Estimation of β-cyfluthrin and imidacloprid in okra fruits and soil by chromatography techniques

Dissipation of β-cyfluthrin and imidacloprid in okra was studied following three applications of a combination formulation of Solomon 300 OD (β-cyfluthrin 9 % + imidacloprid 21 %) @ 60 and 120 g a.i. ha^?1 at 7 days interval. Residues of β-cyfluthrin and imidacloprid in okra were estimated by gas liquid chromatography (GLC) and high performance liquid chromatography (HPLC), respectively. Residues of β-cyfluthrin were confirmed by gas chromatograph–mass spectrometry (GC-MS) and that of imidacloprid by high performance thin layer chromatography (HPTLC). Half-life periods for β-cyfluthrin were found to be 0.91 and 0.68 days whereas for imidacloprid these values were observed to be 0.85 and 0.96 days at single and double the application rates, respectively. Residues of β-cyfluthrin dissipated below its limit of quantification (LOQ) of 0.01 mg kg^?1 after 3 and 5 days at single and double the application dosage, respectively. Similarly, residues of imidacloprid took 5 and 7 days to reach LOQ of 0.01 mg kg^?1, at single and double dosages respectively. Soil samples collected after 15 days of the last application did not show the presence of β-cyfluthrin and imidacloprid at their detection limit of 0.01 mg kg^?1.     

Variability in the content and composition of alkaloids found in canadian ergot. I. Rye

Abstract

The total alkaloid content and individual alkaloid composition were determined by colorimetry and high performance liquid chroma‐tography, respectively, for Canadian rye ergot sclerotia. The total alkaloid content was highly variable between sclerotia from the same head, field, or region and ranged from 0.011 to 0.452% (av. 0.249%). Levels were lowest in ergot from Prince Edward Island. The individual alkaloid composition was uniform throughout a single sclerotium or in different sclerotia from the same head, somewhat uniform for averages in different fields throughout a region, but highly variable from head to head in a given field. On a regional basis, ergotamine followed by ergocristine were the major alkaloids observed in the east whereas the order wasreversed in the west. Ergometrine, ergosine, ergocornine, and ergocryptine were also observed to a lesser degree; ergostine was not observed. Isomerization of ergometrine increased from near 0% in the east to about 40% in the west, but was relatively constant (about 30%) for the peptide alkaloids in all regions.     

微囊藻毒素测定中产生的干扰及排除

采用固相萃取-高效液相色谱法定性、定量测定水中微囊藻毒素,对水样富集管(观赏鱼用氧气塑料管、橡胶管、医用乳胶管和硅胶管)、塑料材质(聚丙烯离心管等)、针式过滤器(水系、有机系针式过滤器)产生的干扰和吸附现象进行了深入探索.结果表明,观赏鱼用氧气塑料管对微囊藻毒索测定会产生严重的正干扰,在流动相甲醇:磷酸盐缓冲溶液(体积比)为50:50时,干扰得以排除;聚丙烯离心管在微囊藻毒素投加量较低时,对微囊藻毒索吸附率较高,造成回收率偏低;不同的针式过滤器对溶解在不同体积分数的甲醇溶液中的微囊藻毒素有明显不同的吸附能力.     

高效液相色谱法测定鸡蛋清和蛋黄中磺胺类药物残留

采用高效液相色谱法测定鸡蛋清和蛋黄中磺胺嘧啶、磺胺吡啶、磺胺二甲基嘧啶、磺胺甲氧哒嗪、磺胺甲恶唑、磺胺间甲氧嘧啶、磺胺喹恶啉等7种磺胺类药物残留,优化了色谱条件和样品预处理方法。7种磺胺类药物在0.050 mg/L~10.0 mg/L范围内线性良好,检出限和定量限分别低于0.02 mg/kg和0.04 mg/kg。在0.250 mg/kg和0.500 mg/kg两个添加水平,蛋清中的回收率为81.0%~100%,RSD为0.8%~4.8%,蛋黄中的回收率为72.2%~94.1%,RSD为1.1%~6.9%。     

