紫杉醇原料药中有机溶剂残留量的气相色谱分析

对紫杉醇原料药中多种有机溶剂残留量,用气相色谱法同时进行了测定．提出该药品有机溶剂残留量测定的标准及方法,本法准确、灵敏、简便、快捷,为紫杉醇原料药质量标准的制定提供了实验依据．     

HCH residues in point-source contaminated samples of the Teltow Canal in Berlin,Germany

Contaminated groundwater and a riverine sediment core heavily affected by the same industrial point source were analysed for hexachlorocyclohexanes (HCH) and its degradation products. A detailed quantification by GC/MS revealed contamination levels up to 730 μg/L and 396 ng/g in sum for the water and sediment samples, respectively. The isomer pattern differed significantly in both compartments. The ground water samples were depleted in γ-HCH, whereas a significant loss of α-HCH was evident in the sediments as compared to the technical composition. The data obtained revealed interesting insights into the transformation behaviour and fate of HCH mixtures in anaerobic environmental compartments. In the affected groundwater system an ongoing microbial degradation was pointed out by the identification of indicative anaerobic metabolites. On the contrary in the sedimentary system a high environmental stability or rather a hindered degradation was observed as indicated by unaltered concentration levels as compared to production rates as well as by the absence of metabolites. Interestingly, the environmental fate of HCH in subaquatic sediments as well as in anaerobic ground water differs highly in contrast to the behaviour in anaerobic soil or surface water systems. Further on, it has to be stated, that the knowledge about the long-term behaviour of HCH residues in sedimentary material under anaerobic conditions is rather limited so far.     

长江南京段水体中7种苯胺类化合物的检测方法及生态风险评价

应用固相萃取结合高效液相色谱-串联质谱法,建立了同时测定环境水样中7种苯胺类化合物的检测方法.实验表明,以ZORBAX Eclipse Plus C18 (3.5μm,2.1×150mm)色谱柱为分离柱,乙腈-水(2mmol/L甲酸铵)为梯度洗脱的流动相,在电喷雾质谱正离子模式下,7min内可以分离目标化合物;在1~200μg/L浓度范围内,7种苯胺类化合物的峰面积与质量浓度的线性关系良好;添加水平分别为0.8、4.0、20.0mg/L时,目标化合物的平均回收率分别为68.5%~102.2%、71.4%~89.4%、62.0%~78.3%,相对标准偏差均小于6.9%;利用本方法对长江南京段平水期(2014.4)、丰水期(2014.8)和枯水期(2014.12)的14个采样点的环境水样进行检测,检出4-硝基苯胺、2,6-二乙基苯胺、3,4-二氯苯胺和4-异丙基苯胺4种苯胺类化合物,且4-硝基苯胺在3个时期14个采样点均能检出;风险商值法评估长江南京段水体中4-硝基苯胺的生态风险为低生态风险.     

The adsorption of PCBs to Yangtse River sediment

The adsorption of six PCB congeners to natural sediments from the Yangtse River was investigated. Experiments were conducted at different PCB concentrations to get the adsorption isotherm for each compound. Analytical determinations were carried out using gas chromato‐graphy with ECD detector. Results showed that the adsorption mechanism of PCBs on Yangtse River sediment fitted the best to the Langmuir adsorption model. It was also found that the adsorption rate decreased as the solubility increased or the octanol‐water partition coefficient decreased for each compound.     

Monitoring of drinking water treatment plants using ICP‐MS

More than sixty inorganic parameters were monitored in the Ter and Llobregat Drinking Water Treatment Plants (DWTPs) using ICP‐MS. Both DWTPs supply approximately four million inhabitants with water in Barcelona and neighbouring areas (NE Spain). The profile of inorganic parameters throughout the treatment process is similar in the Ter and Llobregat DWTPs. Sodium, K, Mg, Ca, Si, Cl^‐, SO₄ ^‐2, Li, Rb, Cs (only in the case of the Llobregat DWTP), Sr, Ba, B, Ti, Cr, V, Co, Ni, Zn, Cu, Sb, Mo, Pb and U were not removed from raw water. Consequently, no improvement was shown as regards the high salinity of Llobregat raw water which is related to the mining activities on the large salt deposits located in the upper part of the basin. However, P, Fe, Mn, Cu and As were removed during treatment. The results obtained reveal the suitability of ICP‐MS for inorganic water quality monitoring in DWTP.     

