高效液相色谱-二极管阵列检测器测定邻苯二甲酸酯色谱条件优化

采用高效液相色谱-二极管阵列检测器对6种PAEs类物质进行测定,并对梯度洗脱条件、流速、检测波长等影响化合物色谱响应的关键参数进行优化。综合考虑样品测试效率、分析精度、实际样品中存在杂质干扰等因素,确定以乙腈-水为流动相进行梯度洗脱,洗脱0~11 min流动相乙腈-水梯度比例为50∶50,11 min后流动相调整为100%乙腈,各化合物均能完全分离;色谱分析流速为0.8 m L/min;PAEs的最佳吸收波长为225 nm。在优化的色谱条件下,6种PAEs的线性良好,相关系数均大于0.999 8,仪器检出限为0.08~0.12 mg/L,保留时间、峰面积的相对标准偏差分别为0.02%~0.60%、0.13%~0.86%。方法灵敏度较高,适合土壤等邻苯二甲酸酯含量较高基质样品的快速分析。     

高效液相色谱法测定水中的六种邻苯二甲酸酯研究

建立了高效液相色谱法测定水中六种邻苯二甲酸酯(邻苯二甲酸二甲酯、邻笨二甲酸二乙酯、邻苯二甲酸二丁酯、邻苯二甲酸二(2-乙基己基)酯、邻苯二甲酸二辛酯、邻苯二甲酸丁基苄酯)的检测方法.对水样中邻苯二甲酸酯的萃取条件和高效液相色谱分析条件进行优化,采用正己烷二次萃取,浓缩定容后分析,以乙腈-水为流动相梯度洗脱,紫外检测波长226 nm,16 min可将六种邻苯二甲酸酯分离出.方法的检出限为0.13μg/L ～0.37 μg/L,加标回收率为78.6％～118.5％,相对标准偏差为0.82％～2.17％,是一种理想的测定水中六种邻苯二甲酸酯的方法.     

“引江济太”过程中塑化剂类污染物的输入特征和环境健康风险评价

为了解"引江济太"过程中塑化剂类污染物对贡湖的输入特征,于2013年8月对14个采样点的7种邻苯二甲酸酯类化合物(PAEs)的浓度进行采样分析,并通过美国环保署(USEPA)推荐的方法,对其环境风险进行评价.结果表明:各采样点邻苯二甲酸二丁酯(DBP)和邻苯二甲酸二环己酯(DCHP)均有检出,除采样点10、11和12外,邻苯二甲酸二乙酯(DEP)也有检出,其余4种均未检出,长江引水经望虞河进入贡湖后,DEP、DBP和DCHP浓度均有不同程度的降低,且其最高浓度均出现在望虞河长江引水处(采样点1),说明在引水过程中长江水对望虞河有明显的PAEs输入,而贡湖锡东水厂DEP浓度高于贡湖其他采样点,南泉水厂DBP和DCHP浓度高于贡湖其他采样点,金墅湾水厂PAEs浓度总体处于较低水平.环境健康风险评价结果显示:DEP的最大非致癌风险值为3.91×10-8a~(-1),未超过国际组织规定范围,而DBP的最大非致癌风险值为1.17×10-5a~(-1),超过英国皇家协会RS规定的1×10-6a~(-1),但均对人体无明显非致癌危害.     

Pollution levels and characteristics of phthalate esters in indoor air of offices

The pollution status and characteristics of PAEs (phthalate esters) were investigated in indoor air of offices, and PAEs of both gas-phase and particulate-phase were detected in all the samples. The concentration (sum of the gas phase and the particulate phase) was 4748.24 ng/m³, ranging between 3070.09 and 6700.14 ng/m³. Diethyl phthalate, dibutyl phthalate, and di(2-ethylhexyl) phthalate were the most abundant compounds, together accounting for 70% of the Σ6PAEs. Dividing the particulate-phase PAEs into four size ranges (<2.5, 2.5-5, 5-10, >10 μm), the result indicated that PAEs in PM_2.5 were the most abundant, with the proportion of 72.64%. In addition, the PAE concentration in PM_2.5 correlated significantly with the total particulate-phase PAEs (R² = 0.85). Thus, the amount of PAEs in PM_2.5 can be estimated from the total amount of particulate-phase PAEs using this proportion. In a comparison between the offices and a newly decorated study room, it was found that pollution characteristics were similar between these two places. Thus, it is implied that the PAE concentration decreased by 50% 2 yr after decorating.     

Pollution levels and characteristics of phthalate esters in indoor air in hospitals

The concentrations of phthalate esters(PAEs) in Chinese hospitals were investigated by simultaneously determining concentrations of gas- and particle-phase PAEs. PAEs were detected in two third-class first-grade hospitals, two second-class first-grade hospitals, and a community health service center. Hospital drugstores had the highest concentration(24.19 μg/m3), which was 1.54 times that of newly decorated houses. The second highest concentration was found in the transfusion rooms, averaging 21.89 μg/m3; this was followed by the concentrations of PAEs in the nurse's workstations, the wards, and the doctor's offices, with mean concentrations of 20.66, 20.0, and 16.92 μg/m3, respectively. The lowest concentrations were found in the hallways(16.30 μg/m3). Of the six different kinds of PAEs found, major pollutants included diethyl phthalates, dibutyl phthalates, butylbenzyl phthalates and di(2-ethylhexyl) phthalates, comprising more than 80% of all PAEs present.Meanwhile, a comparison between different wards showed that PAE concentrations in the maternity wards were 1.63 times higher than in the main wards. Based on known health hazards, our results suggest that the PAEs seriously influence the health of the pregnant women and babies; therefore, it is of great importance to take the phthalate concentrations in hospitals into consideration. In addition, hospital indoor air was more seriously contaminated than the air of newly decorated houses.     