HPLC determination of chlorate metabolism in bovine ruminal fluid

Salmonella and Escherichia coli are two bacteria that are important causes of human and animal disease worldwide. Chlorate is converted in the cell to chlorite, which is lethal to these bacteria. An HPLC procedure was developed for the rapid analysis of chlorate (ClO₃ ^?), nitrate (NO₃ ^?), and nitrite (NO₂ ^?) ions in bovine ruminal fluid samples. Standard curves for chlorite, nitrite, nitrate, and chlorate were well defined linear curves with R² values of 0.99846, 0.99106, 0.99854, and 0.99138, respectively. Concentrations of chlorite could not be accurately determined in bovine ruminal fluid because chlorite reacts with or binds a component(s) or is reduced to chloride in bovine ruminal fluid resulting in low chlorite measurements. A standard curve ranging from 25 to 150 ppm ClO₃ ^? ion was used to measure chlorate fortified into ruminal fluid. The concentration of chlorate was more rapidly lowered (P < 0.01) under anaerobic compared to aerobic incubation conditions. Chlorate alone or chlorate supplemented with the reductants sodium lactate or glycerol were bactericidal in anaerobic incubations. In anaerobic culture, the addition of sodium formate to chlorate-fortified ruminal fluid appeared to decrease chlorate concentrations; however, formate also appeared to moderate the bactericidal effect of chlorate against E. coli. Addition of the reductants, glycerol or lactate, to chlorate-fortified ruminal fluid did not increase the killing of E. coli at 24 h, but may be useful when the reducing equivalents are limiting as in waste holding reservoirs or composting systems required for intense animal production.     

高效液相色谱法测定水和废水中邻(对)硝基氯苯

用高效液相色谱法测定了水和废水中的邻 (对 )硝基氯苯。流动相为甲醇 /水 (70 /3 0 ) ,紫外检测波长 2 2 0 nm,方法的线性范围为 0～ 1 0 0 μg/ml,相关系数大于 0 .9998,检测限为 2 μg/L。本方法快速、准确 ,满足地面水的测定要求     

转Bt基因棉花抗虫萜烯类化合物时空动态的HPLC分析

利用高效液相色谱（HPLC）技术对转Bt基因棉花抗虫萜烯化合物种类、含量以及时空动态进行了初步研究。结果表明，被研究的抗虫棉品种抗虫萜烯类化合物在不同品种、不同组织器官间含量差异较大。叶片中杀实夜蛾素（包括H1、H2、H3、H4)含量较高，花及蕾中棉酚含量的比例明显高于叶片。总抗虫萜烯类（包括棉酚、半棉酚酮、杀实夜蛾素H1、H2、H3、H4以及甲氧基半棉酚酮等）均以铃、顶叶含量最高，蕾、花柱等器官次之。说明在棉花不同品种、同一品种不同器官中是不同的萜烯类化合物在起到抗虫作用。图3参16     

Depolymerization of polyaromatic hydrocarbons by Penicillium spp. inhabit the phyllosphere of urban ornamental plants

A variety of anthropogenic sources release hazardous polyaromatic hydrocarbons (PAHs) into the phyllosphere which is an excellent niche for diverse fungi, and some of them have PAHs degradation capabilities. Therefore, this research attempted to determine the PAHs (phenanthrene, anthracene, naphthalene, and pyrene) degradation capability of phyllosphere inhabited Penicillium species. The leaf samples were collected from highly polluted urban areas (Panchikawatta, Pettah, Orugodawatta, Maradana, Sapugaskanda, and Colombo Fort) in Sri Lanka to isolate fungal species inhabiting the phyllosphere. Furthermore, their distribution patterns among the leaf tissue layers were studied using bright-field microscopic observations. Moreover, the best PAH degraders were screened out using plate assays and confirmed through High Performance Liquid Chromatography (HPLC) analysis. Further, their enzymatic activities during the PAHs degradation were analyzed. As per the microscopic observations, the highest fungal distribution was in the upper epidermis of the leaves followed by the fungal distribution in the interspaces of palisade mesophyll layers. Out of isolated fungal species, two Penicillium spp. (Penicillium citrinum P₂₃B-91 and Penicillium griseofulvum P₉B - 30) showed the highest PAHs (phenanthrene, anthracene, naphthalene, and pyrene) degradation capabilities. Manganese peroxidase (MnP) enzyme dominated phenanthrene degradation in P. griseofulvum P₉B - 30, which showed the highest phenanthrene degradation ability (61%). In addition, P. citrinum P23B-91 was good at degrading anthracene (88%) and also displayed a higher MnP activity during the anthracene degradation than laccase and lignin peroxidase activities. The discoveries from the toxicity assay during the PAHs degradation processes revealed that the produced byproducts had no toxic effects on the fungal growth cycle and the phyllosphere. Therefore this phyllosphere Penicillium spp. are ideal for the bioremediation of polluted air in urbanized areas.     

固相膜萃取-高效液相色谱法测定地下水中的多环芳烃

采用C18固相膜萃取对地下水中15种多环芳烃进行富集净化，以二氯甲烷作洗脱溶剂，高效液相色谱法，荧光检测器测定。对萃取、浓缩和色谱条件进行优化，在1．ooixg／L～40．0μg／L范围内测定标准系列溶液并绘制标准曲线，相关系数R2〉0．999；15种多环芳烃的仪器检出限为0．4ng／L～3．0ng／L；对地下水样品加标，平均回收率在75．7％～96．7％之间；标准溶液平行测定7次的RSD为3．1％～11．9％。     

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.