吹扫捕集-气相色谱法测定水中四氢呋喃

建立了吹扫捕集-气相色谱测定水中四氢呋喃的方法,不用有机溶剂萃取和浓缩,减少了损失和对环境的污染,具有灵敏度高、检出限低、定量准确、操作简便等特点。当进样量为5 mL时,检出限可达到0.18μg/L级,相对标准偏差为0.9%-4.0%,加标回收率在77.2%-100.8%之间。     

Sorption of lambda-cyhalothrin,cypermethrin, deltamethrin and fenvalerate to quartz,corundum, kaolinite and montmorillonite

Sorption to mineral surfaces may be important for retention and degradation of hydrophobic pesticides in subsoils and aquifers poor in organic matter. In this work the title pyrethroids have been used to investigate selective interactions with the surfaces of four minerals. Sorption of the four pyrethroids was quantified in batch experiments with initial pyrethroid concentrations of 1–100 μg/l. Sorption to centrifuge tubes used in the batch experiments accounted for 25–60% of total sorption. Net sorption was obtained from total sorption after subtracting the amounts of pyrethroids sorbed to centrifuge tubes used. All isotherms could be fitted by the Freundlich equation with n ranging between 0.9 and 1.1. Bonding affinities per unit surface area decreased in the order: corundum>quartz>montmorillonitekaolinite. A similar sequence as found for the total surface tension of the minerals. All minerals showed the same selectivity order with respect to sorption affinity of the four pyrethroids: lambda-cyhalothrin>deltamethrin>cypermethrin>fenvalerate, which shows that the most hydrophobic compound is sorbed most strongly. Stereochemical properties of the four pyrethroid formulations may also contribute to the selectivity pattern.     

粮食中绿麦隆残留量的气相色谱分析

本文用六氟丁酸酐直接衍生化气相色谱法测定粮食中绿麦隆农药残留量.粮食样品用甲醇-水提取.滤液用二氯甲烷或三氯甲烷-石油醚混合溶剂萃取,经硅镁吸附剂净化.以丙酮-石油醚为洗脱剂,洗脱液浓缩后用七氟丁酸酐直接衍生化,采用气相色谱法,电子捕获检测器测定.方法的线性范围为0—2.5μg·ml~(-1).对5g粮食样品,方法检出限为0.01mg·kg~(-1).对于小麦、玉米和大豆样品,加标回收率为82.4—91.2%,相对标准偏差为4.1—10.3%.对实际样品的测定和有关单位验证的结果表明,本方法适合于粮食中绿麦隆残留量的测定.     

气相色谱法中液体样品的进样技术

阐述了气相色谱中液体样品的4种进样技术。     

Recommendations for Monitoring of Polybrominated Diphenyl Ethers in the Canadian Environment

Polybrominated diphenyl ethers (PBDEs) have been reported in air, surface waters, suspended sediments, soil, sediment, fish, marine mammals, and bird eggs throughout Canada, from the St. Lawrence Estuary to the Strait of Georgia and the northernmost reaches of the Canadian Arctic. Canadian scientists have detected the presence of PBDEs in breast milk in every Canadian province. In fact, recent data on temporal trends strongly suggests that the concentrations of PBDEs are on the rise in the Canadian environment. These findings are similar to those reported in other nordic countries, and have prompted several countries to implement environmental monitoring programs. Among the key challenges currently facing Canada and other countries concerns how best to measure these chemicals in different matrices. In this paper, several analytical methods cited in the scientific literature for determining PBDE concentrations in different abiotic and biological matrices are reviewed. The critical criteria required for accurate determination of PBDEs in complex environmental matrices are discussed, including instrument sensitivity, reliability, potential interference's and the need for specialized instrumentation for the determination of compounds up to 975 Daltons. While a single analytical method that meets these and other criteria has not yet been perfected by scientists, GC/HRMS-based methods amenable to isotope dilution techniques warrant further refinement, and likely represent the best tools for future environmental monitoring programs.     

