茶叶中三氯杀螨醇残留量的微波萃取-固相微萃取-气相色谱快速检测方法

建立了微波辅助萃取-固相微萃取-气相色谱/电子捕获检测法快速测定茶叶中三氯杀螨醇的方法。采用自制的PDMS萃取头,优化了萃取溶剂的种类,微波辐射时间和微波功率等微波辅助萃取条件;研究了SPME萃取时间、搅拌速度、离子强度、解吸温度和解吸时间对萃取效率的影响。方法对三氯杀螨醇的检出限为0.048 ng/mL,线性范围为0.2~200 ng/mL。在优化的实验条件下,对乌龙茶进行添加回收试验,平均回收率为61.3%~72.8%,相对标准偏差为8.0%~16.3%。本方法适合于茶叶中痕量三氯杀螨醇快速检测。     

微波加热对以槲皮素为甙元的黄酮甙的稳定性的影响

以乙醇为溶剂．分别采取微波和回流加热萃取法从番石榴叶中萃取槲皮素．高效液相色谱法测定槲皮素的萃取收率。对回流萃取液进行微波加热．槲皮素收率随微波加热温度的增加而显著增加。分别测定了温度为100、110、120℃的微波萃取动力学曲线以及60、70和78℃的回流加热萃取动力学曲线,计算结果显示,微波萃取和回流加热萃取均符合一级动力学方程,微波萃取槲皮素的活化能是回流加热萃取活化能的2倍多．平均表观速率常数是回流加热萃取的125倍。计算得到的活化能数据和实验结果均显示微波加热产生的高温可导致以槲皮素为甙元的黄酮甙发生分解。     

烟草中有机氯类农药多残留分析前处理方法对比研究

以烟草中有机氯类农药为研究对象,从检出限、回收率、重复性和色谱图4个方面系统比较了机械振荡萃取法、超声波溶剂萃取法、微波辅助萃取法和加速溶剂萃取法4种常用前处理方法。由于加速溶剂萃取法是在高温高压下进行萃取,在提取出残留农药的同时,也提取出更多的干扰物。机械振荡法、超声波溶剂萃取法和微波辅助萃取法各项结果差别较小,其中机械振荡萃取法回收率和重复性最好,但提取时间较长。考虑溶剂消耗和提取时间等方面的因素,微波辅助萃取是较理想的样品前处理方法。     

微波辅助萃取-固相微萃取联用气相色谱-质谱法测定土壤中的扑草净

研究了微波辅助萃取-固相微萃取联用、气相色谱-质谱联用测定土壤中除草剂扑草净的分析方法。采用正交设计实验优化了萃取溶剂种类和体积、微波辐射时间和微波功率等微波辅助萃取条件;研究了SPME萃取涂层、搅拌速度、萃取时间和解吸时间等对萃取效率的影响。方法的检出限为0．01ng／g;线性范围为0．2—200μg／L。在优化的条件下测定了5和50ng/g的合成土壤样品,回收率分别为90．1％和91.6％;相对标准偏差分别为9．4％和8．8％(n=6)。本法综合了微波辅助萃取和固相微萃取的优点,操作简便．灵敏度高,特别适合于固体样品中痕量有机物的萃取分离。     

加速溶剂萃取-气相色谱-质谱法测定土壤中醚类杀虫剂

农药的使用,对发展现代农业起到了积极作用,但是其大量使用甚至滥用,不仅对环境造成严重的污染,同时对人体健康造成危害,因此,对农药进行分析和检测十分必要[1]。固相基质(土壤等)的萃取方法主要有索氏提取[2]、超声辅助萃取[3]、微波辅助萃取[4]、超临界萃取[5]和加速溶剂萃取[6]等。加速溶剂萃取是在较高温度(50℃~200℃)、较高压力(6.89~20.68MPa)下对样品进行萃取,溶剂用量     

微波辅助萃取与超声波萃取丹参中丹酚酸B的比较研究

本文对微波辅助萃取和超声波萃取丹参中丹酚酸B进行了比较研究,并用高效液相色谱法(HPLC)测定了丹参中丹酚酸B.考察了微波辅助萃取和超声波萃取参数的影响,在各自最佳萃取条件下进行了丹参中的丹酚酸B提取率的比对,结果表明:微波辅助萃取6 min的提取率高于超声波萃取30 min的提取率.微波辅助萃取法与超声波萃取法相比具有省时、高效和溶剂用量少的特点.利用指纹图谱比较了两种萃取方式提取的化学成分的差异,结果显示两种萃取方法提取的主要成分组成基本相同,其共有成分比例相近.     

微波辅助萃取鬼箭羽叶中芦丁和槲皮素

建立了鬼箭羽中主要有效成分芦丁和槲皮素的MAE-HPLC定量分析方法, 该方法具有测定准确、操作简便和分析速度快等优点. 此外, 利用扫描电镜观察了鬼箭羽叶经微波辅助萃取后植物结构的变化, 初步证明了微波辅助萃取鬼箭羽叶的萃取机理符合细胞破壁学说.     

