HPLC-FLD测定水中联苯胺的方法研究

探讨了利用液相色谱分离,荧光检测器测定地表水中联苯胺的可行性。前处理方法对比验证了液液萃取法和固相萃取法。水样在碱性条件下(pH=11~12)进行提取,当提取体积为1.0 L时,液液萃取液相色谱荧光法检测,方法检出限为1.4 ng/L,定量下限为5.5 ng/L;固相萃取液相色谱荧光法检测,方法检出限为0.9 ng/L,定量下限为3.6 ng/L。分别对地表水、生活废水、工业废水3种不同水体进行基体加标试验,加标浓度为10.0、40.0、80.0 ng/L。结果显示,对于3种不同基体和不同加标浓度的水样,两种方法均有较好的准确性和重现性,方法回收率为80%~120%,相对标准偏差均小于20%,满足《地表水环境质量标准》(GB 3838—2002)中对联苯胺的监测需求。     

大体积进样技术结合同位素稀释法测定地表水中多环芳烃的研究

采用C18固相萃取柱预处理水样,由于固相萃取柱的选择吸附性,净化了样品的基质;同液-液萃取相比,固相萃取柱和硅胶小柱的双重净化,更适合大体积进样。萘、苊、菲、屈艹的氘代化合物作为同位素稀释剂,由于待测分析物与同位素稀释剂物理化学的相似性,其在固相萃取柱的保留行为和色谱运行行为都有基本一致性。同一般内标法相比,同位素稀释法具有较高的回收率。大体积进样由于进样绝对量的增加,降低了检出限。方法检出限0.05～0.1ng/L,回收率范围90%～110%。     

加速溶剂萃取气相色谱负化学离子源质谱法分析土壤中有机氯农药

通过优化萃取条件建立了一套土壤中有机氯农药的加速溶剂萃取方法;采用固相萃取实现了样品的净化,气相色谱负化学离子源质谱实现了高灵敏度检测,建立了一套土壤中19种有机氯农药的快速分析方法,各目标物的检出限为0.001～0.009μg/g,采用来自于不同地区的砂土、黏土、亚黏土等不同类型的样品进行加标实验,回收率为60%～120%。     

在线固相萃取-HPLC法测定公共绿地土壤中新烟碱类农药残留

土壤样品经二氯甲烷-乙腈混合溶液超声提取后,用PEP固相萃取柱在线净化,再用HPLC法测定样品中吡虫啉、啶虫脒、噻虫嗪、噻虫啉、烯啶虫胺等5种新烟碱类农药残留。通过优化试验条件,使该方法在0.01 mg/L~2.00 mg/L范围内线性良好,当取样量为3.00 g时,方法检出限为0.002 mg/kg~0.003 mg/kg。8种土壤样品3个质量比水平的加标回收率为72.5%~119%,RSD均低于9.6%。     

固相净化气相色谱法测定水产品中多种有机磷农药残留

建立了水产品中8种有机磷农药残留同时测定的方法,选择乙腈提取,ENVI-C18串联PSA固相萃取柱净化,经丙酮/正己烷混合溶液（体积比1∶1）洗脱,洗脱液氮吹浓缩后采用气相色谱外标法定量。8种有机磷农药在0.050 mg/L～1.00 mg/L范围内线性良好,检出限在1.8 μg/kg～2.5 μg/kg之间,3个添加水平加标样品平行测定的相对标准偏差为1.1%～5.7%,回收率为69.8%～116%。     

中空纤维膜萃取-气相色谱法测定水中有机氯农药

提出了中空纤维膜萃取-气相色谱法测定水中有机氯农药的方法。首先研究了8种有机氯农药的线性范围,然后测定了中空纤维膜萃取对水中有机氯农药的回收率,最后用中空纤维膜萃取-气相色谱法对实际水样进行检测。结果表明,8种有机氯农药在0.5~10μg/L范围内具有良好的线性关系,中空纤维膜萃取法对水中8种有机氯农药的富集倍数为389~464,回收率为77%~92%,可以满足分析要求。     

蕃茄转基因受体系统的研究

对蕃茄基因转化的受体系统进行了研究结果表明：在蕃茄离体子叶（或子叶切段）培养中,只加细胞分裂素（Zt或BA）即可使不定芽充分分化,而少量生长素对不定芽的分化反而有抑制作用;在所试验过的多种外植体中,以2／3子叶片处切割子叶所产生的外植体用作转化受体最好;不同蕃茄品种、同一品种的不同外植体及同一外植体的不同培养方式等均对转化频率有一定的影响;通过生长素短期刺激诱导,可解决转基因植物生很困难的问题．     

