Evaluation of C18 solid‐phase extraction cartridges for the isolation of select pesticides and metabolites

Abstract

Nine different C₁₈ solid‐phase extraction (SPE) cartridges were evaluated for their efficiency at extracting nine pesticides and two s‐triazine metabolites from spiked deionized water samples. The SPE cartridges were found to contain nitrogen (N) and/or phosphorus (P) contaminants and varied in their extraction efficiency for certain pesticides and metabolites. Four of the nine SPE cartridges gave acceptable (70 to 120%) pesticide and metabolite recovery percentages, while five cartridges had marginal (50 to 70%) to poor (< 50%) recoveries. Statistical analyses showed that the poor to marginal recoveries found for three compounds could not be explained by considering several indigenous chemical and physical traits of the cartridge. It is suggested that proper SPE cartridge selection for pesticide recovery should be evaluated using several different cartridges.     

Determination of 10 particle-associated multiclass polar and semi-polar pesticides from small streams using accelerated solvent extraction

A new analytical method using accelerated solvent extraction was developed for the determination of 10 particle-associated polar and semipolar pesticides. In addition, six deuterated analogues of the target compounds were evaluated as internal standards. The method yielded acceptable accuracy (73–103% recovery) and precision (<25% relative standard deviation) for eight compounds. Using size exclusion chromatography (SEC) as cleanup step resulted in higher recoveries compared to solid phase extraction (SPE) cleanup.

Deuterated standards with 10 or more deuterium atoms performed well as internal standards concerning similar recovery and correlation with the target analytes.

The method was employed to extract particle-associated pesticides from 16 streams located in an area with intense agriculture in France. Acetochlor, pirimicarb, tebuconazole, fenpropidin, -endosulfan and chlorfenvinphos were detected at concentrations up to 1 mg kg⁻¹ dry weight. A comparison with aquatic toxicity data indicated potential risk to the benthic fauna exposed to these concentrations of pirimicarb, -endosulfan and chlorfenvinphos.

We suggest that the method presented here be used for the extraction and quantitation of particle-associated polar pesticides.     

用海泡石处理采油废水

用海泡石吸附法处理采油废水,考察了处理时间、海泡石加入量和采油废水pH对采油废水COD去除率的影响,并通过正交实验优化了采油废水处理工艺条件。通过正交实验得到的采油废水处理最佳工艺条件为：处理时间6h,粒径为150μm的海泡石加入量200g／L,采油废水pH9。在该条件下处理采油废水,COD去除率达到91％,处理后出水的COD为34．71mg／L,小于GB8978-1996（（污水综合排放标准》中的一级标准（60mg／L）。     

微波萃取技术在分析土壤中有机污染物的应用

介绍了微波萃取技术及其使用的试剂、设备和条件,对微波萃取在分析土壤中有机污染物的应用予以综述,阐述了微波萃取技术是分析土壤中有机污染物的好方法。     

底泥中多环芳烃(PAHs)提取方法评析

总结了底泥中多环芳烃(PAHs)提取的处理流程和国内外多种提取方法,比较了几种在我国较为常用的提取方法的效率.同时还提出了PAHs分离纯化的方法和步骤,并指出了提取过程中影响实验回收率的几个因素.     

浊点萃取分离富集荧光光度法测定水中α - 萘酚

基于非离子表面活性剂Triton X-114,采用浊点萃取分离富集荧光光度法测定水中α-萘酚,优化了影响浊点萃取的各种因素,包括样品酸度、表面活性剂体积分数、氢氧化钠溶液浓度、平衡温度和时间等,讨论了常见无机离子和可能共存的有机物的干扰。方法在0.010 mg/L～0.400 mg/L范围内线性良好,检出限为3.0μg/L,标准溶液测定的RSD为4.8%,水样加标回收率为94.3%～103%。     

固相萃取- GC/MS法测定水中邻苯二甲酸酯类

采用固相萃取-GC／MS法测定水中6种邻苯二甲酸酯类有机污染物,比较了不同固相萃取柱对萃取效果的影响,优化了水样pH值、水样流量、穿透体积、洗脱溶剂、洗脱剂体积、洗脱流量等萃取条件。方法在0．050μg/L-800μg/L范围内线性良好,检出限为0．008μg/L～0．03μg／L,标准溶液测定的RSD≤10．5％,实际水样加标回收率为80．0％-100％。     

ASE—GPC—GC—MS快速分析土壤中的PAHs

建立了土壤中多环芳烃的气相色谱—质谱联用的快速检测方法。样品经过加速溶剂萃取、凝胶色谱净化、GC—MS分离测定,优化了加速溶剂萃取和凝胶色谱净化的条件。结果表明,多环芳烃的平均回收率为82.1%~106.4%,相对标准偏差为1.2%~4.8%。方法具有灵敏度高、准确度好、快速、消耗溶剂少的优点,适用于土壤等固体样品中多环芳烃的分离、净化和分析。     

气相色谱-质谱法分析污水中溶解态有机物

采用0.45μm玻璃纤维滤膜将污水分离为悬浮态和溶解态有机物质,以二氯甲烷为萃取剂,采用液液萃取-气质联用法对污水中溶解态有机物进行测定,同时还对萃取条件(萃取次数,萃取时间,无机盐加入量)进行优化.结果表明:萃取回收率最高的是每个pH范围各萃取2次、静置5 min,氯化钠加入15g.该方法分析时间短,准确度好(样品平均加标回收率为91.1％ ～ 103％),精密度高(相对标准偏差小于5％),易于操作.     

顶空固相微萃取-气相色谱法测定水中氯苯类化合物

采用顶空固相微萃取（HS －SPME）技术萃取水中6种氯苯类化合物,全面分析对目标物萃取效率的影响因素,并确定萃取试验的最佳条件。用顶空固相微萃取联合气相色谱法（HS －SPME －GC）测定水中6种氯苯类化合物,方法在0.500 ng／L～2.00×10^5 ng／L范围内线性良好,检出限为0.05 ng／L ～2000 ng／L,空白样品加标回收率为69.8％～121％, RSD为4.8％～18.3％。用该方法测定实际水样,平行双样的相对偏差低于20％。