微波辅助萃取/样品前处理联用技术的研究进展

微波辅助萃取是近年来新发展的一种样品前处理技术,随着微波辅助萃取的发展和成熟,它与其它样品前处理技术的联用得到了迅速发展。与传统前处理方法相比,这些联用方法具有快速、高效、操作简便、节省溶剂、选择性好、应用范围广的特点。该文综述了微波辅助萃取及其与其它样品前处理技术联用的特点及适用性,并对近年来微波辅助萃取与其它前处理方法联用的发展概况及在分析领域中的应用情况进行了详细总结。     

赤芍及其相关药对中挥发油成分的研究

运用微波辅助萃取从赤芍及其相关药对中提取了挥发油,通过GC-MS检测,确定了主要成分及相对含量。结果表明,赤芍挥发油主要成分是水杨醛,在赤芍-川芎药对挥发油中它仍占较大比重。微波辅助萃取大大缩短了提取时间和提高了提取效率。     

微波辅助萃取应用研究进展

近年来关于微波辅助萃取(MAE)与其他各种样品前处理技术的结合使用,以及与多种检测技术在线联用的研究越来越多,此外离子液体等新型绿色溶剂作为萃取剂在MAE中的应用也开始得到广泛关注.本文综述了近几年微波辅助萃取在环境、天然产物提取、食品和药物分析领域的应用情况,并对其将来的发展进行了展望.     

三丁基氧化膦-离子液体体系萃取UO2(NO3)2的机理和选择性

研究了三辛基氧化膦(TOPO)和三丁基氧化膦(TBPO)在离子液体(ILs) 1-烷基-3-甲基咪唑双三氟甲基磺酰亚胺盐(C_nmimNTf₂, n=2, 4, 6, 8)中萃取分离UO₂(NO₃)₂. TOPO-C₂mimNTf₂和TOPO-C₄mimNTf₂体系萃取UO₂(NO₃)₂时会出现三相, 而TBPO萃取UO₂(NO₃)₂的萃合物可以很好地溶解在所有离子液体中. 论文也考察了萃取过程中的萃取剂浓度效应、酸效应、盐效应. 水相加入HNO₃会降低萃取效率. 盐效应证明了萃取是一种阳离子交换机理. 水相中加入NO₃^-能够提高U的萃取, 这说明NO₃^-参与萃取. 选择性研究表明: 除了在高酸度下对Zr 的显著萃取, TBPO-C₄mimNTf₂萃取体系在低酸度下对U呈现较好的选择性; 去除U后, 在低酸度下该体系对三价Nd 仍保持较好的选择性. 通过定量比较离子液体中NO₃^-进入量, 电喷雾质谱(ESI-MS)和紫外光谱表征确定了TBPO-C_nmimNTf₂中萃取机理的差异性. 萃取中存在两种萃合物, 即UO₂(TBPO)₃(NO₃)⁺和UO₂(TBPO)₃²⁺, 其中UO₂(TBPO)₃(NO₃)⁺的比例从C₂mimNTf₂体系到C₈mimNTf₂体系逐渐增加.     

Comparison of Conventional,Ultrasound- and Microwave-Assisted Extraction Techniques Applied for the Determination of Metals in Spruce Needles

In the present study the extraction of trace and major elements (Al, B, Ba, Ca, Cd, Cr, Cu, Fe, Mg, Mn, Ni, Pb, Sr, Ti, V and Zn) from spruce (Picea) needle samples under various experimental conditions, i.e., extractant, temperature and time of extraction, was examined. The effectiveness of conventional, ultrasound- and microwave-assisted extraction techniques was investigated. The replacement of a sample decomposition procedure by leaching prior to multielemental analysis by ICP-AES as well as the aspect of fractionation analysis is discussed. Standard Reference Material (CRM 101-Norway spruce needles) was used for validation of the applied analytical procedures.     

Membrane approach to solid-phase extractions

A novel material for separations has been developed in which efficient chromatographic particles are enmeshed in a network of PTFE fibrils to form a strong, porous sheet or “membrane”. The membrane can have a variety of sorptive or reactive properties, which are determined by the characteristics of the particulate chosen. The membranes, in the form of 47- or 25-mm disks, are used with standard filtration equipment. The use of hydrophobic octyl- and octadecyl-bonded silica particulates for reversed-phase extractions of environmental pollutants from an aqueous matrix, replacing conventional liquid-liquid extraction (LLE) is described. The water sample is filtered through the disk and adsorbed organic species are eluted from the disk with a small volume of an appropriate solvent for subsequent chromatographic separation. The technique is rapid, less labor intensive then LLE and eliminates the need for large volumes of hazardous and expensive solvents. Specific applications investigated include the analysis of ground, surface and tap waters for pesticides, polychlorinated biphenyls and phthalates at the μg l^?1 level.     

