Capillary zone electrophoretic determination of hydroxymetabolites of atrazine in potable water using solid-phase extraction with Amberchrom resins

A CZE-separation system for hydroxyatrazine, desisopropylhydroxyatrazine, desethylhydroxyatrazine and ammeline is presented that allows their determination in environmental waters in the subgL^–1 domain after solid-phase extraction/enrichment with styrene-divinylbenzene and methacrylate macroporous (Amberchrom) resins. The CZE separation and determination system uses the stacking effect and an increased light path for UV-detection (bubble cell). The etching of the bubble cell was done in our laboratory. A ruggedness check of the CZE-system revealed the resolution of theN-dealkylated metabolites to be sensitive to pH, temperature and current variations as well as to changes of capillary dimensions. Fine-tuning of the separation is performed by variation of the current intensity in the constant-current mode. Recoveries from fortified tap-water samples were 95% for hydroxyatrazine, 70% for desethylhydroxyatrazine and approximately 20% for desisopropylhydroxyatrazine at the 0.2 g L^–1 concentration level. Due to its high polarity, ammeline is only slightly adsorbed on Amberchrom resins and cannot be enriched using these materials.     

活性炭吸附处理高盐农药废水的研究

采用活性炭吸附预处理后的莠去津农药废水中的有机物,研究了活性炭种类、溶液pH值、盐含量对吸附的影响,测定了吸附等温线,并探讨了活性炭的再生性能.结果发现:pH值小于3时粉状木质活性炭对农药废水的吸附效果最好;废水中的盐含量越高,越有利于吸附;Freundlich模型比Langmuir模型能更好地拟合吸附等温线,pH值为3时的最大吸附量为250 mg/g.碱液可以将吸附在活性炭上的有机物解吸下来,再生后活性炭的吸附量可达到新鲜活性炭的98%以上.     

Label‐Free Colorimetric Detection of Trace Atrazine in Aqueous Solution by Using Molecularly Imprinted Photonic Polymers

Based on the combination of colloidal‐crystal templating and a molecular imprinting technique, a sensor platform for efficient detection of atrazine in aqueous solution has been developed. The sensor is characterized by a 3D‐ordered interconnected macroporous structure in which numerous nanocavities derived from atrazine imprinting are distributed in the thin wall of the formed inverse polymer opal. Owing to the special hierarchical porous structure, the molecularly imprinted polymer opals (or molecularly imprinted photonic polymer; MIPP) allow rapid and ultrasensitive detection of the target analyte. The interconnected macropores are favorable for the rapid transport of atrazine in polymer films, whereas the inherent high affinity of nanocavites distributed in thin polymer walls allows MIPP to recognize atrazine with high specificity. More importantly, the atrazine recognition events of the created nanocavities can be directly transferred (label‐free) into a readable optical signal through a change in Bragg diffraction of the ordered macropores array of MIPP and thereby induce color changes that can be detected by the naked eye. With this novel sensory system, direct, ultrasensitive (as low as 10^?8 ng mL^?1), rapid (less than 30 s) and selective detection of atrazine with a broad concentration range varying from 10^?16 M to 10^?6 M in aqueous media is achieved without the use of label techniques and expensive instruments.     

莠去津吸附的土壤淋溶柱色谱法研究

采用新发展的土壤淋溶柱色谱法,研究农药在水－土壤体系中的吸附。用土壤装填成液相色谱柱,以农药水溶液为流动相,以除草剂莠去津（２－氯－４－乙胺基－６－异丙胺基－ｓ－三嗪）为例,质量浓度从１９．７３μｇ／Ｌ至２９．６０ｍｇ／Ｌ,紫外检测器监测吸附平衡。吸附相中莠去津的质量浓度经甲醇淋洗液的测定值扣除柱内液相中的质量浓度后得到。对于极稀溶液,可采用在ＯＤＳ柱上富集－液相色谱台阶梯度法测定。莠去津在沙壤土上的吸附行为符合Ｆｒｅｕｎｄｌｉｃｈ方程式,其吸附常数Ｋｆ＝８４２．６ｍＬ／ｋｇ。     

阿特拉津降解细菌的直接检测及分离

摘要：利用改良的 SM固体培养基,对受除草剂污染的土壤中阿特拉津降解菌进行了检测、计数及分离。研究发现,在工业污染土壤中,阿特拉津降解菌群成为微生物群落的主要组成部分,而在农业土壤中仅占次要地位。用多重PCR分析了靶向基因trzN 和 atzABC,表明含trzN-atzBC基因组合的降解菌在山东省工业及农业土壤中占主导地位。因为富集偏差的消除,直接分离方法更利于阿特拉津降解菌多样性分析的研究。     

