A self-penetrating and chemically stable zinc (ii)-organic framework as multi-responsive chemo-sensor to detect pesticide and antibiotics in water

Guided by the self-penetrating features can improve the stability of metal organic frameworks (MOFs), an unprecedented 3D self-penetrated framework, {[Zn (tptc)_0.5(bimb)]·H₂O}_n ( NUC-6 , here NUC corresponding to North University of China), with 3D (4,4)-c {8⁶} net, was designed. Benefit from the high chemical stability and excellent luminescent property, NUC-6 can be act as an efficient multi-response chemo-sensor in detecting dichloronitroaniline pesticide and nitrofuran antibiotics in water with the detection limits are 116 ppb for DCN pesticide, 16 ppb for NFT antibiotic, and 12 ppb for NTZ antibiotic. Besides, the mechanisms of luminescence quenching were revealed from the viewpoint of internal filter effect (IFE) and photo-induced electron transfer (PET), implied by the optical spectroscopy and quantum chemical calculation. This work provides a promising strategy to design stable MOFs by improving the self-penetrating features and to expand their practical applications in the detection of organic pollutants in aqueous medium.     

甲基对硫磷的快速测定及电化学性质

研究了杀虫剂甲基对硫磷的电化学性质。在pH10．38的Bdtton—Robinson缓冲溶液中，采用微分脉冲溶出伏安法在悬汞电极上得到一个还原峰，峰电位为-0．5V(vs．Ag/AgCl)，本工作对实验条件进行了深入的研究，结合线性扫描伏安法等手段。研究了体系的电化学行为。实验表明，甲基对硫磷在汞电极上具有吸附性，电极反应具有不可逆性。该法用于水果及水样中甲基对硫磷残余量的测定，结果满意。     

毛细管气相色谱法测定中药中有机氯农药残留量

建立了江西省两种中药中有机氯农药残留量的气相色谱分析方法。样品以丙酮提取,在NaCl存在下,以正已烷进行液—液分配,提取液用H2SO4净化,采用DB—1701毛细管柱,GC—ECD检测有机氯农药残留量。最低检测限为1.0×10-3-5.0×10-3mg/kg,添加回收率为85.7%-115.2%,应用于实际样品中有机氯农药残留量的检测,获得了较为满意结果。     

2—（4,6—二甲基—2—嘧啶巯基）乙酰芳胺的合成及其生物活性的初步研究

许多乙酰芳胺类化合物具有优异的生物活性，例如除草剂苯噻草胺，可抑制细胞生长和分裂，防除稻田中禾本科杂草［１］；杀菌剂甲霜灵可防治作物霜霉病［２］。本文将具有多种生物活性的嘧啶基团引入到乙酰芳胺结构中［３］，合成下列１０个未见文献报道的标题化合物Ⅰ，通...     

Progress in the quality assurance of environmental trace organic analysis

An overview is given on the stepwise learning programmes undertaken to identify the main sources of error associated with the determination of the mandatory organic contaminants in the marine monitoring programmes. Details are given on the preparation and use of LRMs and CRMs to maintain analytical control and quantify the laboratory errors in relation to the measurement of changes in the environment.     

Voltammetric determination of mesotrione at hanging mercury drop electrode

A study of the electrochemical reduction of the mesotrione pesticide on a hanging mercury drop electrode (HMDE) was performed as a basis for the development of a sensitive analytical method for natural samples. The electrochemical characteristics of herbicide mesotrione dissolved in a phosphate buffer (pH 7.0) have been determined by means of electrochemical techniques such as cyclic voltammetry (CV) and differential pulse voltammetry (DPV) over a wide range of pH from 2.0 to 10.0. The experimental parameters, such as electrolyte type and its pH, pulse amplitude, and scan rate were optimized. The method was applied to the determination of the pesticide in a spiked soil samples. Using this method, a linear calibration curve for mesotrione was obtained up to the 0.1 μM range in pH 7 phosphate buffer solution with a detection limit (S/N = 3) of 50 nM. The method can be applied successfully to the determination of mesotrione in soils. The text was submitted by the authors in English.     

毛细管气相色谱法测定5种中草药中有机氯农药的残留量

建立了怀牛夕等 5种中草药中六六六及滴滴涕异构体含量的气相色谱分析方法。样品以石油醚 +丙酮在索氏提取器中提取 ,提取液以浓硫酸净化。采用SE 30弹性石英毛细管柱分离样品 ,GC ECD检测六六六、滴滴涕农药的残留量。方法的线性范围为 5 .7× 10 - 7～ 2 .8× 10 - 4μg ;最小检测量为 1.3× 10 - 1 4～ 2 .5×10 - 1 2 g ;加样平均回收率为 88.8%～ 99.1% ;RSD为 0 .9%～ 5 .3%。     

芳基汞化合物的性质研究——Ⅶ.邻位取代苯基氯化汞的质子分解反应

本文研究了邻位取代苯基氯化汞o-XC_6H_4HgCl(X=CH_3、H、Cl、Br、COOC_2H_5、NO_2)与HCl(NaI)在85％对氧陆圜水溶液中的质子分解反应,证明反应按S_El历程进行。视取代基不同,反应速度次序如下:CH_3>H>Cl>COOC_2H_5～Br>NO_2。从化学反应与紫外光谱的研究以及理论计算结果表明,p或π电子的邻位取代基对水原子有分子内配位,它对反应速度有重要影响。测定了15种p-、m-、o-取代苯基氯化汞在80％对氧陆圜水溶液中在40.0℃的质子分解反应的速度常数k_1,表明给电性取代基加速反应,吸电性取代基使反应减慢,这可以看作是反应中心在芳环上的芳基汞化合物的S_E1反应所具有的一个特点。     

固相微萃取/二氧化锡气体传感器联用技术对果蔬中有机磷农药残留的快速检测

研究了固相微萃取(SPME)和二氧化锡气体传感器的联用技术对果蔬中有机磷农药残留乐果、氧乐果、甲胺磷、乙酰甲胺磷、马拉硫磷、敌百虫等的快速检测。结果表明，在85℃下，解吸8min，二氧化锡气体传感器在2min内完成对有机磷农药残留的快速检测。零解吸时间测量的甲胺磷的动态响应曲线表明。SPME／二氧化锡气体传感器联用技术对分析SPME的解吸平衡非常有利。     

Determination of Organochlorine Pesticides in Sediments from Authie Bay Using Microwave Assisted Solvent Extraction

The aim of this study was to develop an analytical method to determine the organochlorine concentrations in sediments. Combination of Microwave assisted Solvent Extraction (MASE) and capillary gas chromatography with specific detection (electron capture detector) was a viable approach for the determination of pesticides in solid matrixes. In this study, MASE development was focused on the selection of a suitable extraction solvent for all the target analytes. MASE procedure was validated by comparison with conventional methods such as Soxhlet and sonication extraction. The proposed method was then applied to determine the organochlorine insecticides concentrations in samples from Authie Bay (France). Environmental water samples were analysed and five target analytes were detected in concentrations from 0.03 to 0.56 ng/g of dry sediment. These investigations showed the accumulation and the persistency of these products in sediments in spite of the fact they were banned a few decades ago.