Optimizing conditions for the extraction of catechins from green tea using hot water

Six different factors involved in the extraction of catechins from green tea using water were examined for their impact on the yield of catechins and on the efficiency of water use. The best temperature and time combination for catechin extraction was at 80°C for 30 min. The yield of catechins was also optimal with a tea particle size of 1 mm, a brewing solution pH <6 and a tea‐to‐water ratio at 50:1 (mL/g). In terms of efficient use of water in a single extraction, a water‐to‐tea ratio of 20:1 (mL/g) gave the best results; 2.5 times less water was used per gram of green tea. At the water‐to‐tea ratio of 20:1 mL/g, the highest yield of catechins per gram of green tea was achieved by extracting the same sample of green tea twice. However, for the most efficient use of water, the best extraction was found to be once at a water‐to‐tea ratio of 12:1 (mL/g) and once at a water‐to‐tea ratio of 8:1 (mL/g). Therefore, all six of the factors investigated had an impact on the yield of catechins extracted from green tea using water and two had an impact on the efficiency of water use.     

Advanced analytical techniques for the extraction and characterization of plant‐derived essential oils by gas chromatography with mass spectrometry

In recent years, essential oils have received a growing interest because of the positive health effects of their novel characteristics such as antibacterial, antifungal, and antioxidant activities. For the extraction of plant‐derived essential oils, there is the need of advanced analytical techniques and innovative methodologies. An exhaustive study of hydrodistillation, supercritical fluid extraction, ultrasound‐ and microwave‐assisted extraction, solid‐phase microextraction, pressurized liquid extraction, pressurized hot water extraction, liquid–liquid extraction, liquid‐phase microextraction, matrix solid‐phase dispersion, and gas chromatography (one‐ and two‐dimensional) hyphenated with mass spectrometry for the extraction through various plant species and analysis of essential oils has been provided in this review. Essential oils are composed of mainly terpenes and terpenoids with low‐molecular‐weight aromatic and aliphatic constituents that are particularly important for public health.     

Study of enrichment factors for six β‐blockers in aliphatic alcohols by hollow‐fiber liquid‐phase microextraction

The selectivity of a suitable organic solvent is key for extraction in liquid‐phase microextraction experiments. Nevertheless, the screening process remains a daunting task. Our research aimed to study the relationship between extraction efficiency and extraction solvents, analytes, and finally select the appropriate extraction solvent. In the present article, β‐blockers and six extraction solvents were chosen as the models and hollow‐fiber liquid‐phase microextraction was conducted. The relationship was built by statistical analysis on the data. Factors affecting extraction efficiency including the logarithms of the octanol/water partition coefficient (logP_o/w) of analytes, acid dissociation constants, the logarithms of the octanol/water partition coefficient of solvents and pH of the sample solution were investigated. The results showed that a low water solubility of extraction solvent is the foundation to ensure higher extraction efficiency. Moreover, when ΔlogP_o/w > 0, a higher extraction efficiency is observed at lower ΔlogP_o/w, on the contrary, when ΔlogP_o/w < 0, extraction efficiency is higher as the absolute value of ΔlogP_o/w becomes greater. Finally, the relationship between enrichment factor and extraction solvents, analytes was established and a helpful guidance was provided for the selection of an optimal solvent to obtain the best extraction efficiency by liquid‐phase microextraction.     

Physicochemical Principles of Extraction with Supercritical Gases

The present review considers some physicochemical properties of fluid mixtures that are of importance for fluid extraction and supercitical fluid chromatography (SFC). Firstly, the important types of phase diagrams are treated, the occurrence of solid phases also being considered in some simple cases. Specific examples are given of mixtures of a highly volatile component I (e.g. CO₂, C₂H₆) with a relatively involatile component II (e.g. squalane) of very different molecular size, shape, structure, and/or polarity, and it is shown how the rather complicated types of phase diagrams can be calculated and correlated. The importance of fluid mixtures extends far beyond the fields of science and technology reviewed.     

Clean up Procedures for Determination of Amphetamine in Urine Samples.

ABSTRACT

A comparative study of the main sample preparation techniques used for spectrofluorimetric amphetamine determination in urine is presented. The advantages and disadvantages of three procedures based on liquid-liquid or solid-liquid extraction are tested, and a method for amphetamine determination in presence of methamphetamine and its metabolites is proposed. The results obtained are in agreement with the theoretical contents (spiked samples) or the results provided by a reference (GC) method (r8543161 sample).     

Efficiency of Different Methods and Solvents for the Extraction of Polycyclic Aromatic Hydrocarbons from Soils

The efficiencies of supercritical fluid extraction (SFE), accelerated solvent extraction (ASE), Soxhlet, and ultrasonic extraction in the analysis of polycyclic aromatic hydrocarbons (PAHs) in soils were evaluated. Solvents with different polarity were used to extract the PAHs from two soils, one with high and one with low contamination level. ASE showed good results with all solvents almost independent of the solvent polarity and the best results with acetone-toluene (1 : 1). Ultrasonic extraction with acetone-toluene for the uncontaminated soil and acetone-ethanolamine for the highly contaminated also showed good recoveries. The time-consuming Soxhlet extraction with pentane or dichloromethane was less effective. The PAH recovery from SFE was related to the soil matrix or the contamination level. The best extraction conditions (CO 2 /10% pentane) are successful for the soil with a low contamination level and a high humic acid content whereas the extractions of the highly contaminated soil gave poor results irrespective of the solvent used.