畜牧业污水中大环内酯和拟除虫菊酯类驱虫剂物质的LCMSMS检测

采用无需衍生化的同相萃取为前处理手段,高效液相色谱-串联四极杆质谱联用技术(LCMSMS)为检测手段,在电喷雾电离正离子模式下,对澳大利亚畜牧业污水中常见的大环内酯和拟除虫菊酯两类共7种驱虫剂物质的残留,建立了一次进样下的有效快速分析方法.经一系列优化试验,确定了以50%丙酮+50%乙腈为洗提剂、每次4 mL共8 mL的洗提方法.结果表明,该固相萃取技术(SPE)的加标回收试验结果较好,各化合物的平均回收率为95.50%～108.00%,相对标准差范围为0.73%-8.82%.以含10mmoL/L醋酸铵、0.1%甲酸的超纯水和甲醇混合溶液为流动相,以准分子离子峰[M+NH_4]~+、[M+H]~+作为母离子的定量离子对,所建立的1～500 ng/mL范围内的8点校正曲线中.各物质的相关系数均高于0.998 0,定量限范围为0.03-2.47 ng/mL.实际样品测定时.不同处理流程中各化合物的残留浓度有较好地体现.     

河口区域反硝化作用研究进展

反硝化作用是河口区域去除NO-3的重要途径.其产物之一N2O是一种温室效应很强的温室气体.本文综述了河口区域反硝化作用在N元素生物地球化学循环过程中的重要作用,概述了不同测定反硝化速率的方法,并提出了各种方法的优缺点.总结了反硝化作用的影响因素:O2浓度,NO3-,有机质,温度,生物等.在这些因素的影响下,反硝化存在着区域性,季节性以及昼夜性差异.最后,提出了目前研究中存在的不足及发展方向.     

静态顶空进样气相色谱法测定水中CS2的研究

采用气相色谱法静态顶空进样,极性柱分离,ECD检测器检测,对CS2的测定进行了全面的实验.实验表明,本方法简单、快速,并且具有精密度好、准确度高和检出限低的特点,完全能够满足快速分析水中CS2的要求.     

石墨炉原子吸收法测定无铅汽油中铅

探讨了用石墨炉原子吸收法测定无铅汽油中的铅。系统地研究了测定波长、测定浓度对测定方法的影响。提出了高浓度石墨炉原子吸收法测定无铅汽油中铅的方法。铅的检出限为 0 .0 0 5 mg/L,相对标准偏差 ( RSD,n=1 1 )在 1 .9%～2 .0 %之间 ,加标回收率在 95 .5 %～ 99.5 %之间     

污染物总量控制中载体水流量的测定

示踪剂法测定河水流量是较为准确的办法 ,利用河流动力模型计算出示踪剂投放点 ,利用示踪剂投放量与测定浓度之间的关系可方便地获得河水流量结果     

环境监测中确定最佳点位的关键技术

环境监测网络设计的关键问题是确定最佳的环境监测点位 ,而最优的监测点位必须既能代表所在区域环境质量的平均水平 ,又能反映该区域环境质量的变化状况。为此提出一个兼容样本贴近与相似程度的统计量——近似度 ,不仅在理论上证明了其合理性 ,而且在厦门的应用中得到满意的结果 ,从而解决了如何确定环境监测中最佳点位的问题     

紫外分光光度法测定水中硫酸盐的探讨

紫外分光光度法测定水中微量硫酸盐,具有简便、快速、灵敏等优点,适用于清洁环境水样的分析,回收率为96％－110％,其分析指标符合水质分析要求。     

Rapid determination of phenolic compounds in water samples by alternating-current oscillopolarographic titration

A rapid, simple and sensitive method was demonstrated for the determination of phenolic compounds in water samples by alternating-current oscillopolarographic titration. With the presence of sulfuric acid, phenol could be transferred into a nitroso-compound by reacting with NaNO2. The titration end-point was obtained by the formation of a sharp cut in the oscillopolarographic with infinitesimal NaNO2 on double platinum electrodes. The results showed that phenol concentration had an excellent linear relationship over the range of 4.82×10-6-9.65×10-3 mol/L, the RSD of the proposed method was lower than 1.5%, and the spiked recoveries of three real water samples were in the range of 95.6%-106.9%.     

Dechlorination of carbon tetrachloride by the catalyzed Fe-Cu process

The electrochemical reduction characteristics of carbon tetrachloride (CT) were investigated using cyclic voltammetry in this study. In addition, the difference in reduction mechanisms of CT between Master Builders' iron and the catalyzed Fe-Cu process was discussed. The results showed that CT was reduced directly on the surface of copper rather than by atomic hydrogen produced at the cathode in the catalyzed Fe-Cu process. The reduction was realized largely by atomic hydrogen in Master Builders' iron. The entire CT in 350 ml aqueous solution with 320 mgL was reduced to trichloromethane and dichloromethane in 2.25 h when 100 g of scrap iron with FeCu ratio of 10:1 (ww) were used. Moreover, the reduction rate slowed with time. CT could be reduced at acidic, neutral and alkaline pH from solution by Fe-Cu bimetallic media, but the mechanisms were di?erent. The degradation rate was not significantly in?uenced by pH in the catalyzed Fe-Cu process; in Master Builders' iron it clearly increased with decreasing pH. The kinetics of the reductions followed pseudo-first order in both cases. Furthermore, the reductions under acidic conditions proceeded faster than that under the neutral and alkaline conditions. The catalyzed Fe-Cu process was superior to Master Builders' iron in treating CT-containing water and this advantage was particularly noticeable under alkaline conditions. The reduction was investigated in the cathode (Cu) and anode (Fe) compartments respectively, the results showed that the direct reduction pathway played an important role in the reduction by the catalyzed Fe-Cu process. The catalyzed Fe-Cu process is of practical value.     

Germline mosaicism complicates molecular diagnosis of Lesch–Nyhan syndrome

A healthy female with a brother suffering from Lesch–Nyhan syndrome was assigned a carrier status on the basis of haplotype analysis employing flanking and intragenic polymorphic markers of the HPRT gene. Her mother has been confirmed as a definite carrier by cell growth selection studies in cultured fibroblasts. In our proposita's first pregnancy, a male fetus was identified carrying the risk allele. Afterwards, the underlying novel mutation A161E (GCA→GAA at position c482) could be identified in the affected brother and in the heterozygous mother but not in the DNA of the pregnant sister and fetus. The fetus was also confirmed to be normal by uptake of 14C-hypoxanthine in cultured amniotic cells. To test the discrepancy, the investigation was extended by recruiting additional family members. The data obtained showed that the mother had passed her risk haplotype to the affected son as well as to her mutation-carrying and non–mutation-carrying daughters. This provides the first evidence of concomitant somatic and germline mosaicism in Lesch–Nyhan syndrome. The study has a bearing on genetic counselling and cautions against the reliability of only using indirect genetic diagnosis even with intragenic markers. Copyright © 2004 John Wiley & Sons, Ltd.