珍珠岩-磷酸化聚乙烯醇生物材料的制备及其降解阿特拉津特性

 阿特拉津因其普遍性、高污染性和难降解性一直是历年来的研究热点.其降解方法很多,其中基于阿特拉津降解菌、生物固定化和一些无机材料的生物降解是最有效的.本文利用磷酸交联剂对聚乙烯醇(PVA)进行改性,以珍珠岩作为添加介质,对阿特拉津降解菌——Pseudomonas W4包埋固定,制备出一种新型珍珠岩-磷酸化聚乙烯醇(PPVA)生物活性材料(简称珍珠岩-PPVA),并对其最佳制备条件以及在不同反应条件下该材料降解阿特拉津的效果进行探讨.该材料最佳制备条件为,珍珠岩(粒径为0.60~2.00mm)/10% PVA(V/V)=35/65,Pseudomonas W4包埋量1.0g/L,磷酸盐浓度1.25mol/L;外加碳源、磷源能够促进其降解阿特拉津;珍珠岩-PPVA在pH值为5.99~9.03时具有较好的降解效果,其抗酸碱能力优于游离W4菌.说明珍珠岩-PPVA可有效去除阿特拉津,可以作为新型材料加以深入研究应用于废水或土壤中阿特拉津降解.     

SPE-UPLC-MS/MS测定环境水体中呋喃丹、莠去津、甲萘威及6种邻苯二甲酸酯类

建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定环境水体中呋喃丹、莠去津、甲萘威和6种邻苯二甲酸酯的分析方法。采用Pak C18固相萃取小柱对样品进行富集和净化,甲醇-水为流动相梯度洗脱,以BEH C18柱分离,在串联质谱的多反应监测模式(MRM)下检测,外标法定量。结果表明,在优化实验条件下,9种目标化合物在0.5~20.0μg/L范围内线性关系良好,相关系数均大于0.998,方法检出限(LOD)和方法定量下限(LOQ)分别为0.05~0.12μg/L和0.2~0.3μg/L,回收率为86.0%~96.5%,相对标准偏差(RSD)小于5%。方法快速准确、回收率高,适用于环境水体中呋喃丹、莠去津、甲萘威及6种邻苯二甲酸酯的测定。     

莠去津分子印迹聚合物的合成及识别性能研究

以莠去津为模板分子,α-甲基丙烯酸为功能单体,在氯仿溶剂中合成了莠去津分子印迹聚合物．紫外光谱研究表明莠去津与功能单体α-甲基丙烯酸之间确实存在作用力,通过红外光谱分析了聚合物结构,可以确定模板分子与功能单体之间的作用力为氢键．利用透射电镜表征了溶剂用量对印迹聚合物微观形貌的影响,综合利用平衡结合实验考察了不同溶剂用量...     

固相萃取富集-高效液相色谱法测定水中莠去津

用高效液相色谱仪分析水中的三嗪类除草剂-莠去津(ATR)。样品经C18固相萃取柱富集后测定,流动相为甲醇-水,检测波长为220nm。莠去津浓度在0.1~5.0mg/L范围内与峰面积线性关系良好,相关系数r=0.9995,样品的加标回收率为82.0%~90.3%,测定结果的相对标准偏差为1.3%。     

聚乙烯醇固定化的微球菌AD3对除草剂阿特拉津的生物降解

从农药厂的工业废水和污泥的混合物中分离到高效降解除草剂阿特拉津的藤黄微球菌(Micrococcusluteus)AD3菌株。以聚乙烯醇(PVA)为包埋材料进行AD3菌株的固定化,对影响固定化细胞降解阿特拉津的因素(如阿特拉津浓度、温度、pH)和操作稳定性进行了研究。结果表明,在最适条件下(30℃、pH7.2、阿特拉津浓度500mg/L)固定化细胞的阿特拉津降解速度明显高于游离细胞。固定化细胞在低温、低pH和高阿特拉津浓度条件下的阿特拉津降解率,以及贮存和操作稳定性,也明显好于游离细胞。固定化细胞在15℃、pH7.2、阿特拉津浓度为500mg/L的条件下培养72h以后,阿特拉津降解率为90%,在相同条件下游离细胞的降解率仅为35%。固定化细胞在pH5.0、30℃、阿特拉津浓度为500mg/L的条件下培养72h以后,降解率为96%,在相同条件下游离细胞的降解率仅为40%。固定化细胞能够快速降解1000mg/L的阿特拉津,而游离细胞则不能。稳定性实验表明,固定化细胞重复使用30次以后其降解活力没有明显降低。