Determination of the insecticide diflubenzuron in mushrooms by kinetic method and high-performance liquid chromatographic method

In the present study, a new sensitive and simple kinetic-spectrophotometric method for the determination of the insecticide diflubenzuron [1-(4-chlorophenyl)-3-(2,6-diflubenzoil)urea] is proposed. The method is based on the inhibited effect of diflubenzuron on the oxidation of sulphanilic acid (SA) by hydrogen peroxide in phosphate buffer in presence Cu(II) ion. Diflubenzuron was determined with linear calibration graph in the interval from 0.31 to 3.1 μg mL^?1 and from 3.1 to 31.0 μg mL^?1. The optimized conditions yielded a theoretical detection limit of 0.18 μg mL^?1corresponding to 0.036 mg Kg^?1mushroom sample based on the 3S_b criterion. The RSD is 5.03–1.83 % and 2.81–0.71 % for the concentration interval of diflubenzuron 0.31–3.1 μg mL^?1and 3.1–31.0 μg mL^?1, respectively. The reaction was followed spectrophotometrically at 370 nm. The kinetic parameters of the reaction are reported, and the rate equations are suggested. The developed procedure was successfully applied to the rapid determination of diflubenzuron in spiked mushroom samples of different mushroom species. The HPLC method was used like a comparative method to verify results.     

磺酰脲类除草剂及其主要降解产物分配系数的测定与预测

本文测定了甲黄隆，氯黄隆，苄嘧黄隆及其主要降解产物取代磺胺和取代氮杂环化合物的辛醇－水分配系数，研究了反相高效液相色谱容量因子、分子连接性指数、Ｌｅｏ碎片常数与分配系数间的相关关系，从而建立了估算磺酰类除草剂及其降解产物的疏水性方程。     

Syntrophic co-culture of Bacillus subtilis and Klebsiella pneumonia for degradation of kraft lignin discharged from rayon grade pulp industry

In order to search the degradability of kraft lignin, the potential bacterial strains Bacillus subtilis (GU193980) and Klebsiella pneumoniae (GU193981) were isolated, screened and applied in axenic and co-culture conditions. Results revealed that mixed culture showed better decolorization efficiency (80%) and reduction of pollution parameters (COD 73% and BOD 62%) than axenic culture. This indicated syntrophic growth of these two bacteria rather than any antagonistic effect. The HPLC analysis of degraded samples of kraft lignin has shown the reduction in peak area compared to control, suggesting that decrease in color intensity might be largely attributed to the degradation of lignin by isolated bacteria. Further, the GC–MS analysis showed that most of the compounds detected in control were diminished after bacterial treatment. Further, the seed germination test using Phaseolus aureus has supported the detoxification of bacterial decolorized kraft lignin for environmental safety. All these observations have revealed that the developed bacterial co-culture was capable for the effective degradation and decolorization of lignin containing rayon grade pulp mill wastewater for environmental safety.     

北京东南郊土壤剖面氟喹诺酮类抗生素分布特征

采用Geoprobe在北京东南郊地区实施了土壤剖面钻探,针对8种不同类型土地利用状况的土壤剖面进行土壤采集工作,11个采样点共采集86个土壤样品,分析了土壤样品的理化参数,并且采用高效液相色谱法对土壤样品中5种氟喹诺酮类抗生素(FQs)进行了定量分析.结果表明,北京地区土壤样品中5种氟喹诺酮类抗生素总含量的平均值为46.1μg·kg-1,组成以氧氟沙星(OFL)为主,其次为诺氟沙星(NOR),而恩诺沙星(ENR)、环丙沙星(CIP)和洛美沙星(LOM)的含量很低;不同土壤剖面中氟喹诺酮类抗生素的含量和组成差异明显.5种氟喹诺酮类抗生素总含量的平均值随土壤深度的增加呈现降低的趋势.OFL、NOR、LOM和ENR的平均含量随着深度增加而降低;CIP的平均含量随深度增加先降低后升高.对42个位于浅层(0~3 m)的土壤样品进行模糊聚类分析,结果表明,蔬菜大棚、树林、再生水灌区、地下水灌区(清灌区)、养殖场、排污河沉积物的浅层土壤样品中的喹诺酮类抗生素具有相似的组成特征,即抗生素污染水平较低、种类较少;而制药企业及垃圾填埋场的组成特征与前者明显不同,即抗生素污染水平中等、种类较多.     