Determination of phenolic and steroid endocrine disrupting compounds in environmental matrices

BACKGROUND, AIM AND SCOPE: Many pollutants have received significant attention due to their potential estrogenic effect and are classified as endocrine disrupting compounds (EDCs). EDCs comprise many classes of organic compounds. The development or optimization of analytical protocols for the simultaneous determination of EDCs in environmental samples is an analytical challenge because these compounds exhibit different physicochemical characteristics, they occur in the aquatic environment in relatively low concentrations and, furthermore, environmental samples are considered as complex matrices. The aim of this study is the development of analytical methods for the simultaneous determination of phenolic and steroid EDCs in aqueous and solid samples. The target compounds are 4-nonylphenol, 4-octylphenol, their ethoxylate oligomers (mono- and di-ethoxylates of nonylphenol and octylphenol), bisphenol A, the estrogens (estriol, estrone, 17beta-estradiol, 17alpha-estradiol) and the synthetic steroids (mestranol and 17alpha-ethynylestradiol). MATERIALS AND METHODS: Solid phase extraction employing Oasis HLB cartridges and different elution solvents was used for the recovery studies of the target compounds from various types of water samples (ultrapure water, artificial seawater, river water and seawater). Ultrasonic assisted extraction was applied for the recovery of the target EDCs from the solid samples. The recoveries were assessed using various solvents for the extraction and the elution of EDCs from different SPE cartridges used for clean up. Gas chromatography-mass spectrometry after derivatization with N,O-bis(trimethylsilyl)-trifluoroacetamide was employed for the determination of these compounds. RESULTS AND DISCUSSION: The recovery rates of three elution solvents (methanol, acetone and ethylacetate) for the extraction of target EDCs from artificial seawater were assessed after preconcentration on SPE cartridges. Acetone showed better recoveries and was further tested for its extraction efficiency in different water types (river water, seawater). Ultrasonic assisted extraction was used for the recovery of target EDCs from solid matrices. Acetone, methanol, mixture of acetone-methanol (1:1) and ethylacetate were used as extraction solvents. Ethylacetate and the mixture of acetone-methanol (1:1) exhibited better extraction efficiencies. An additional clean up step was necessary for sediment samples. Different SPE cartridges were employed for clean up of the extracts (Oasis HLB, C18, Florisil, silica, combination of silica and alumina). Florisil cartridges were finally used. The proposed methods were further validated on the determination of target EDCs in field collected samples (river water, seawater, wastewater, total suspended solids and sediments) from the major area of Thessaloniki, Greece. CONCLUSIONS: Efficient and accurate integrated methods for the simultaneous determination of alkylphenols (nonylphenol, octylphenol), their ethoxylate oligomers (mono- and di-ethoxylate of nonylphenol and octylphenol), bisphenol A and steroids (estriol, estrone, 17beta-estradiol, 17alpha-estradiol, mestranol and 17alpha-ethynylestradiol) in aqueous and solid samples were developed. The proposed methods were applied for the determination of the target compounds in representative environmental samples in the area of Thessaloniki, Northern Greece. RECOMMENDATIONS AND PERSPECTIVES: This study confirms the occurrence of selected EDCs in inland and marine waters in the area of Thessaloniki, Northern Greece. Since there is no previous data on the occurrence of the target EDCs in the major area, an extended survey is in progress to evaluate the occurrence and fate of these compounds.     

城市内河生物修复及其对底泥氮素转化影响的实验研究

对在城市内河底泥有机质与有机氮含量高的特殊环境下进行水体修复的可行性与修复方法进行了探讨.富含高有机氮的城市内河底泥是氮素的重要释放源,采用向水体曝气可以有效地促使总氮与NH3-N的降解,与未曝气相比,10 d后曝气条件下二者的去除率分别达到81%和92%;此时再以土著水生植物进行修复可以显著地提高水体修复的效果、稳定性与修复成功率,并使总氮、NH3-N维持在1 ms/L和0.5 ms/L以下.但应避免城市内河有效光辐射的减少对水体修复影响.     

连续流动-固相微萃取方法富集水中多环芳烃的探讨

建立了连续流动-固相微萃取富集、气相色谱测定水中多环芳烃的方法,探讨了流量和溶液体积对萃取效果的影响。方法在0μg／L-40μg／L范围内线性良好,8种多环芳烃的检出限为0．05μg／L-0．5μg／L,样品测定的相对标准偏差〈7％,加标回收率为87．0％～112％。