Pollution levels and characteristics of phthalate esters in indoor air of offices

The pollution status and characteristics of PAEs(phthalate esters) were investigated in indoor air of offices, and PAEs of both gas-phase and particulate-phase were detected in all the samples. The concentration(sum of the gas phase and the particulate phase) was4748.24 ng/m3, ranging between 3070.09 and 6700.14 ng/m3. Diethyl phthalate, dibutyl phthalate, and di(2-ethylhexyl) phthalate were the most abundant compounds, together accounting for 70% of the ∑ 6PAEs. Dividing the particulate-phase PAEs into four size ranges( 2.5, 2.5–5, 5–10, 10 μm), the result indicated that PAEs in PM2.5were the most abundant,with the proportion of 72.64%. In addition, the PAE concentration in PM2.5correlated significantly with the total particulate-phase PAEs(R2= 0.85). Thus, the amount of PAEs in PM2.5can be estimated from the total amount of particulate-phase PAEs using this proportion. In a comparison between the offices and a newly decorated study room, it was found that pollution characteristics were similar between these two places. Thus, it is implied that the PAE concentration decreased by 50% 2 yr after decorating.     

高效液相色谱-三重四级杆/复合线性离子阱质谱法测定饮用水中22种邻苯二甲酸酯

建立了一种同时测定饮用水中22种邻苯二甲酸酯(PAEs)的高效液相色谱-三重四级杆/复合线性离子阱质谱方法:饮用水样品经针头过滤器过滤,选用Biphenyl液相色谱柱进行分离,以含0.1%甲酸的水溶液和含0.1%甲酸的甲醇溶液为流动相,电离模式为电喷雾正离子,选用多反应监测触发增强子离子扫描模式进行检测。结果表明,22种PAEs的灵敏度良好,定量限为0.001～0.1 μg/L。配制浓度为0.1～100.0 μg/L的混标溶液进行进样分析,分析结果显示,22种PAEs在该范围内的线性关系良好,相关系数均大于0.995,方法的平均回收率为82.9%～108.9%,相对标准偏差为0.9%～11.2%。同时,使用增强子离子扫描谱图进行搜库匹配,定性准确性高。该方法适用于饮用水中PAEs的检测。     

南京某城市污水二级处理系统中酞酸酯类的分布及去除特征

以南京某城市污水厂污水和污泥中的酞酸酯类（PAEs）为研究对象，分别采用固相萃取-气相色谱-质谱联用（SPE—Gc．Ms）和超声提取．气相色谱．质谱联用（USE—GC—Ms）检测其中的优先控制污染物邻苯二甲酸二甲酯（DMP）、邻苯二甲酸二乙酯（DEP）、邻苯二甲酸二丁酯（DBP）和邻苯二甲酸单（2-乙基己基）酯（MEHP），研究其在厌氧／好氧（A／O）污泥处理过程中的分布特征及降解规律。研究结果表明，各类PAEs在该污水厂的污水和污泥中均有检出，二级处理出水中4种酞酸酯类物质的浓度在0．151—2．419μg／L。污水中4种酞酸酯的分布规律为MEHP〉DBP〉DMP〉DEP，污泥中4种酞酸酯的分布规律为MEHP〉DBP〉DEP〉DMP。该污水厂二级处理工艺对4种PAEs的去除效果较明显，去除效率DBP〉DEP〉DMP〉MEHP．     

集中式饮用水源地邻苯二甲酸酯类物质分布特征与健康风险评估

以某地区7个集中式饮用水源地为研究对象,采用固相萃取气相色谱-质谱法(SPE-GC-MS)对水体中16种邻苯二甲酸酯的分布特征和溯源进行了研究,并利用健康风险评估模型对水体PAEs进行了健康风险评价。结果表明:邻苯二甲酸二正丁酯、邻苯二甲酸二(2-乙基己基)酯、邻苯二甲酸二异丁酯和邻苯二甲酸二正辛酯在所有PAEs同系物中含量丰富,而所有样品均无邻苯二甲酸二(2-甲氧基)乙酯和邻苯二甲酸二戊酯的检出;二水厂和亨达水务断面Σ_(16)PAEs浓度最高,四水厂和五水厂断面Σ_(16)PAEs浓度最低;水体12种PAEs共提出3个主成分,揭示了91%的影响因子;层次聚类分析表明:7个采样断面聚为2类,分别代表了内河和长江水体。水体中PAEs的致癌风险值和非致癌风险值均远低于参考值,说明研究水体PAEs不会对居民构成致癌风险或其他明显的健康风险,但需加强该地区PAEs使用的规范与监管,强化末端处理,以规避风险。     

Production of soybean ethanol-based biodiesel using CaO heterogeneous catalysts promoted by Zn,K and Mg

This article focuses on the optimization of the production of fatty acid ethyl esters from soybean oil using CaO-based heterogeneous catalysts. Three different catalytic promoters were evaluated: Magnesium, zinc, and potassium. The reaction has evaluated the promoter content (promoter to calcium molar ratio), catalyst load, alcohol to oil molar ratio, and temperature. Response surface methodology (RSM) was used to evaluate the influence of each variable on the yield of biodiesel. The addition of K₂O or MgO in the catalyst has enhanced the yield in fatty acid ethyl esters, while the use of ZnO as a promoter was not successful.