通过式固相萃取/超高效液相色谱-串联质谱法测定蔬菜中18种农药残留

建立了超高效液相色谱-串联质谱(UPLC-MS;MS)快速测定蔬菜中18种农药残留的方法.样品经乙腈提取后,经Oasis PRiME HLB固相萃取柱净化,采用ACQUITY UPLC HSS T3 C18(50 mm×2.1 mm,1.8μm)色谱柱进行分离,以0.1%甲酸水溶液和乙腈作为流动相进行梯度洗脱.采用电喷雾电离源、正离子模式下以多反应监测(MRM)进行定性和定量分析.结果表明,18种农药在0.5—50μg·L^-1范围内线性关系良好(r2>0.995),方法最低检出限为0.4—1.5μg·kg^-1,最低定量限为1.4—5.0μg·kg^-1.在韭菜、芹菜、番茄、白菜基质中,5、10、50μg·kg^-1添加水平下的加标回收率为60.2%—126.9%,相对标准偏差(RSD)为0.4%—21.6%(n=3).     

Preconcentration of cadmium and copper ions on magnetic core–shell nanoparticles for determination by flame atomic absorption

Magnetic core–shell nanoparticles modified by (3-aminopropyl) trimethoxy silane were prepared and used as adsorbent for the extraction and preconcentration of cadmium and copper ions. The ions were desorbed with nitric acid followed by determination with flame atomic absorption spectrometry. The extraction conditions were investigated systematically. The method was applied for the determination of Cd(II) and Cu(II) ions in different water samples. The accuracy was also evaluated through analysis of certified reference material.     

湿热水解预处理对餐厨废弃物液相物质转化的影响

设计湿热水解预处理温度(80、120、150和200 ℃)、时间(40、50、60和70 min)、加水量(40%、60%、80%和100%)的三因素四水平正交试验,研究湿热水解预处理对餐厨废弃物液相可浮油脱出量、ρ(COD_Cr)、糖类、ρ(VFA)(VFA为挥发性脂肪酸)等的影响. 结果表明:餐厨废弃物经湿热水解预处理后可浮油脱出量明显提高. 在150 ℃、加水量40%、处理60 min的湿热水解条件下,可浮油脱出量(67.7 mL/kg)最高,比未经预处理的对照组提高了2.65倍;同时,ρ(还原糖)和ρ(总糖)也达到最高,分别比对照组增加了16.29%和38.92%.随着温度升高和处理时间的延长,ρ(COD_Cr)不断升高,在200 ℃、加水量40%、处理70 min的湿热水解条件下,ρ(COD_Cr)最高为109.729 g/L,比对照组提高了1.39倍. 经湿热水解预处理后,ρ(VFA)也呈显著增加,在200 ℃、加水量100%、处理40 min的湿热水解条件下,ρ(VFA)达到最高,比对照组增加了66.26%.预处理后,ρ(乙酸)、ρ(丁酸)升高,ρ(乙醇)降低. 方差、极差综合分析表明,在湿热水解过程中,温度是影响餐厨废弃物液相物质转化的主控因子,其次是加水量和时间.      

一体化固相萃取-GC／ECD测定水中有机氯农药

建立了采用一体化固相萃取提取和净化、GC－MS／GC－ECD联合定性定量同时检测水中14种有机氯农药的方法,优化了固相萃取和色谱条件。样品于一体化固相萃取仪上以10 mL／min流速经C18柱富集、6 mL体积比为1∶1的二氯甲烷／乙酸乙酯混合溶剂洗脱、氮吹浓缩后,GC－MS／GC－ECD分离检测。结果表明,14种OCPs在1．00～500μg／L范围内线性良好,方法检出限为1．76～15．10ng／L,平均加标回收率为69．6％～102．8％,RSD为1．62％～18．9％。实际样品分析表明该方法灵敏度和精密度高、准确性好、操作简便,适用于大批量水样中微量和痕量OCPs的测定。     

Uncertainties in a risk management context in early phases of offshore petroleum field development

The current risk management approach for the Norwegian offshore petroleum industry came into effect in 2001 and has been stable with minor changes for 15 years. Relatively few new installations were slated for development until quite recently, and several new projects have been started in the last few years. The paper considers the risk management approach in the pre-FEED phase and builds on two case studies selected from the most recent cases. These case studies have been evaluated with respect to how uncertainties are considered in the early phase, based on the submission of the Plan for Development and Operation, their evaluations by authorities and the supporting documents. Both case studies involve new concepts for which there is no experience from similar environments and/or water depths. In spite of what could have been expected, the case studies conclude that uncertainties have not been in focus at all during concept development. This appears to be definitely the case for the licensees, but also to be the case for the authorities. Some suggestions are presented for what could have been considered by the licensees and authorities.     

