be able to discriminate the analyte from interfering substances that might be present in the sample, including isomers. For the first time a quantitative method for the analysis of trace levels of eight chloramphenicol isomers in urine by chiral liquid chromatography in combination with tandem mass spectrometric detection is reported. The separation of the isomers on the analytical column, the clean-up of urine and the selectivity of the monitored product ions turned out to be critical parameters. To obtain reproducible retention isocratic elution on a chiral AGP column was applied. For urine samples matrix compounds present in the final extract caused decreased retention of the isomers on the chiral stationary phase and a lack of chromatographic resolution. Therefore an extended clean-up procedure that combines solid phase extraction and liquid-liquid extraction had to be developed. The final method was fully validated and showed satisfactory performance for all isomers with decision limits (CCα) ranging from 0.005 to 0.03 μg L(-1) and within-laboratory reproducibility of all isomers below 20% at the minimum required performance limit level of 0.3 μg L(-1).     

A ruled residue theorem for function fields of conics

The ruled residue theorem characterises residue field extensions for valuations on a rational function field. Under the assumption that the characteristic of the residue field is different from 2 this theorem is extended here to function fields of conics. The main result is that there is at most one extension of a valuation on the base field to the function field of a conic for which the residue field extension is transcendental but not ruled. Furthermore the situation when this valuation is present is characterised.     

基于DEMON线谱的轴频提取方法研究

目标的螺旋桨不同则轴频不相同。轴频是目标的特征之一,可以应用于目标识别当中。本文提出一种改进的高频噪声解调分析(DEMON)方法,能够得到具有明显线谱的DEMON谱;提出最大公约数算法,并给出提取轴频的具体步骤。海试数据实验结果验证了本文所提方法及算法的有效性和可行性。