基于微流控芯片的液相微萃取的研究进展

微流控芯片通过微通道网络,将样品的采集、混合、反应、分离和富集等分析过程集成在芯片上完成,为化学反应的微型化提供了一个良好的操作平台。利用液体在微观尺度下表现出的特殊的表面物理性质,将液相微萃取技术移植到微流控芯片上,可以实现小体积样品中低含量目标分析物的萃取。本文介绍了基于微流控芯片的液相微萃取近年的研究进展,并总结了层流、液滴、捕陷液滴几种基本的萃取模式。     

Extraction of oleic acid from soybean oil and jojoba oil-phase diagrams

Formamide,N-methylformamide,N-dimethylformamide, dimethylsulfoxide, 1,2-butanediol, and 2-butane-1,4-diol were considered as potential extractants of fatty acids from soybean and jojoba oils. Ternary liquid-liquid phase diagrams at 298.15 K, distribution, and selectivity coefficients of oleic acid are reported. Of the investigated solvents, onlyN-methylformamide and 1,2-butanediol have desirable extraction characteristics.     

凝固分散液液微萃取-HPLC法测定水中萘芴菲

建立了凝固分散液液微萃取(SFO-DLLME)-高效液相色谱法(HPLC)测定水中萘、芴和菲的新方法。以1-十二醇为萃取剂,甲醇为分散剂,优化了影响SFO-DLLME萃取效率的因素。在最佳条件下,萘、芴和菲的检出限分别为0.011、0.056、0.049μg/L,萘的线性范围为0.1~50.0μg/L,芴和菲的线性范围为1.0~500μg/L。实际水样加标回收率78.6%~95.1%,相对标准偏差(n=5)3.9%~7.2%。方法简便快速,灵敏度高,环境友好,成功用于实际水样分析。     

顶空-固相微萃取法测定地表水中四乙基铅

建立了满足地表水中四乙基铅限值要求的"顶空-固相微萃取-气质联用法".分析结果表明:采用空调及水浴控温使萃取温度恒定在23.0～24.5℃范围内,结合内标法进行定量分析,标准曲线线性关系良好(r=0.9995),检出限(3.143SD)为O.085μg/L;河流及水库水水样的加标回收率为93.2%～128%,加标样品平...     

微通道内液-液两相流研究进展

从流型、传质和应用3个方面,介绍了近年来微通道内液-液两相流的研究进展。液-液两相流型研究内容主要有两部分,即流型的观察、流型谱图的绘制以及考察多种因素对流型的影响,但是具有普适性的流型谱图和流型转变线仍未提出。液-液两相传质研究方法包括实验研究和数值模拟两种,主要研究在液滴流、弹状流和平行流3种稳定流型下的传质过程;且相对于定性研究,定量的传质研究较少。对于微通道内液-液两相流应用研究,主要体现在萃取、材料合成、生物结晶等方面。此外,对今后微通道内液-液两相的流型、传质和应用研究进行了展望,指出需从实验与模拟计算相结合以及拓展微通道内液-液两相流的应用研究两个方面进行深入研究,推进其工业化进程。     

新型复合T型管对液液二相流的分离

T型管分离器是一类新型的二相流分离器,具有集约、连续、简单、经济、安全以及安装、更新、维护方便等优点,缺点是简单T型管作为分离器在分离二相流时的分离效率往往不高,只能起到部分分离的作用。新型复合T型管是对简单T型管的一种改进,以期能提高二相流的分离效率。以煤油和水为液液二相工作介质,用主管水平,侧支管垂直向上的简单T型管和复合T型管作为二相流分离器,在分层流和有混合界面的分层流的二相流型条件下,进行二相流的相分离实验。实验结果表明:2种流型下复合T型管对二相流的分离效果都比简单T型管好,增加复合T型管的连接管数,能进一步提高分离效率;在分层流时连接管数为5管及以上的复合T就能将液液二相完全分离;入口流型中二相的混合程度越高,最高分离效率越低;水相体积分数对分离效率的影响与流型相关。复合T型管分离液液二相流技术具有很好的工业应用前景。     

Virgin rapeseed oils obtained from different rape varieties by cold pressed method – their characteristics,properties, and differences

