中国三个不同富营养化湖泊沉积物中Cu、Zn赋存特征及其与营养盐的相关性分析

对太湖、南四湖、白洋淀三个不同富营养化湖泊沉积物进行采样,采用Tessier连续提取法,测定了3个湖泊表层沉积物中Cu、Zn两种重金属的赋存形态,并初步探讨了重金属各形态与沉积物及上覆水中营养盐的相关关系。结果表明,沉积物中重金属总量以白洋淀最高,太湖最低,但重金属污染程度为太湖＆gt;南四湖＆gt;白洋淀,太湖Cu污染指数为1.34~1.6,白洋淀Cu污染指数仅为0.79~1.17。沉积物中重金属赋存形态Cu主要以残渣态和有机质结合态为主（二者之和占73%以上）, Zn则以残渣态和Fe-Mn氧化态占优（二者之和比例达83%以上）,含量最少的均为可交换态。不同湖泊沉积物重金属赋存形态差异较大,太湖残渣态重金属占总量的比例最小（Cu为43%~56%,Zn为49%~63%）,南四湖残渣态占的比例最大（Cu为59%~82%、Zn为64%~77%）;可交换态比重在太湖中最高（Cu占3.2%~5.6%,Zn为1.3%~1.5%）,在南四湖中最低（Cu为1.1%~2.9%,Zn未检出）。从“非稳定态”重金属（除残渣态外的四种形态之和）所占比例看,相较其它两个湖泊,太湖沉积物中重金属污染人为输入的活性态占较大比重,具有较高的二次释放风险。相关性分析得出,重金属Cu的可交换态与上覆水中总氮及总磷之间存在着极显著的正相关关系,碳酸盐结合态Cu与沉积物中营养盐呈现出显著的负相关性,说明水体的富营养化程度加剧可能会增强沉积物中Cu向水体释放的风险。     

Determination of 4-nonylphenol in carp blood samples by solid phase extraction and chromatographic techniques

In this study, selective methods were developed for isolation, purification, separation and determination of 4-nonylphenol (4NP) in biological samples. Several methods such as high-performance liquid chromatography (HPLC) with fluorescence and diode array detection and gas chromatography coupled to mass spectromotry (GC-MS) are described for the simultaneous determination of 4NP. The nonylphenols in the plasma of fish were extracted through solid phase process by using octadecyl, polymeric and octadecyl endcapping sorbents. The average recoveries in plasma samples spiked with 4NP of levels 1?µg?mL^?1 were between 80–95% using added surrogate standards. The aim of this study was to determine whether trace amounts of 4NP in fish plasma samples could be detected by solid phase extraction and chromatographic methods (HPLC, GC-MS). This technique of monitoring the levels of endocrine-disruptors in plasma samples is consistent, reliable as well as inexpensive.     

Polycyclic aromatic hydrocarbons in medicinal plants from Syria

The levels of 16 US Environmental Protection Agency polycyclic aromatic hydrocarbons (EPA PAHs) in 10 medicinal plants in different used parts of plant (leaves and flowers) have been determined. The analytical method consists of sample preparation by ultrasonic extraction with dichloromethane followed by silica gel clean-up. Subsequently, the analysis was carried out by reversed-phase high-performance liquid chromatography (HPLC) coupled to both ultraviolet and fluorescence detections in series to insure the detection of all 16 EPA PAHs. It was observed that the sum of the 16 PAHs (ΣPAHs) in the investigated medicinal plants ranged from 47 to 890 μg kg^–1 where the highest ΣPAHs was found in Sage plant sample. Light PAHs were dominants in all studied medicinal plants. The sum of eight genotoxic PAHs (ΣPAH8) have shown a better indicator of the degree of contamination with carcinogenic PAHs compared to benzo[a]pyrene in these products.     

Rapid liquid chromatographic analysis of Metoclopramide in pharmaceutical preparations

A sensitive, accurate and reproducible method for the analysis of metoclopramide, a gastrointestinal drug, has been described. An isocratic HPLC elution method was employed which requires about 10 minutes to be performed. The concentration of metoclopramide hydrochloride preparations was found to be 95.1 ±0.3% and 94.21 ±0.25% in tablet and injection formulations, respectively.     

The estimation of bioconcentration factors of aromatic hydrocarbons by high‐performance liquid chromatography

The determination of Bioconcentration Factors (BCF) via HPLC capacity factors (k') has been studied, including the effect of column type and mobile phase composition on the correlation between log BCF and log k’. Values of BCF correlate well with the phenylsilica column capacity factors. The phenylsilica column followed by C18 column give better correlations than either C8 or C2 column. The use of HPLC with phenylsilica as stationary phase and methanol‐water as mobile phase in the prediction of BCF can be at least as good or better than the use of n‐octanol/water partitioning system. There are no significant differences in the correlations between log k’ and log BCF with the changes of methanol concentration in the mobile phase, and it seems that a high proportion of methanol in the eluent is required to obtain good results.     

