Determination of three endocrine disrupting chemicals,triclosan, 4-n-nonylphenol,and di-n-butyl phthalate using stir bar sorptive extraction in samples of different matrices

Three endocrine disrupting chemicals (EDCs), triclosan (TCS), 4-n-nonylphenol (4-n-NP), and di-n-butyl phthalate (DBP) were determined using stir bar sorptive extraction (SBSE) along with high-performance liquid chromatography/photodiode array detection (HPLC/DAD). Benzyl butyl phthalate was used as an internal standard. The targeted analytes could be rapidly determined with limits of quantification (LOQ) ranging from 4.1 (DBP), 10 (TCS), to 34 (4-n-NP)?µg?L^?1 in real samples such as bottled waters, personal care products, soaps, lotions, and urine. The results show that the developed analytical scheme is solvent-saving, efficient, and capable of fast screening samples for these common EDCs.     

SBSE-GC/MS法测定饮用水源水中7种多氯联苯单体

采用搅拌棒吸收萃取(SBSE)-溶剂解吸-气相色谱/质谱联用法测定饮用水源水中7种多氯联苯单体,优化了萃取和解吸条件。方法在5 ng/L~100 ng/L范围内线性良好(r≥0.979),7种多氯联苯单体的检出限为0.8 ng/L~3.4 ng/L(100 mL水样SBSE萃取2 h),加标10 ng/L时实际水样回收率为93.0%~116%。     

搅拌棒萃取-热脱附/气质联用法测定水中2-MIB和土臭素

采用搅拌棒萃取-热脱附/气质联用法测定水中2-甲基异莰醇和土臭素,优化了搅拌棒萃取和热脱附进样的条件。试验表明：两种目标化合物在1．00 ng/L～200 ng/L范围内线性良好,2-甲基异莰醇的相关系数为0．9993,土臭素的相关系数为0．9997,方法检出限分别为0．31 ng/L和0．15 ng/L;空白和实际样品的加标回收率为82．4％～116％,测定结果的RSD＜10％。     

搅拌棒吸附萃取-气相色谱-质谱联用测定海水中邻苯二甲酸酯

为了测定海水中痕量邻苯二甲酸酯,构建并优化了搅拌棒吸附萃取-气相色谱-质谱联用方法.选取邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯、邻苯二甲酸丁基苄基酯、邻苯二甲酸二(2-乙基己基)酯和邻苯二甲酸二辛酯这6种邻苯二甲酸酯作为研究对象,优化了萃取时间和解析时间等5种因素,通过回收率和相对标准偏差等对SBSE-GC-MS方法进行验证.结果表明,最佳萃取时间为2 h,最佳甲醇添加量为10%,最佳氯化钠添加量为5%,最佳解析时间为50 min,最佳解析溶剂为甲醇∶乙腈=4∶1(体积比).6种邻苯二甲酸酯的峰面积和质量浓度线性对应关系良好,相关性系数均大于0.997,检出限在0.25~174.42 ng·L-1之间,不同质量浓度的回收率均在56.97%~124.22%之间,相对标准偏差在0.41%~14.39%之间.在建立方法的基础上,测定了胶州湾主要河流入海口的样品,结果表明所有采样点均检出邻苯二甲酸酯,邻苯二甲酸二乙酯检出率为100%,质量浓度较大的污染物为邻苯二甲酸二丁酯、邻苯二甲酸丁基苄基酯、邻苯二甲酸二(2-乙基己基)酯和邻苯二甲酸二辛酯.     

New insights in analysing parasitoid attracting synomones: early volatile emission and use of stir bar sorptive extraction

Summary. It is well known that feeding by Pieris brassicae caterpillars on cabbage leaves triggers the release of volatiles that attract natural antagonists such as the parasitoid Cotesia glomerata. The temporal dynamics in the emissions of parasitoid attracting volatiles has never been elucidated in this system. In a time course experiment, caterpillar infested leaves attracted the parasitoid within one hour after infestation. At such an early stage of infestation, as much as fifty percent of the parasitoids flew towards the infested plant in a wind tunnel bioassay, while only five percent flew towards the non-infested control plant. Three hours after infestation and later, the response to the volatiles from the infested plant reached its maximum and then continued at a constantly high level for the remaining 14 hours of the experiment. Chemical analyses of volatiles collected from infested leaves at short time intervals during the first 24 hours identified a total of ten compounds, comprising green leaf volatiles, terpenoids, and a nitrile. Significant increase of emission within the first 5 hours following initial herbivory was detected for (Z)-3-hexen-1-ol, (Z)-3-hexen-1-yl acetate, cineole and benzylcyanide. Subsequently, a coupled bioassay-chemical analysis procedure was developed allowing for testing and analyzing the same sample for future identification of the bioactive compounds. This was achieved by using stir bar sorptive extraction for the analysis of solvent extracts of caterpillar-damaged leaves.     

搅拌棒吸附萃取技术在环境样品分析中的应用

搅拌棒吸附萃取(SBSE)是继固相微萃取(SPME)之后的又一种无溶剂的用于痕量有机物分离和浓缩的技术,其萃取涂层体积大,具有灵敏度高、检出限低、重现性好、不使用有机溶剂等优点。适用于环境样品中挥发性及半挥发性有机物的痕量分析。本文综述了SBSE在环境样品分析中的应用,以及该技术的应用展望。     

新型吸附搅拌棒被动采样器研制及应用——基于多壁碳纳米管的改性

结合传统被动采样器原理和新发展的吸附搅拌棒技术,研制了以多壁碳纳米管-聚二甲基硅氧烷(MWCTNs/PDMS)作为涂层的新型吸附搅拌棒被动采样器,并以苯酚(PhOH)、己烯雌酚(DES)和铅(Pb)作为目标污染物,考察被动采样器其吸附性能,优化其吸附条件.结果表明,与商业化PDMS涂层吸附搅拌棒被动采样器相比,含MWCTNs/PDMS涂层吸附搅拌棒被动采样器能更快达到吸附平衡时间、具有更大的饱和吸附容量.甲醇是PhOH和DES优良解吸剂,0.6mol/L HNO₃为Pb最优解吸剂.该新型被动采样器重复使用50次以上其解吸效率仍能达到70%以上,具有良好的稳定性和重复利用效果.