Isolation and Purification of Unstable Iridoid Glucosides from Traditional Chinese Medicine by Preparative High Performance Liquid Chromatography Coupled with Solid-phase Extraction

An efficient preparative method was successfully developed for isolation and purification of unstable components from medicinal plant extracts, using a combined method of preparative high performance liquid chro-matography(HPLC) and solid-phase extraction(SPE). The aim of this study was to obtain an effective method with high preparative efficiency and importantly to avoid the transformation of unstable compounds. The preparative HPLC system was based on an LC/MS controlled four-channel autopurification sys...     

Use of solid-phase extraction to enable enhanced detection of acyl homoserine lactones (AHLs) in environmental samples

A challenge for understanding the role of bacterial cell–cell signalling in the environment is the detection of those signals, which are often present in low (nmol L⁻¹) concentrations. We describe here a simple purification method, solid-phase extraction (SPE), for increasing the sensitivity of detection for one such group of signals, acyl homoserine lactones (AHLs), in environmental samples. Spiking of dried marine sponge tissue (Stylinos sp.) with AHLs resulted in detection down to 0.01 ppm for 3-oxo-hexanoyl homoserine lactone (3-oxo C₆-HSL) and 1 ppm for hexanoyl homoserine lactone (C₆-HSL). Compared with liquid extraction methods use of SPE resulted in twofold and tenfold improvements in sensitivity, respectively.     

Multi-walled carbon nanotubes as a solid-phase extraction adsorbent for the determination of chlorophenols in environmental water samples

Multi-walled carbon nanotubes (MWCNs) are used as adsorbent for solid-phase extraction (SPE) of several chlorophenols (CPs). CPs were adsorbed on MWCNs cartridge, then desorbed with pH 10.0 methanol, finally determined by HPLC. Under the optimized conditions, detection limits of 0.08-0.8 ng mL(-1) were obtained. The method had been applied to analyze the five CPs in tap water and river water.     

Analysis of earthy and musty odors in water samples by solid-phase microextraction coupled with gas chromatography/ion trap mass spectrometry

A method for the determination of the earthy and musty odors geosmin, 2-methylisoborneol (2-MIB), 2-isobutyl-3-methoxy pyrazine (IBMP), 2-isopropyl-3-methoxy pyrazine (IPMP) and 2,4,6-trichloroanisole (2,4,6-TCA) in water by headspace solid-phase microextraction (HSSPME) combined with gas chromatography-ion trap mass spectrometry (GC-ITMS) is described. Several parameters of the extraction and desorption procedure were studied and optimized (such as types of fibers, extraction temperature, extraction time, desorption temperature, desorption time, ionic strength and elutropic strength and pH of samples). The method shows good linearity over the concentration range 1-500 ng l⁻¹ and gives detection limits of sub-part per trillion levels for all compounds. Good precision (5.9-9.8%) is obtained using IBMP as internal standard. Finally, the method was successfully applied to analyze earthy and musty odors in tap water and lake water.     

固相微萃取涂层及其形貌特征研究

采用物理涂渍、溶胶-凝胶技术(sol-gel)制备了固相微萃取(SPME)固相涂层：),γ-Al2O3涂层、聚丙烯酸树脂涂层、聚酰亚胺-二氧化硅溶胶凝胶涂层、聚酰亚胺-二氧化钛涂层。通过扫描电镜显示涂层表面形貌,并比较了萃取容量与涂层形貌间的关系.证明涂层的微观形态结构对涂层性能具有一定的影响,可以通过微观形态分析,了解不同微观结构对宏观性质的影响。     

动态液相微萃取GC/MS-SIM方法检验毛发中的苯丙胺类毒品

建立了动态液相微萃取GC/MS-SIM方法检测毛发中4种苯丙胺类毒品的方法.毛发样品首先用1 mol/L NaOH溶液消解,然后用50μL氯仿涡旋提取1min,离心后用注射器直接抽取有机相,提取液进行GC/MS-SIM方法检测.毛发样品的测出限(S/N=3)分别为苯丙胺1 ng/mg,甲基苯丙胺、3、4-(亚甲二氧基)苯丙胺、3、4(亚甲二氧基)-甲基苯丙胺500 pg/mg.在毛发中添加上述4种苯丙胺毒品的质量分数为5 ng/mg时,5次测定的RSD分别为苯丙胺8.3%,甲基苯丙胺8.2%,3、4-(亚甲二氧基)苯丙胺2.0%,3、4(亚甲二氧基)2.7%.该方法可用于毛发中低含量苯丙胺类毒品的分析.     

