预富集技术在原子吸收光谱环境分析中的应用

原子吸收光谱法是分析环境水样中金属离子含量的有效方法之一。在测定时往往需要对样品进行前处理,然后再进行测定。文章介绍了近些年较新的一些分离富集技术在原子吸收光谱分析环境中金属离子时的应用,分析了离子交换树脂在样品中金属离子富集分离过程中的研究近况,评述了固相萃取、析相微萃取、单滴液滴微萃取、分散液液微萃取、离子液体萃取、浊点萃取等多种萃取方式在样品预富集中的应用进展,综述了活性炭、纳米粒子、淀粉、分子筛等吸附剂在富集环境水样中金属元素的应用现状,同时还对在线富集技术与流动注射分析技术联用在金属元素分析中的应用进展进行了评述。     

河水-地下水交互带沉积物中抗生素和代谢产物提取方法优化及其分布特征

河水-地下水交互带是污染物发生富集、降解和转化等生物地球化学过程的重要场所.抗生素作为一类广泛关注的有机污染物,探索其在交互带中的分布特征对认识特殊生境下污染物迁移转化过程具有重要意义.由于交互带氧化还原条件变化敏感,沉积物组成特殊,建立了一种有效提取交互带中22种抗生素及4种磺胺类代谢产物的前处理方法,并对样品初始状态、提取温度、提取液p H值以及有机提取溶剂进行了优化.同时对汉江下游河水-地下水交互带沉积物中的抗生素含量进行分析,结果表明,采用p H=3的乙腈/乙二胺四乙酸二钠(Na₂EDTA)-Mcllvaine缓冲液(1∶1,体积比)对未经氧化的沉积物原样在40℃条件下进行3次微波提取,目标抗生素的回收效果最好.汉江下游交互带沉积物中共检出11种抗生素,其中以土霉素(OTC)和氧氟沙星(OFL)为主,最高检出含量分别为6.77 ng·g^-1和5.81 ng·g^-1.不同交互剖面中抗生素含量的垂向分布差异较大,主要与沉积物岩性、抗生素理化性质和地表水-地下水交互作用等影响因素有关.     

超临界二氧化碳萃取－GC／MS测定土壤中的多环芳烃

本文开发了一种采用超临界二氧化碳萃取土壤中多环芳烃、不须经过纯化步骤,直接可用于ＧＣ／ＭＳ分析的简便、高效的方法。本实验中超临界革取的流体是二氧化碳,改善剂是５％的二氯甲烷／甲醇,萃取温度为１２０℃、压力为３４ＭＰａ。ＧＣ／ＭＳ分析时除了采用外标外,还加入了６种同位素ＰＡＨｓ内标以校正各段ＰＡＨｓ的响应因子。采用本方法成功地测定了我国未开垦森林土壤中的ＰＡＨｓ。     

石墨炉原子吸收光谱法测定海河下游水中痕量镉

原子吸收光谱法直接测定高盐水中痕量镉时,有很大背景吸收和误差。本文采用络合—萃取技术使共存元素与待测元素分离,既消除了基体干扰,又达到了富集作用,使测定结果准确可靠。     

A miniature stainless steel net dumbbell-shaped stir-bar for the extraction of phthalate esters in instant noodle and rice soup samples

Abstract

This work reports the development of a very-simple-to-construct stir-bar extraction device so called “a dumbbell-shaped stainless steel stir-bar.” The extraction device was assembled from a rolled up stainless steel net filled with an XAD-2 sorbent and a metal rod to allow the use of a magnetic stirrer during extraction. The dumbbell-shaped stainless steel stir-bar was used to extract diethyl phthalate (DEP), dibutyl phthalate (DBP), and di(2-ethylhexyl) phthalate (DEHP) before analysis by a gas chromatograph equipped with an electron capture detector (GD-ECD). Under the optimal conditions, the developed method provided a good linearity from 10.0 to 1,000.0?ng mL^?1 for all three compounds. Limits of detection and limits of quantification were 9.37?±?0.29?ng mL^?1 and 31.22?±?0.95?ng mL^?1 for DEP, 5.73?±?0.31?ng mL^?1 and 19.1?±?1.0?ng mL^?1 for DBP and 3.30?±?0.06?ng mL^?1 and 11.0?±?0.19?ng mL^?1 for DEHP, respectively. Good recoveries in the range of 81.89?±?0.17 to 109.5?±?2.0% were achieved when the method was used to extract phthalate esters in five instant noodle and two rice soup samples.     