Determination of phenol,cresols and xylenols in workplace air using XAD‐2 sorbent cartridges

A method for sampling and analysis of phenolic compounds in workplace atmospheres using Amberlite XAD‐2 sorbent tubes has been laboratory and field tested. After extraction of the adsorbed phenols with methylene chloride, the concentrated extract was analyzed by capillary column gas chromatography coupled with a flame ionization detector or a mass spectrometer. For a 3L air sample, the method has a detection limit for phenol, cresols, alkyl‐substituted phenols and xylenols of 0.3 mg/m³ using gas chromatography with flame ionization detection (GC/FID) analysis and 0.07 mg/m³ using gas chromatography mass spectroscopy/selected ion monitoring GC‐MS/SIM. Evaluation tests conducted in the laboratory indicated recoveries >85% for a wide range of phenols, cresols, xylenols and other alkyl‐substituted phenols and resorcinol. Sampling conditions were established to ensure that no breakthrough occurred for a predetermined sample volume of three (3) liters even in humid atmospheres. Stability tests indicated that for storage of up to 2 weeks at 4°C, only resorcinol showed a significant reduction in sample recovery. The proposed method and NIOSH Method 3502 were compared for the determination of phenol concentrations in air samples collected at a plant processing phenolic resins. Phenol was positively identified in the XAD sample using GC‐MS/SIM and was detected at concentrations of 40–50% of the total phenols detected using NIOSH Method 3502. This difference is attributed to the airborne paniculate matter which is known to contain bisphenols that will contribute to the total phenolic content sampled in Method 3502, but not on the XAD sample.     

臭氧—生物活性炭工艺去除水中有机微污染物

在臭氧化的反应柱中填装陶粒滤料,构成了臭氧－陶粒→生物活性炭不深度净化流程,用该流程去除水中有机微污染物,ＣＯＤＭＮ去除率近近４０％,浊度和色度大大降低,色－质联机分析表明,原水中有机物由５８种降至３０种,潜在有毒有害物质由１３种减少到４种。     

GC/MS在监测甲胺磷工业废水中的应用

就甲胺磷工业废水监测中甲胺磷及其干扰组分进行了色谱分离及质谱定性分析,并以火焰光度检定量,用甲胺磷工业原油作为标准,圆满完成了甲胺磷工业废水的监测任务。     

UPLC-MS/MS测定地表水中总微囊藻毒素的快速前处理方法探究

为方便地表水中总微囊藻毒素(TMCs)的预警监测,探究提取MC-LR、MC-RR、MC-YR的不同快速前处理方法,建立同时测定3种TMCs的煮沸-过滤-UPLC-MS/MS法.该方法在0.006μg/L～50.0μg/L范围内线性良好,方法检出限为0.006μg/L～0.010μg/L,实际水样3个质量浓度水平的加标回...     

秸秆燃烧产生的颗粒物中有机示踪物的分析方法

针对秸秆燃烧产生的颗粒物建立了测定4种有机示踪物的GC-MS分析方法,着重讨论了柱前衍生反应的条件,通过条件实验确定了在样品中加入80-100μl BSTFA/TMCS作为衍生试剂,在70℃下反应2h的最佳反应条件.方法的检测限为0.042-0.260μg,精密度为2.7%-19.7%,加标回收率为60.3%-111%.应用本方法定量分析了小麦秸秆闷烧排放的细颗粒物中22种有机物的含量,其分布特征为糖类物质含量最高,其次为含-OCH3酚类和甾醇类物质,而烷醇类物质含量最低.