ASE-气相色谱法测定油田区土壤中多种石油烃

采用气相色谱法测定油田区土壤中C_(10)～C_(40)的石油烃,通过优化加速溶剂萃取的条件,使方法在62 mg/L～3 100 mg/L范围内线性良好,方法检出限为4.8 mg/kg。用该方法测定石油区短期、中期、长期油井污染土壤样品,5次测定结果的RSD为1.3%～5.2%,加标回收率为84.8%～98.5%,有证标准样品测定结果在可信区间内。     

Evaluation of photolysis and hydrolysis of pyraclostrobin in aqueous solutions and its degradation products in paddy water

This study evaluated the hydrolysis and photolysis kinetics of pyraclostrobin in an aqueous solution using ultra-high-performance liquid chromatography–photodiode array detection and identified the resulting metabolites of pyraclostrobin by hydrolysis and photolysis in paddy water using high-resolution mass spectrometry coupled with liquid chromatography. The effect of solution pH, metal ions and surfactants on the hydrolysis of pyraclostrobin was explored. The hydrolysis half-lives of pyraclostrobin were 23.1–115.5?days and were stable in buffer solution at pH 5.0. The degradation rate of pyraclostrobin in an aqueous solution under sunlight was slower than that under UV photolysis reaction. The half-lives of pyraclostrobin in a buffer solution at pH 5.0, 7.0, 9.0 and in paddy water were less than 12?h under the two light irradiation types. The metabolites of the two processes were identified and compared to further understand the mechanisms underlying hydrolysis and photolysis of pyraclostrobin in natural water. The extracted ions obtained from paddy water were automatically annotated by Compound Discoverer software with manual confirmation of their fragments. Two metabolites were detected and identified in the pyraclostrobin hydrolysis, whereas three metabolites were detected and identified in the photolysis in paddy water.     

加速溶剂同时萃取和净化-气相色谱-三重四极杆串联质谱测定土壤和沉积物中8种多溴联苯醚

建立了土壤和沉积物中8种多溴联苯醚(PBDEs,BDE-28、BDE-47、BDE-99、BDE-100、BDE-153、BDE-154、BDE-183和BDE-209)加速溶剂同时萃取和净化-气相色谱-三重四极杆串联质谱(ASE-GC-MS-MS)的分析方法。通过优化加速溶剂萃取与弗罗里硅土在线净化和串联质谱多反应监测模式的条件,较好地去除基质干扰,并提高了三重四极杆串联质谱定性的准确性及定量的灵敏性。该方法采用改进的色谱柱能同时分析包括高溴代联苯醚BDE-209在内的8种PBDEs,其浓度范围为1～100 ng/mL(BDE-209为10～1 000 ng/mL),线性良好,线性回归系数均大于0.997。方法检出限为0.004～0.1 ng/g,方法回收率为75%～110%,方法精密度为2.4%～15.6%。适于批量处理土壤和沉积物中含有多组分痕量PBDEs的样品。     

宁波市饮用水源地爆发蓝藻水华时微囊藻毒素的污染分析

通过固相萃取净化,建立了超高效液相色谱-串联四极杆质谱法测定水中微囊藻毒素MC-LR和MC-RR的方法,并用该方法监测了宁波市两个饮用水源地爆发蓝藻水华时水体中的微囊藻毒素.监测结果表明,姚江水体中的微囊藻毒素污染水平低,MC-LR和MC-RR没有被检出;梅湖水库水体中MC-RR也未被检出,采取措施后,虽MC-LR有时被检出,但最高时也低于国家标准值(1.0μg/L).     

固相萃取气相色谱法测定地表水中有机磷农药

建立了固相萃取(SPE)气相色谱火焰光度(GC-FPD)检测方法,并且检测了地表水中8种有机磷农药,检测限在0.09～0.26μg/L之间,相对标准偏差为3.1%～9.7%(n=8),加标回收率达到61.3%～103.2%,与传统的气相色谱法相比,该方法具有比较高的重现性和选择性,在地表水有机磷农药的测定中具有很好的应用前景.     

Magnetic resonance image findings of placental lake: report of two cases

Two cases with a large cystic mass within the placenta are reported. By ultrasonography, it was found that both women had a subchorionic hypoechoic lesion (11.0 × 4.8 × 4.0 cm and 6.6 × 3.7 × 2.2 cm, respectively) at 24 and 35 weeks of gestation, respectively. In both cases, turbulent blood flow generated by a pulsatile jet flow (pulse rate; 40 to 60 beats per minute) into the cystic lesion seen on real-time imaging and lesions being low intensity on T1-weighted and isointensity on T2-weighted magnetic resonance image suggested that they contained fresh maternal blood. In both cases, the sonolucency of the lesions did not change until cesarean deliveries of females, both of whom were small-for-gestational-age infants (1940 g at 37 weeks and 2195 g at 37 weeks, respectively). Biochemical analysis of the fluid in the cystic lesion sampled during the cesarean section in the latter case confirmed that the fluid had originated from the maternal blood. These lesions histologically corresponded to large avillous areas surrounded by normal villi. Thus, a huge placental lake was diagnosed in both cases. Copyright © 2005 John Wiley & Sons, Ltd.     