固相微萃取技术与环境样品前处理

固相微萃取技术是80 年代末发展起来的一项新型的无溶剂化环境样品前处理技术, 它主要与气相色谱和高效液相色谱联用, 能快速和有效地分析环境样品中的痕量有机污染物。技术从出现至今主要在萃取装置(萃取纤维涂层)、萃取方式及后序分析仪器上有较大的发展和变化, 这使得技术的应用范围不断拓宽。通过对现有文献的总结, 本文还提出了固相微萃取技术今后的发展趋势。     

A new liquid-phase microextraction method based on solidification of floating organic drop

In the present study, a new and versatile liquid-phase microextraction method is described. This method requires very simple and cheap apparatus and also a small amount of organic solvent. Eight microliters of 1-undecanol was delivered to the surface of solution containing analytes and solution was stirred for a desired time. Then sample vial was cooled by inserting it into an ice bath for 5 min. The solidified 1-undecanol was transferred into a suitable vial and immediately melted; then, 2 μL of it was injected into a gas chromatograph for analysis.Some polycyclic aromatic hydrocarbons (PAHs) were used as model compounds for developing and evaluating of the method performance. Analysis was carried out by gas chromatography/flame ionization detection (GC/FID).Several factors influencing the microextraction efficiency, such as the nature and volume of organic solvent, the temperature and volume of sample solution, stirring rate and extraction time were investigated and optimized. The applicability of the technique was evaluated by determination of trace amounts of PAHs in environmental samples. Under the optimized conditions, the detection limits (LOD) of the method were in the range of 0.07-1.67 μg L⁻¹ and relative standard deviations (R.S.D.) for 10 μg L⁻¹ PAHs were <7%. A good linearity (r² > 0.995) in a calibration range of 0.25-300.00 μg L⁻¹ was obtained. After 30 min extraction duration, enrichment factors were in the range of 594-1940. Finally, the proposed method was applied to the determination of trace amounts of PAHs in several real water samples, and satisfactory results were resulted. Since very simple devices were used, this new technique is affordable, efficient, and convenient for extraction and determination of low concentrations of PAHs in water samples.     

Dispersive liquid-liquid microextraction followed by high-performance liquid chromatography as an efficient and sensitive technique for simultaneous determination of chloramphenicol and thiamphenicol in honey

Dispersive liquid-liquid microextraction (DLLME) coupled with high-performance liquid chromatography-variable wavelength detector (HPLC-VWD) was developed for extraction and determination of chloramphenicol (CAP) and thiamphenicol (THA) in honey. In this extraction method, 1.0 mL of acetonitrile (as dispersive solvent) containing 30 μL 1,1,2,2-tetrachloroethane (as extraction solution) was rapidly injected by syringe into a 5.00-mL water sample containing the analytes, thereby forming a cloudy solution. After extraction, phase separation was performed by centrifugation and the enriched analytes in the sedimented phase were determined by HPLC-VWD. Some important parameters, such as the nature and volume of extraction solvent and dispersive solvent, extraction time, sample solution pH, sample volume and salt effect were investigated and optimized. Under the optimum extraction condition, the method yields a linear calibration curve in the concentration range from 3 to 2000 μg kg⁻¹ for target analytes. The enrichment factors for CAP and THA were 68.2 and 87.9, and the limits of detection (S/N = 3) were 0.6 and 0.1 μg kg⁻¹, respectively. The relative standard deviations (RSDs) for the extraction of 10 μg kg⁻¹ of CAP and THA were 4.3% and 6.2% (n = 6). The main advantages of DLLME-HPLC method are simplicity of operation, rapidity, low cost, high enrichment factor, high recovery, good repeatability and extraction solvent volume at microliter level. Honey samples were successfully analyzed using the proposed method.     

An improved method for the simultaneous analysis of phenolic and steroidal estrogens in water and sediment

This paper describes an improved method for the extraction and analysis of seven endocrine disrupting chemicals with wide-ranging polarities from water and sediments using gas chromatography-tandem mass spectrometry (GC-MS/MS). The analytes were 4-tert-octylphenol, 4-nonylphenol, bisphenol A, estrone, 17β-estradiol, 17α-ethynylestradiol and 16α-hydroxyestrone. The optimised GC-MS/MS method produces increased selectivity and sensitivity compared to GC-MS, with limit of detection ranging from 0.01 to 0.49 ng L⁻¹ in water and from 0.05 to 0.14 ng g⁻¹ in sediment. Extraction from aqueous samples was performed by solid-phase extraction (SPE) and from sediment samples by microwave-assisted extraction (MAE). The improved method for the clean-up of sediment extracts carried out by SPE enhanced EDC recovery (86-102%) while reducing matrix interference and sample drying time. Derivatisation of final sample extracts was achieved using N,O-bis(trimethylsilyl)trifluoroacetamide and pyridine, and their stability was enhanced by reconstituting the derivatised extracts with hexane. The method was validated by spiking experiments which showed good recovery and reproducibility. The method was applied to samples taken from the Medway estuary in Kent, UK, where non-conservative behaviour of EDCs was demonstrated.