对羧基苯偶氮硫代若丹宁固相萃取光度法测定环境样品中的铅

合成了新试剂对羧基苯偶氮硫代若丹宁(CPATR),并用红外光谱、核磁共振氢谱和元素分析鉴定其结构。研究了CPATR与铅的显色反应,在pH3 8的HAc—NaAc缓冲介质中,吐温-80存在下,CPATR与铅反应生成2∶1稳定络合物,该络合物可被WatersSep-PakC18小柱固相萃取,小柱上富集的络合物用乙醇洗脱后富集倍数可达50倍,在乙醇介质中,λmax=500nm,体系摩尔吸光系数ε=8.01×104L·mol-1·cm-1。铅含量在0 05～4 0mg/L内符合比耳定律。本方法可用于环境样品中铅含量的测定,结果满意。     

Early murine immune responses from endotracheal exposures to biotechnology-related Bacillus strains

An immunology-based in vivo screening regime was used to assess the potential pathogenicity of biotechnology-related microbes. Strains of Bacillus cereus (Bc), Bacillus subtilis (Bs), Bacillus thuringiensis (Bt), and Bt commercial products (CPs) were tested. Balb/c mice were endotracheally instilled with purified spores, diluted CP, or vegetative cells (VC) (live or dead). Exposed mice were evaluated for changes in behavioral and physical symptoms, bacterial clearance, pulmonary granulocytes, and pulmonary and circulatory pyrogenic cytokines (interleukins (IL)-1β, IL-6 and tumor necrosis factor (TNF)-α), as well as acute phase biomarkers (fibrinogen and serum amyloid A). Except for some differences in clearance rates, no marked effects were observed in mice exposed to any spore at 10⁶ or 10⁷ colony forming units (cfu). In contrast, live Bc or Bt VCs (10⁵ or 10⁶?cfu) produced shock-like symptoms (lethargy, hunched appearance, ruffled fur, and respiratory distress), and 11–200-fold elevations in pyrogenic cytokines at 2-h post-exposure. In the study, 4-h effects included increased lethargy, ocular discharge, and 1.5–4-fold rise in circulatory acute phase markers, but no indications of recovery. Bs VC did not produce any changes in symptoms or biomarkers. After 2 or 4?h of exposure to dead VC, increases of only plasma IL-1β and TNF-α (4.6- and 12.4-fold, respectively) were observed. These findings demonstrate that purified spores produced no marked effects in mice compared to that of metabolically active bacteria. This early screening regime was successful in distinguishing the pathogenicity of the different Bacillus species, and might be useful for assessing the relative hazard potential of other biotechnology-related candidate strains.     

Oxidized multiwalled carbon nanotubes modified with 2-(2-hydroxy-5-nitrophenyl)-4,5-diphenyl imidazole for solid phase extraction and preconcentration of some metal ions

In this work, a new procedure for the enrichment of the trace amount of Cu²⁺, Ni²⁺, Co²⁺, Pb²⁺, Fe²⁺, and Zn²⁺ ions based on the utilization of multiwalled carbon nanotubes (MWCNT) modified with 2-(2-hydroxy-5-nitrophenyl)-4,5-diphenyl imidazole as chelating agent prior to their determination by flame atomic absorption spectrometry has been described. The influence of effective parameters including pH, amount of ligand and MWCNT, composition of eluent, and coexisting ions on recoveries of understudy metal ions was examined. At the optimum pH of 5.0, all metal ions were quantitatively sorbed onto the proposed solid phase and completely desorbed with 8?mL of 5.0?mol?L^?1 HNO₃. The detection limit of Cu²⁺, Co²⁺, Ni²⁺, Pb²⁺, Fe²⁺, and Zn²⁺ ions was 1.7, 2.4, 2.3, 2.9, 2.8, and 1.4?µg?L^?1, while the preconcentration factor was 63 for Cu²⁺ and 94 for the other metal ions and relative standard deviations between 1.8 less than 3.0%. The proposed procedure was applied for the analysis of various samples.     

Determination of cadmium in water and herbal medicine by Penicillium chrysogenum immobilized on silica gel for flame atomic absorption spectroscopy

Penicillium chrysogenum was immobilized on silica to develop a simple and cost effective method for solid phase extraction of Cd(II) and determination using flame atomic absorption spectrometry (FAAS). The sorbent was characterized by Fourier transform infrared spectroscopy and packed into a column. The conditions for quantitative sorption and desorption of Cd(II) were optimized. The preconcentration factor was 100 while detection limit was 0.61 µg L^?1 with a relative standard deviation of 1.0%. The method was applied for determination of Cd in herbal medicine and tap water.     

Pah characteristics in ambient air within a steel industrial complex

Ambient air samples at ten sites in an iron and steel industrial complex were collected from June to December for analyzing polycyclic aromatic hydrocarbons (PAHs). Sixteen species of PAH components in air samples were identified. The results indicate that both gaseous phase and particle‐bound PAHs at the top of the cokemaking plants are unusually high. The profiles of particle‐bound PAHs indicate that the predominant species at the top of, the coke oven batteries are those of high molecular weight components. The major components of particle‐bound PAHs at sampling sites near the fenceline, however, include the medium molecular weight components. The PAH profiles of air samples within the industrial complex show a strong similarity to those of cokemaking plant samples. The concentrations and the specific content of benzo(a)pyrene in the iron and steel industrial complex are higher than those values measured in urban area, petrochemical industry park, and open‐air burning area.