利用两种采样技术监测淮河水中的有毒有机污染物

利用固相萃取（SPE）和三油酸酯－半渗透膜采样器（triolein－SPMD）采集并测定了淮河信阳、淮南２个采样点水样中有毒有机污染物浓度．对２种采样方法的比较发现,对于水中多氯联苯、多环芳烃、取代苯３类目标污染物检出种类基本相同,但这些污染物在SPMD样品中浓度的富集倍数明显增加．污染物在triolein－SPMD酯中的高浓度,便污染物的定性和定量更加容易和准确,可以根据triolein－SPMD酯／水分配平衡理论计算目标污染物在水中的平均浓度,其结果与SPE具有可比性．综合triolein－SPMD在经济和操作上的诸多优点,本研究认为triolein－SPMD技术可在我国的优先污染物的监测工作中发挥作用．     

气提式三重循环生物膜反应器处理制药废水中的甾体雌激素

为验证气提式三重循环生物膜反应器处理甾体雌激素的效能,建立了一套SPE/HPLC/MS/MS分析方法,对反应器进、出水中的甾体雌激素--甾酮(E1),17β-雌二醇(E2),雌三醇(E3)以及17α-乙炔基雌二醇(EE2)进行检测.该方法的加标回收率为88%～103%,精密度为4%～9%.该方法对E1,E2,E3和EE2的进水定量限(LOQ)分别为0.7,0.8,0.9和0.5 ng/L;对出水的定量限分别为2.0,1.0,2.0和 1.0 ng/L.CODCr和氨氮容积负荷最高为7.5和1.6 kg/(m3·d),出水依然能够保持稳定.进水pH稳定在9.0～10.5,而反应器的pH一直稳定在9.0以下,体系对pH变化造成的冲击比较适应.同时,反应器内形成了稳定的NO2--N积累,CODCr和氨氮的去除率分别达到了70%和73%.     

土壤中残留苯磺隆的高效液相色谱分析

本文报道了一种固相萃取净化，高效液相色谱测定土壤中苯磺隆的残留分析方法，不同土壤的添加回收率平均为８３．３％，８６．３％，７７．２％，线性范围２．５５－５１０ｎｇ，利用本法分析苯磺隆，精确、简便、快速。     

Influence of Suspended Clay Minerals and Humic Matter on the Solid Phase Extraction Efficiency of Selected Pesticides from Water

The purpose of this investigation was to determine the influence of humic acids (HA) and Ca-montmorillonite (CaM) on the solid-phase extraction (SPE) efficiency of atrazine, alachlor and α-cypermethrin from water samples at various pH-values. The nature and intensity of binding of the studied pesticides to CaM were determined by X-ray diffraction analysis and termogravimetric analysis (TGA) test. The studied pesticides eluted from discs were analysed by thin-layer chromatography (TLC). The effects of CaM and humic acid were generally pH-dependent and acted independently in extraction efficiency influence. Lower recovery of pesticides was observed at higher pH values when CaM was ≥0.1 g and was attributed to greater dispersion of clay, increased surface area and subsequent adsorption. Concentrations of dissolved organic carbon (DOC) in humic acid had less effect on the extraction efficiency when water was at pH 8 compared to water at pH 2, which was probably due to greater nonpolar interactions of the pesticides to the charge-neutralized humic acid molecule.     

固相萃取—气相色谱法测定海水中的666、DDT

采用固相萃取技术富集海水中的666、DDT,并使用气相色谱进行测定。主要包括不同填料(C8、C18、C18-N)、SPE柱规格(500 mg/3 mL、500 mg/6 mL)、洗脱试剂、上样流速、水样pH和洗脱试剂体积6个因素对666、DDT富集效率的影响。最终确定最优条件为:采用500 mg/6 mL C18SPE小柱,调节海水pH=6,上样流速4~5mL/min,10 mL二氯甲烷洗脱。优化后的固相萃取-气相色谱方法测定海水中666、DDT加标10 ng/L回收率为75.7%~110.4%,精密度为1.16%~4.00%,方法检出限为0.19~1.20 ng/L。     