Determination of T‐2 toxin in grain and grain products by HPLC and TLC

Abstract

The purpose of this study was to investigate the T‐2 toxin contaminated grain and grain products consumed especially by Turkish population. The T‐2 toxin was detected using the high performance liquid chromatography (HPLC) with UV detector at 208 nm and the identify of T‐2 was further confirmed by thin layer chromatography (TLC). The recovery was 91 ±4.24% for corn flour fortified with the known amount of T‐2 toxin (1 ppm). The detection limits of T‐2 toxin for the HPLC and the TLC were 25 ng and 50 ng, respectively. A total of 30 commercially available grain and grain product samples were analyzed. Two corn flour samples were found to contain detectable levels of T‐2 toxin at a level of 1.60 ppm and 4.08 ppm.     

高效液相色谱法测定水中对(邻)硝基苯胺

建立了用高效液相色谱法测定水中对(邻)硝基苯胺的方法。水中对(邻)硝基苯胺用乙醚萃取,在40℃水浴将乙醚挥发至干,用1.0ml甲醇提取后测定。对(邻)硝基苯胺浓度在0～1.0mg/L范围内线性良好,相关系数大于0.9994,日内相对标准偏差为6.5%和5.4%,平均回收率为104.3%和107.4%。     

印钞行业废水中邻苯二甲酸酯类化合物残留分析

建立了以HLB固相萃取柱和反相液相色谱法测定水体中8种邻苯二甲酸酯类环境激素的方法,同时对印钞行业废水中邻苯二甲酸酯类环境激素进行了测定,检出邻苯二甲酸丁基苄基酯(BBP)一种邻苯二甲酸酯类环境激素。使用标准保留时间定性及实际水样加标定性两种定性方法,对实验结果进行了质量控制。结果表明,这两种定性方法所得结论完全一致,证明数据准确可信。     

工业废水中烟酸、烟酰胺和3-氰基吡啶的HPLC检测

探讨了采用HPLC法检测某烟酰胺生产废水中所含的烟酸、烟酰胺和3-氰基吡啶的方法。结果显示,该方法的检测范围(S/N=3)为0.70~1.18 mg/L,方法的回收率为87%~102%,相对标准偏差为0.9%~3.9%,是一种快速、敏感和可靠的测定方法。     

Determination of dissolved selenium species in environmental samples

This article reports on the technique for the determination of selenium at ppt level and the procedure for the speciation of dissolved selenium in the environmental samples. By combining the high-performance liquid chromatography (HPLC) and a fluorescent detector (FLD), this technique permits the determination of selenium at 0.001 μg/L for Se(IV) and 0.005 μg/L for Se(VI) and the total concentration of selenium for a sample volume of 20 ml. In the speciation procedure, Se(IV) is firstly determined based on the selectivity of 2, 4 - diaminonaphthalene (DAN), the Se (VI) and the total element concentration are determined after reduced to Se(IV) by boiling in 4 mol/L HCl and by digesting in HNO3-HClO4 mixture, respectively. Discussions are given on the relationship between selenium speciation in waters and soil water extract and solution pH, EH and total organic carbon concentration (TOC).     

海洋浮游藻类的化学分类法

综述了以色素分析为基础的海洋浮游藻类化学分类法的发过程，发现基础性数据缺乏和应用范围不够广阔是阻碍此项研究发展的主要问题。本文详细讨论了高效液相色谱（HPLC）藻类色素分析数据之数学解析技术的进展，对最近出现的分析软件（CHEMTAX）进行了重点介绍。最后，对海洋浮游藻化学分类法的发展趋势进行了分析预测。