基于稳定氢同位素的太原市大气单环芳烃来源

采集太原市城北和城南区域环境空气和5类污染源挥发性有机物样品,测定样品中典型单环芳烃稳定氢同位素（δD）组成,基于同位素质量平衡原理计算单环芳烃从源到环境空气受体的δD初始混合值,探讨单环芳烃来源.结果表明,柴油挥发源、溶剂挥发源、汽油挥发源（97^#）、汽油挥发源（95^#）、机动车尾气（97^#）、机动车尾气（95^#）和民用燃煤源中单环芳烃δD范围依次为：（-138.7‰~-115.5‰）、（-147.0‰~-121.0‰）、（-150.8‰~-117.6‰）、（-131.8‰~-113.8‰）、（-171.2‰~-120.0‰）、（-138.9‰~-102.7‰）和（-168.3‰~-142.3‰）,民用燃煤源中单环芳烃δD显著贫重氢同位素（D）组成,机动车尾气源与汽油挥发源中苯的δD相比显著贫D,可用于探索污染物转化过程;城北和城南环境空气中δD范围为（-131.7‰~-115.1‰）和（-131.9‰~-74.9‰）,δD初始混合值为-138.4‰和-173.9‰,体现了其来源差异.     

Advanced molecular-fingerprinting analysis of dissolved organic sulfur by electrospray ionization-Fourier transform ion cyclotron resonance mass spectrometry using optimal spray solvent

Molecular level characterization of dissolved organic sulfur (DOS) by electrospray ionization-Fourier transform ion cyclotron resonance mass spectrometry (ESI-FTICR MS) is necessary for further understanding of the role of DOS in the environment. Here, ESI spray solvent, a key parameter for ion production during ESI process, was investigated for its effect on the molecular characterization of DOS by ESI-FTICR MS. 100% MeOH as spray solvent was found for the first time to remarkably enhance the ionization efficiency of the majority of CHOS-molecules in NOM, which facilitated a total of 1473 CHOS-molecular formulas with one sulfur atom to be detected. The number of CHOS-molecular formulas obtained using 100%MeOH as spray solvent increased notably over 740 in comparison with those using 50% MeOH aqueous solution (731) or 50% ACN aqueous solution (653). Moreover, due to the enhancement of ionization efficiency of DOS during ESI processes, the tandem mass spectra of the NOM CHOS-molecules could be easily obtained using 100% MeOH as spray solvent, which were hardly obtained using 50% MeOH aqueous solution as spray solvent. The results of the tandem mass spectra suggested the first discovery of organosulfates or sulfonic acids in Suwannee River NOM sample. A simple method based on 100% MeOH as ESI spray solvent for advanced molecular characterization of DOS by ESI-FTICR MS was proposed and applied, and the results revealed more molecular information of DOS in sea DOM samples.     

厦门市冬季PM2.5污染情境识别及其与气象条件的关系

为研究厦门市冬季不同PM_2.5污染情境与气象条件和气团轨迹路径特征的关系,结合PM_2.5观测数据,使用AGAGE（Advanced Global Atmospheric Gases Experiment）统计方法识别2014—2018年冬季厦门市PM_2.5观测值、基线值和污染值情境,通过气象数据统计和气团后向轨迹聚类对不同PM_2.5污染情境下气象条件和气团轨迹路径特征进行探究.结果表明:①厦门市冬季不同PM_2.5污染情境下,ρ（PM_2.5）及PM_2.5污染值情境时长占比均呈波动中下降的趋势,具体表现为冬季PM_2.5观测值、污染值和基线值情境下,ρ（PM_2.5）平均值分别从2014年的42.2、90.7、16.4 μg/m3降至2018年的26.3、56.9、8.8 μg/m3,冬季PM_2.5污染值情境时长占比从2014年的10.2%降至2018年的3.0%.②冬季PM_2.5污染值情境下气象要素呈低风速、低气压、高温度、高相对湿度的特征.③冬季到达厦门市的气团轨迹路径中,局地路径由于大气条件稳定易累积形成PM_2.5污染;偏北路径和西北路径易从临近省份携带污染物输入导致PM_2.5污染,属于重要的外源污染输入路径;沿海路径和偏西路径均属于清洁路径,但沿海路径易在福建省北部与偏北路径重合形成污染输入,加强了偏北路径的污染物输送能力.研究显示,近年来厦门市冬季PM_2.5污染有明显减弱趋势,但不利的气象条件和外来污染输入仍会造成PM_2.5污染的发生.