Green pre-concentration techniques during pesticide analysis in food samples

The ever-increasing demand for determining pesticides at low concentration levels in different food matrices requires a preliminary step of pre-concentration which is considered a crucial stage. Recently, the parameter of “greenness” during sample pre-concentration of pesticides in food matrices is as important as selectivity in order to avoid using harmful organic solvents during sample preparation. Developing new green pre-concentration techniques is one of the key subjects. Thus, to reduce the impact on the environment during trace analysis of pesticides in food matrices, new developments in pre-concentration have gone in three separate directions: the search for more environmentally friendly solvents, miniaturization and development of solvent-free pre-concentration techniques. Eco-friendly solvents such as supercritical fluids, ionic liquids and natural deep eutectic solvents have been developed for use as extraction solvents during pre-concentration of pesticides in food matrices. Also, miniaturized pre-concentration techniques such as QuEChERS, dispersive liquid–liquid micro-extraction and hollow-fiber liquid-phase micro-extraction have been used during trace analysis of pesticides in food samples as well as solvent-free techniques such as solid-phase micro-extraction and stir bar sorptive extraction. All these developments which are aimed at ensuring that pesticide pre-concentration in different food matrices is green are critically reviewed in this paper.     

8-羟基喹哪啶固相萃取光度法测定生物样品中的钴

研究了8-羟基喹哪啶与钴的显色反应,在pH为8.0的氯化铵—氨水缓冲介质中,乳化剂-OP存在下,8-羟基喹哪啶与钴反应生成3∶1稳定的蓝紫色配合物,该配合物可被Waters Plus-C18固相萃取小柱萃取富集,小柱上富集的配合物用乙醇为洗脱剂洗脱后用光度法测定,在乙醇介质中,配合物最大吸收波长λmax为595 nm,ε为7.82×103L.mol-1.cm-1。钴含量在0.1~5.0 mg/L内符合比耳定律,方法用于生物样品中痕量钴的测定,结果令人满意。     

Comparison of in-house-developed ELISA with HPLC techniques for the analysis of atrazine residues

In-house developed ELISA was standardized to monitor atrazine residues in different environmental samples. The standard curve was linear, indicating an increase in log concentration with decrease in absorbance (%B/B₀ = 1.075–0.042 Log C; r = ?0.966). The middle of the test was at 75 ng/L and the lowest detection limit at 4 ng/L. ELISA significantly correlated with the high performance liquid chromatography (HPLC) (r = 0.990). Internal validation showed good accuracy and precision. Maximum atrazine residues were present in Jehlum River water/sediments and maize/sugarcane plant roots. Most of the food samples were found to be contaminated. ELISA required less clean-up steps than HPLC, but showed matrix effect in soil/colored extracts.     

A sensitive enzyme‐linked immunosorbent assay amplified by biotin–streptavidin system for detecting non‐steroidal anti‐inflammatory drug ketoprofen

A sensitive biotin–streptavidin‐amplified enzyme‐linked immunosorbent assay (BA‐ELISA) method was developed for detecting non‐steroidal anti‐inflammatory drug ketoprofen. Compared with traditional ELISA method, the sensitivity of proposed immunoassay was enhanced by the biotin–streptavidin system. Under the optimal condition, the median inhibitory concentration (IC₅₀) was 0.25 ng mL^?1, with minor cross‐reactivity to a number of structural analogs. This developed assay was successfully applied to detect the ketoprofen residues in different fish samples, and good recoveries (72.6–105.5%) were obtained. The results indicated that this immunoassay method could specifically detect trace ketoprofen residues and could be widely used for routine monitoring of food samples.     

辐射热流作用下树叶样品的燃烧特征研究

研究植物叶样在外部热辐射和值班火源作用下的燃烧现象特征并探索其成因和物理及化学本质。采用锥形量热仪开展实验,热辐射强度分别设定为35kW m-2、55kW m-2、70kW m-2和85kW m-2。实验样品为针阔叶树种共13种,其含水率在45%至79%间变化。实验表明,样品表现出不同的着火模式,有的为明火,有的则为阴燃,取决于树种和设定的辐射强度。样品出现有焰燃烧现象的最低热释放速率峰值(PHRR)在22.3kW m-2至35.6kW m-2之间,反映了形成气相火焰所需最低挥发分质量流率。气相产物CO2产生速率的峰值与PHRR呈高度线性性,表明了不同样品间气相燃烧或固相表面氧化(阴燃燃烧)反应的相似性。进一步分析表明,出现的独特热释放速率尖锐峰形是样品分层特性以及树叶的物理属性和热物性共同作用的结果。具有热薄特性的样品表层,在实验初期是接受外部辐射热的主体,其热解的产物是形成气相火焰的物质来源;在其转变为焦炭层后,对辐射热流向内层的渗透具有阻挡作用。建立起来的认识对于评估分层样品的燃烧性有一定的指导意义。     

Selective and sensitive extractive spectrophotometric determination of micro amounts of palladium(II) in spiked samples: using a new reagent N-ethyl-3-carbazolecarbaxaledehydethiosemicarbazone