Magnitude of pesticidal contamination in winter vegetables from Hisar,Haryana

Monitoring of 80 winter vegetable samples during 1997–1998 for pesticidal contamination was carried out on GC-ECD and GC-NPD systems with capillary columns following multiresidueanalytical technique. The tested samples were found 100%contaminated with low but measurable amounts of pesticideresidues. Among the four major chemical groups, residue levels oforganophosphorous insecticides were highest followed bycarbamates, synthetic pyrethroids and organochlorines. About 32%of the samples showed contamination with organophosphorous andcarbamate insecticides above their respective MRL values. On thebasis of observations made in these studies, it is suggested thatmore extensive monitoring studies covering all vegetable cropsfrom different agro-climatic regions of the state be carried outto know exact level of pesticidal contamination, which may serveas basis for future policy on chemical use.     

环境大气中半/中等挥发性有机物(S/IVOCs)的测量技术进展

总结了环境大气中半/中等挥发性有机物（S/IVOCs）的主要测量技术及其进展,重点介绍了基于气相色谱技术和化学电离质谱技术的测量方法.S/IVOCs的测量主要由气相色谱技术开始发展,并随着质谱技术的发展而不断发展.基于气相色谱技术的测量方法,能够直接测量非极性化合物,但在面对组分多达千万种的复杂体系时,传统的一维色谱相对耗时,而且由于峰容量不够,峰重叠现象十分严重,难以实现全组分的准确分离.新近发展的多维分离系统如全二维气相色谱,通过正交的分离系统,能够实现复杂体系中物种组分的准确、快速分离.目前基于化学电离质谱技术的在线测量方法已经逐渐应用于S/IVOCs的测量,虽然在物种定性方面相对较弱,但其可提供高时间分辨率的测量结果,帮助分析S/IVOCs在大气中的快速变化.在未来的研究中,高时间分辨率和全组分准确测量是S/IVOCs研究的关键.     

污水中新精神活性物质的分析方法优化及验证

随着对传统毒品打击力度的增大,各种为规避现行法律管制而合成的新精神活性物质(new psychoactive substances,NPS)层出不穷.NPS被滥用后,经人体新陈代谢所生成的代谢产物和未被代谢的原药随尿液进入生活污水,从而汇入污水处理厂,经处理后被排入自然水体.因此在国内外以往相关研究的基础上,应用固相萃取和UPLC-MS/MS技术,建立并优化了污水中11种常见NPS的前处理及检测方法.比较了污水前处理条件(如SPE柱、样品p H值、淋洗和复溶等)对目标物回收率的影响.结果表明最优前处理条件为:选用Oasis MCX柱,在p H=2的条件下加载样品,用2 m L p H=2的超纯水和2m L甲醇淋洗SPE柱,400μL 20%的甲醇水溶液复溶.通过对目标物的保留时间、回收率、基质效应、检出限和定量限、精密度等指标的评价,说明优化后的前处理方法和C18-UPLC-MS/MS检测方法高效可靠.应用优化后的方法对北京市11家污水处理厂的进、出水样进行了分析,验证了方法的可靠性,为进一步开展NPS的污水流行病学研究及健康风险评价提供了参考依据.     

气相色谱法测定水中九种卤代乙酸类化合物研究

建立了液-液萃取气相色谱-双柱-双检测器法测定水中九种卤代乙酸类化合物的检测方法.40 ml水样经4 ml甲基叔丁基醚两次萃取,萃取液经10%硫酸-甲醇50℃衍生后,用气相色谱电子捕获检测器检测.方法检出限为0.6~1.0μg/L,加标回收率75.9%~111%,6次测定的相对标准偏差≤16%.两次萃取显著提高了一氯乙酸和一溴乙酸的回收率,双柱-双检测器有效排除实际样品中假阳性结果,检测结果更准确可靠.     

SPE-GC-MS法对渤海水体中有机锡化合物的痕量分析

摘要：文中采用GC-MS仪器测定方法对海水中六种不同形态有机锡化舍物进行分析。在确定的GC-MS测定方法基础上得到SPE条件优化：选择NH。DDC鳌合剂,用5％的甲醇为携带剂,流速15ml／min,萃取温度45℃,萃取压力300bar,萃取时间为15min．