金黄色葡萄球菌的演相培养及A蛋白的提取

对金黄色葡萄球菌（Ｓｔａｐｈｙｌｏｃｏｃｃｕｓａｕｒｅｕｓ）ＣｏｗａｎⅠ的培养及Ａ蛋白提取工艺进行了优化研究．结果表明：在培养基中分别增加牛肉膏和蛋白陈的含量，有利于提高菌体生物量及Ａ蛋白的得率；少量酵母浸膏及葡萄糖对生物量及Ａ蛋白得率有促进作用，但当达到一定浓度时则会产生基质抑制作用；恒定培养过程的ｐＨ值有利于Ａ蛋白得率的增加，０．０３（）／ｍｉｎ通气量、搅拌速度２００ｒ／ｍｉｎ是能满足菌体生长的条件．根据Ａ蛋白耐热性强这一特性，采用加热法除去大部分杂质，然后用ＩｇＧ－琼脂糖凝胶亲和层析实现了Ａ蛋白的提纯．     

Determination of particulate polycyclic aromatic hydrocarbons in ambient air by gas chromatography-mass spectrometry after molecularly imprinted polymer extraction

A solid phase extraction procedure (SPE) is described for the quantitative analysis of polycyclic aromatic hydrocarbons (PAHs) in atmospheric particulate matter (PM), as ubiquitous environmental pollutants routinely measured in air quality monitoring. A SPE cartridge was used based on a molecular imprinted polymer (MIP-SPE) properly tailored for selective retention of PAHs with 4 and more benzene fused rings. The performance of the clean-up procedure was evaluated with the specific concern of selective purification towards saturated hydrocarbons, which are the PM components mostly interfering GC analysis of target PAHs. Under optimized operative conditions, the MIP-SPE provided analyte recovery close to 95% for heavier PAHs, from benzo(α)pyrene to benzo(ghi)perylene, and close to 90% for four benzene rings PAHs, with good reproducibility (RSDs: 2.5%-5.9%). Otherwise, C₁₇-C₃₂ n-alkanes were nearly completely removed. The proposed method was critically compared with Solid Phase Micro Extraction (SPME) using a polyacrylate fiber. Both methods were successfully applied to the analysis of ambient PM_2.5 samples collected at an urban polluted site. Between the two procedures, the MIP-SPE provided the highest recovery (R% ≥ 93%) for PAHs with 5 and more benzene rings, but lower for lighter PAHs. In contrast, SPME showed a mean acceptable R% value (∼ 80%) for all the investigated PAHs, except for the heaviest PAHs in the most polluted samples (R%: 110%-138%), suggesting an incomplete purification from the interfering n-hydrocarbons.     

Chemical forms of cobalt and nickel extracted by M1, M3 and CaCl2 DTPA

Mehlich 1(M1), mehlich 3(M3) and CaCl₂ DTPA have been used to predict the available micronutrient in soil. However, the forms of micronutrient extractable by these extractants are not known. In the present study, ten soils, collected from five provinces and the capital of China, representing a wide range of chemical and physical properties, were analyzed by sequential extraction to isolate five forms of cobalt and nickel, they are exchangeable, carbonate bound, Fe Mn oxide bound, organically bound and residual forms. The chemical forms extracted by M1, M3 and CaCl₂ DTPA were also investigated. The results show strong correlation between the carbonate bound or organically bound forms of Co or Ni and the amounts of extractable by any of the above three extractants. The main forms extracted by these extractants are carbonate and organically bound forms. The ranking of these three extractants for extraction of Co and Ni are M1>M3=CaCl₂ DTPA and M1=M3>CaCl₂ DTPA, respectively.     

环境水样中邻苯二甲酸二辛酯GC测定固相萃取条件优化研究

借助于均匀设计法合理安排试验,再应用计算机回归技术进行C18柱固相萃取条件的设计和优化研究,建立相关的数学模型,找出了各因素对回收率的影响规律。成功地确定(正己烷:丙酮)配比17∶1、洗脱体积2.0m l、洗脱速率6.0m l.m in-1、上样速率9.0m l.m in-1为优化的萃取条件,此时得到DEHP和DnOP的回收率分别为91.98%、107.3%。     

高效液相色谱法测定水中微量酚

本文报道了水中11种微量酚的高效液相色谱测定方法。用氯化四丁基按作为阳离子对萃取剂。二氯甲烷章取水中微量酚，除本酚外，水中10种微量酚的回收率大于90％。用MicropakMCH－5色谱柱，醋酸—水—乙睛流动相，uv254um和280um双波长检测，流速1ml／min下，对水中11种微量酚进行了分离和定量、11种酚的检测极限是0.1mg／L～1.26mg／L；检测范围为0.1mg／L～7mg／L。对2—甲基—4，6—二硝基酚的峰高与浓度进行了线性回归，γ＝0.9993；该法适用于水中11种微量酚的同时测定。