地表水体中同时分析18种糖皮质激素方法的建立

建立了一种采用固相萃取-超高效液相色谱串极质谱联用系统(UPLC-MS/MS)同时测定地表水体中18种糖皮质激素的高灵敏分析方法.样品经过HLB固相萃取柱富集净化、V(乙腈)/V(乙酸乙酯)=1∶1,洗脱后,用UPLC-MS/MS测定.流动相为甲醇和0.1%乙酸水溶液(体积比),采用梯度洗脱,实现了18种目标物质的基线分离,线性范围为1.0~1 000μg·L-1.实际水样的加标回收率为65%~108%.整个分析的方法检出限(MDL)除醋酸可的松和醋酸氢化可的松为10 ng·L-1外,其他均在0.10 ng·L-1和1.0 ng·L-1之间.应用此方法于北京地表水体5个样品,检测到8种糖皮质激素,浓度范围0.20~476ng·L-1,其中曲安西龙、曲安奈德、醋酸氢化可的松和丙酸氯倍他索在地表水中首次检出,证明了该方法的有效性.     

北京官厅水库中农药类内分泌干扰物分布和来源

研究了北京官厅水库中农药类内分泌干扰物污染水平、分布特点和来源.结果表明,官厅水库及其支流水体受到农药类内分泌干扰物轻度污染.从农药在官厅水库中的分布推断,官厅水库以及各支流周边地区及农田排水渠是水库中农药的重要来源.底泥中农药通过底泥孔隙向表面水扩散,是表面水农药的1个污染源.由于水库周边较多的农业活动,可能导致水中农药浓度提高.为了减少污染和水生生物对内分泌干扰物的暴露,需要进行定期监测,减少农药的使用和农事操作.     

水体中MC-LR的高效液相色谱检测前处理条件优化

通过正交实验设计,对水体中MC-LR前处理过程中SPE柱的选择、水样pH值、洗脱液有机相浓度、酸度和体积等关键因素进行综合分析,得出最优前处理方案。通过精密度和加标回收实验,得出该方法精密度为4.81%,加标回收率为98.96%。     

Simultaneous and direct determination of glyphosate and AMPA in water samples from the hydroponic cultivation of eucalyptus seedlings using HPLC-ICP-MS/MS

Abstract

Glyphosate is the main herbicide currently used in the world due to wide applicability and efficiency in controlling weeds in many crops. However, its overuse may lead to undesirable impacts on the environment and to human health in the long run. This present study aimed to optimize and validate solid phase extraction (SPE) using an anionic resin for the simultaneous and direct determination of glyphosate and aminomethylphosphonic acid (AMPA) in water samples using high-performance liquid chromatography combined with inductively coupled plasma with triple quadrupole mass spectrometer (HPLC-ICP-MS/MS). The results showed that recovery percentage and relative standard deviation were 103.9?±?7.9 and 99.40?±?9.9% for glyphosate and AMPA, respectively. The validation certified that the method was precise, accurate, linear, and selective, with a limit of quantification of 1.09 and 0.29?μg L^?1 for glyphosate and AMPA, respectively. The optimized methodology reached the concentration factor of 250 times and was successfully applied to analyze water samples from hydroponic cultivation of the eucalyptus seedlings. The results showed that the exudation process occurs at glyphosate doses starting from 2?L ha^?1.     

百菌清农药残留的SPE-GC检测

对环境水样中百菌清农药残留进行了SPE-GC分析方法研究。环境水样通过Florisil柱富集、净化,3 mL乙酸乙酯洗脱,GC-ECD进行分析检测。实验表明,百菌清农药残留在0.01~10 mg/L范围内线性关系良好,相关系数为0.9993。外标法定量,检出限为0.0035 mg/L,对实际水样进行加标回收,回收率范围在93.47%~100.14%之间,6次重复测定相对标准偏差在3.97%~4.96%之间,并将方法应用于周边环境地表水的检测。该方法具有简便,快速,准确,灵敏度高等特点,能满足环境水样中农药残留分析要求。