The aim of the present study was to compare different rape varieties. For this purpose oil from six different varieties of rapeseeds was cold pressed under laboratory conditions. In the obtained rapeseed oils the fatty acids composition and minor components, characteristic values (acid value; AV and TOTOX), oxidative stability (DSC test), and volatiles were determined and a sensory evaluation was carried out. The highest oxidative stability was found for oil from sample 5 (IP = 158 min), which also has the lowest amount of C18:3 (7.8%), chlorophylls (0.083 mg/kg), and metals (Cu²⁺ 0.02 mg/kg and Fe²⁺ 0.08 mg/kg). This oil has also the lowest AV (0.17 mg KOH/g), which may be related to the lowest moisture content of the seeds prior to extraction. It was characterized by the highest rapeseed flavor intensity. The lowest induction period was observed for samples 3 and 6 (100 min). Although sample 3 had the same low level of metals as sample 5 and the highest concentration of tocopherols (635 mg/kg), PUFA (33.9%), and AV (1.37 mg KOH/g) it also had the lowest intensity of rapeseed flavor among the analyzed oils. Sample 6, despite its low percentage of PUFA (24.7%), conjugated diens and triens, and the lowest content of total volatiles (0.4Vs), had the highest concentration of metals (Cu²⁺ 0.04 mg/kg and Fe²⁺ 0.34 mg/kg).     

液相微萃取-GC-MS法测定水中的杀真菌剂类农药

用中空纤维膜液相微萃取一气相色谱质谱法测定水中的杀真菌剂类农药（乙烯菌核利、腐酶利）。通过试验选择甲苯为萃取剂,研究了萃取剂的选取及其用量、萃取温度、萃取时间、搅拌速度对萃取的影响。在最佳条件下富集倍数为：乙烯菌核利134倍、腐酶利209倍。方法的线性范围为0．50—1001μg·L-1,检出限为0．05和0．08μg·L-1,测定实际水样加标回收率分别为87．1％和86．3％、相对标准偏差≤9．43％,此方法简单、快速、成本低,可用于水中的杀真菌剂类农药的快速检测。     

Et-Ph-BCTABipy的合成及其对Pd2+的萃取性能

合成了N,N′-二乙基-N,N′-二苯基-［2,2′-联吡啶］-6,6′-二硫代酰胺(Et-Ph-BCTABipy)萃取剂,并利用¹³C NMR和¹H NMR对其进行了表征;研究了相接触时间、萃取剂浓度、水相初始酸度和Pd²⁺浓度等因素对Et-Ph-BCTABipy萃取Pd²⁺性能的影响,利用摩尔比法确定了Et-Ph-BCTABipy与Pd²⁺所形成的配合物组成;同时,在Ln(Ⅲ)与Pd²⁺共存体系中研究了Et-Ph-BCTABipy对Pd²⁺的萃取选择性。结果表明：Et-Ph-BCTABipy在HNO₃体系中对Pd²⁺具有较强的萃取性能和较高的萃取选择性;萃取过程中Et-Ph-BCTABipy与Pd²⁺以1∶2的比例结合,其萃取平衡常数K_ex=3.42×10⁶。     

Magnetic nanocellulose hybrid nanoparticles and ionic liquid for extraction of neonicotinoid insecticides from milk samples prior to determination by liquid chromatography-mass spectrometry

A simple and rapid microextraction procedure is reported on the use of ionic liquid in combination with magnetic nanocellulose hybrid nanoparticles. The procedure is ultrasound-assisted and applicable to selective preconcentration of neonicotinoid insecticides from milk samples, prior to being analysed by liquid chromatography-mass spectrometry. The extraction procedure uses small volume of organic solvents (<1 mL), and there is no need for centrifugation. In the experimental approach the ionic liquid was quickly disrupted by an ultrasonic probe and dispersed in milk samples in a cloudy form. At this stage, neonicotinoid insecticides were extracted into the fine droplets of ionic liquid. Then small amounts of magnetic nanocellulose hybrid nanoparticles were dispersed into the sample solutions to adsorb the ionic liquid containing the analytes and phase separation was completed. The ionic liquid allowed the microextraction of the analytes and a small volume of acetonitrile was used for elution. Magnetic nanocellulose favoured the adsorption of the ionic liquid with the analytes and improved the final recovery with respect to the use of simple magnetic nanoparticles as a sorbent material. Under the optimum conditions, decision capabilities were achieved in the 0.02–0.06 mg kg^?1 range, with recoveries between 91.0% and 109.5%.