N-Ethyl-3-cabazolecarboxaldehydethiosemicarbazone (ECCT) is proposed as a new, sensitive and selective complexing reagent for the separation and extractive spectrophotometric determination of palladium(II) at pH: 4.0 to form a yellowish orange colored 1:1 chelate complex, which is very well extracted in to n-butanol. The absorbance was measured at a maximum wavelength, 410 nm. This method obeys Beer’s law in the concentration range 0.0–6.6 μg mL⁻¹ and the correlation coefficient of Pd(II)-ECCT complex is 0.998, which indicates an excellent linearity between the two variables with good molar absorptivity and Sandell’s sensitivity, 1.647 × 10⁴ l mol⁻¹cm⁻¹, 6.49 × 10⁻³ μg cm⁻², respectively. The instability constant of complex calculated from Edmond’s method, 2.724 × 10⁻⁵ was in good agreement with the value calculated from Asmus’ method 2.624 × 10⁻⁵, at room temperature. The precision and accuracy of the method is checked with calculation of relative standard deviation (n = 5), 0.839. Edmond’s method was observed to be a more selective method in the presence of EDTA, oxalate and phosphate ions. The method was successfully applied for the determination of Pd(II) in water samples, synthetic mixtures and hydrogenation catalysts, employing an atomic absorption spectrometer for comparing these results.     

A Comparison of the Precipitation Chemistry Measurements Obtained by the CAPMoN and NADP/NTN Networks

Precipitation chemistry measurementsobtained by the Canadian Air and PrecipitationMonitoring Network (CAPMoN) and the U.S. NationalAtmospheric Deposition Program/National Trends Network(NADP/NTN) have been examined using more than 7 yrof collocated data from two sites, namely, Sutton,Quebec, Canada and State College, Pennsylvania, U.S.A.In the case of the CAPMoN data, weeklyprecipitation-weighted mean concentrations, totalsample depths and total standard gauge depths werecomputed from daily data and compared to thecorresponding weekly sampling data of the NADP/NTNnetwork. Seasonal and annual precipitation-weightedmean concentrations and deposition values were alsocomputed for both networks and compared. Statisticallysignificant between-network biases were found to existin the weekly results for most of the measuredvariables, particularly standard gauge depth, sampledepth, pH, H⁺, NO₃ ^-,NH₄ ⁺,Na⁺; the NADP/NTN values were consistently lowerthan those of CAPMoN with the exception of pH andNa⁺. The magnitude of the biases was less than35% of the median CAPMoN weekly value for the 7 yr. For most of the measured parameters, thevariability of the between-network differencesrepresented less than 20% of the median CAPMoN weeklyvalue. Both the between-network biases andvariabilities were functions of several physicalparameters, the most dominant being the sample depthand the ionic concentration. For seasonal and annualdeposition values, statistically significantbetween-network biases were found for H⁺,SO₄ ^2-, NO₃ ^-,Ca²⁺,NH₄ ⁺ for both periods; for Mg²⁺ andK⁺ for seasonal data; and Cl^- for yearlydata, with the NADP/NTN deposition values being lowerthan those of CAPMoN. The relative biases ranged from7 to 37%. Part of the between-network bias in thedeposition estimates was directly attributable to astrong bias in the standard gauge depths of the two networks.     

离子色谱法测定水中无机阴离子水样的预处理

本文介绍了用离子色谱法测定无机阴离子，对污染严重的水样通常采用预处理柱法。论述了预处理柱的制备、再生，测定了预处理柱对重金属及有机物的去除率及无机阴离子的回收率。     

环境水样中双酚A的HPLC检测探讨

研究探讨了各种水化学条件（pH值、离子强度、共存阴离子、共存有机质）对高效液相色谱法（HPLC）检测模拟环境水样中微量双酚A的影响.采用高效液相色谱法检测水样中双酚A的标准曲线线性相关系数高（R2 ＞0.999）,在0.1～5 mg/L的双酚A浓度范围内呈现线性.本研究采用的高效液相色谱法可以在pH 2～11、离子强度0.02 mol/L到2 mol/L NaCl范围内有效地检测双酚A;溶液中的共存阴离子N03-、S04-或共存有机质葡萄糖、单宁酸、没食子酸对检测并没有明显影响;然而当溶液中存在CO32-和p034-时,本研究采用的高效液相色谱法将无法有效检测双酚A,应用时需注意.     

关于固相萃取技术富集水中苯系物的探讨

苯系物尤其是苯、甲苯和二甲苯作为重要溶剂和基本化工原料,被广泛应用于油漆、农药、医药、有机化工等行业,由此而产生的废水、废气便成为河流、空气和地下饮用水等有机污染物的重要来源。除苯是已知的致癌物以外,其它几种化合物对人体和水生生物均有不同程度的毒性。在我国水环境中优先控制污染物黑名单中,苯、甲苯、乙苯及二甲苯的三种异构体均榜上有名。因此,测定水中苯系物含量对环境保护具有重要的意义。本文基于固相萃取（SPE）技术富集水样中苯系物的思路,选择苯、甲苯、乙苯、对二甲苯、邻二甲苯、苯乙烯和异丙苯作为目标化合物,对C18键合相吸附剂富集水中苯系物的吸附和脱附过程的参数优化进行了研究,为建立一种简便、高效的水中苯系物的检测方法提供了依据。