Evaluation of linear alkylbenzenesulfonate (LAS) biodegradability in sediment by solid‐phase extraction and HPLC analysis

The linear alkylbenzenesulfonate (LAS) sorption on environmental sediments has been known long ago. Their high concentrations reflect the massive input of these chemicals from household and industrial uses. However few attempts were made to identify biodegradation metabolites of LAS in sediment. In this report, a method for the determination of these compounds in sediment samples by high‐performance liquid chromatography (HPLC) is described. The first step of our work was performed by solid‐phase extraction with octadecyl‐bonded silica (C18) mini‐columns and provided a suitable recovery of LAS (90 ± 5%) and most metabolites. Furthermore, laboratory investigations led to study the behaviour of LAS in sediment. The environmental samples used for this purpose were collected from a pond (named étang de Bolmon) located in the French Mediterranean coast. Our results were in agreement with an aerobic biodegradation process of LAS that occurred only with high values of sediment redox potential and needed the samples to be vigorously shaken to ensure adequate mixing and suspension of particulate material. In a stagnant sediment or under anaerobic conditions, LAS is not degraded. p‐Sulfophenylacetic acid and p‐sulfocinnamic acid were evidenced as predominant metabolites and were found not to be persistent.     

离子液体分析方法研究进展

离子液体(ILs)由于挥发性小和化学稳定性高常称为绿色溶剂而得以广泛生产与应用.同时由于水溶性高和难降解可能给水生生物带来潜在危害,已逐渐引起广大环境化学工作者的关注.如何有效地分离分析ILs是研究其迁移、转化等环境行为及生物毒性的首要问题.为此,本文系统论述了反相液相色谱法、离子对-反相液相色谱法、极性-反相液相色谱法、离子色谱法、毛细管电泳及等速电泳等方法分析ILs的研究进展,分析了各个方法的优缺点和适用对象,展望了ILs分离分析发展的未来趋势.     

高效液相色谱-荧光检测法同时测定畜禽粪便中4种磺胺类药物残留

建立了高效液相色谱-荧光检测法测定畜禽粪便中4种磺胺药物(磺胺甲基嘧啶(SM1)、磺胺氯哒嗪(SCP)、磺胺邻二甲氧嘧啶(SDM’)、磺胺喹噁啉(SQ))的方法.样品用25 mL甲醇提取3次,合并提取液,浓缩干燥,用0.1 mol.L-1的HCL溶解残渣,经荧光胺衍生化后,用反相C18柱为分离柱,以乙腈∶0.5%乙酸=40∶60(V/V)为流动相进行洗脱,20 min内分离4种药物.在0.05—5.00μg.mL-1范围内,4种磺胺类药物的峰面积与质量浓度的线性关系良好(R2≥0.999),SM1、SCP、SDM’、SQ的定量限(LOQ)分别为2.3、6.3、4.3和9.6μg.kg-1;添加水平为50、100、1000μg.kg-1时,SM1、SCP、SDM’、SQ的回收率分别为74.91%—81.82%、78.45%—91.43%和86.10%—92.88%,RSD小于8.82%.     

硝基化合物的高效液相色谱(HPLC)分析

硝基化合物是炸药废水的主要成分,大部分硝基化合物具有较高的毒性.本文对奥克托今、黑索今、1,3,5-三硝基苯、1,3-二硝基苯、硝基苯、2,4,6-三硝基甲苯、2-氨基-4,6-二硝基甲苯、2,4-二硝基甲苯共8种硝基化合物的紫外光谱和液相色谱分离条件进行了研究,其最佳检测波长分别为228 nm、227 nm、227 nm、237 nm、272 nm、230 nm、226 nm、244 nm.本文建立了8种硝基化合物的高效液相色谱测定方法,色谱条件为:色谱柱为ZORBAX SB-C18(3.0 mm×250 mm,5μm),检测器为紫外检测器,流动相为甲醇-水(50∶50),流速为0.5 mL.min-1.水中8种硝基化合物可以在13 min内得到较好的分离,检出限均≤0.8 ng,回收率大于95%.     

氯化对二级处理出水中溶解性有机物结构的影响

以哈尔滨市W污水处理厂污水为研究对象,利用XAD树脂对二级处理出水中的溶解性有机物(DOM)进行分级分离.按照DOM在不同树脂上的吸附特性将其分为5个部分:疏水性有机酸(HPO-A)、疏水性中性有机物(HPO-N)、过渡亲水性有机酸(TPI-A)、过渡亲水性中性有机物(TPI-N)和亲水性有机物(HPI).考察了二级处理出水中有机组分的组成分布、三卤甲烷生成势、紫外光谱和红外光谱.结果表明,二级处理出水中的主要成分是HPO-A和HPI,两者含量之和达70.8%.HPO-A是加氯消毒时产生三卤甲烷的主要有机组分,其三卤甲烷生成活性(STHMFP)为232.9μg/mg.而HPO-N、TPI-A、TPI-N和HPI的STHMFP介于100～125μg/mg之间.氯化反应后,HPO-A、HPO-N、TPI-A和HPI的紫外-可见吸光度均降低,而TPI-N则相反.并且HPO-A、HPO-N、TPI-A和TPI-N中的O-H、C=C和苯环的含量降低,而C-O的含量升高,还生成了C=O和C-Cl.