Preparation and characteristics of sol–gel-coated calix[4]arene fiber for solid-phase microextraction

Li, Xiujuan; Zeng, Zhaorui; Gao, Shengzhe; Li, Haibing

doi:10.1016/j.chroma.2003.09.042

Cited by 105 publications

(30 citation statements)

References 41 publications

(73 reference statements)

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“…The highest percent of amount of calix [4]arene in both a C [4]/OH-TSO coating [10] and an amide bridged-C [4]/ OH-TSO coating [14] is 11%. The level of calixarene is determined mainly by the reaction of calixarene and the coprecursor 3-(2-cyclooxypropoxyl)propyltrimethoxysilane (KH-560), in terms of their chemical reactivity at room temperature and the steric hindrance of calixarene when incorporated into the sol-gel network which links together through the calix [4]arene phenol oxygens.…”

Section: Introductionmentioning

confidence: 98%

“…The fused silica fiber was pretreated according to the method described in [10]. The sol-gel solution was prepared as follows: an appropriate amount of diglycidyloxy-C [4] (25.6 and 51.2 mg, respectively) and 50 mg of KH-550 were dissolved in 400 μL of methylene chloride by ultrasonic agitation and reacted in a polypropylene plastic tube at room temperature for 20 min.…”

Section: Soil Collection and Preparationmentioning

confidence: 99%

“…Two kinds of calixarenes have recently been used to prepare SPME fibers by sol-gel technology, and these have demonstrated high sensitivity and selectivity to aromatics and chlorinated aromatic compounds such as chlorophenols and organochlorine pesticides and their metabolites, which in turn leads to low detection limits (ng/L) [10][11][12][13][14][15].…”

Section: Introductionmentioning

confidence: 99%

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A solid-phase microextraction fiber coated with diglycidyloxycalix[4]arene yields very high extraction selectivity and sensitivity during the analysis of chlorobenzenes in soil

Zeng

2006

Anal Bioanal Chem

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A novel fiber coated with sol-gel (5,11,17,23-tetra-tert-butyl-25,27-dihydroxy-26,28-diglycidyloxycalix [4]arene/hydroxy-terminated silicone oil; diglycidyloxy-C[4]/OH-TSO) was prepared for use with headspace solidphase microextraction (HS-SPME) combined with gas chromatography (GC) and electron capture detection (ECD), which was applied in order to determine nine chlorobenzenes in soil matrices. Due to the improved fiber preparation, which increases the percentage of calixarene in the coating, the new calixarene fiber exhibits very high extraction selectivity and sensitivity to chlorine-substituted compounds. Various parameters affecting the extraction efficiency were optimized in order to maximize the sensitivity during the chlorobenzene analysis. Interferences from different soil matrices with different characteristics were investigated, and the amount extracted was strongly influenced by the matrix. Therefore, a standard addition protocol was performed on the real soil samples. The linear ranges of detection for the chlorobenzenes tested covered three orders of magnitude, and correlation coefficients >0.9976 and relative standard deviations (RSD) <8% were observed. The detection limits were found at sub-ng/g of soil levels, which were about an order of magnitude lower than those given by the commercial poly(dimethylsiloxane) (PDMS) coating for most of the compounds. The recoveries ranged from 64 to 109.6% for each analyte in the real kaleyard soil matrix when different concentration levels were determined over the linear range, which confirmed the reliability and feasibility of the HS-SPME/ GC-ECD approach using the fiber coated with diglycidyloxy-C[4]/OH-TSO for the ultratrace analysis of chlorobenzenes in complex matrices.

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Section: Introductionmentioning

confidence: 98%

Section: Soil Collection and Preparationmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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A solid-phase microextraction fiber coated with diglycidyloxycalix[4]arene yields very high extraction selectivity and sensitivity during the analysis of chlorobenzenes in soil

Zeng

2006

Anal Bioanal Chem

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“…In a validation study of a method to analyse the aroma compounds of vinegar by HS-SPME, Natera et al [7] found considerable differences between the response of the three Carboxen-PDMS (CAR-PDMS) fibres employed and concluded that this coating is characterized by a low reproducibility and, as a consequence, each set of experiments should be performed with a single fibre. In the development of solgel-coated calyx [4]arene fibres, Li et al [8] found a life-time of above 170 samplings and an extremely high inter-fibre and inter-batch reproducibility when they were applied to the analyses of aromatic hydrocarbons and amines, PAHs and phthalic acid esters.…”

Section: Introductionmentioning

confidence: 99%

Reliability of fibres in solid-phase microextraction for routine analysis of the headspace of aromatic and medicinal plants

Bicchi

Cordero

Liberto

et al. 2007

Journal of Chromatography A

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This article evaluates the HS-SPME recovery repeatability, intermediate precision and their performance over time when applied to HS-SPME sampling for quality control of medicinal and aromatic plants. Experiments were carried out on two sets of fibres coated with two different coatings and belonging to different lots (i.e 100 m polydimethylsyloxane (PDMS) and Carboxen/divinylbenzene/PDMS 50/30 m, l: 1 cm (CAR/DVB/PDMS)) and on chamomile (Matricaria chamomilla L.), sage (Salvia lavandulifolia Vahl.) and a standard solution containing 3-hexanol, isoamyl acetate, 1,8-cineole and menthol in diisobutyl phthalate. The performance of each set of fibres was evaluated by determining a group of complementary statistical parameters including: (i) repeatability of the absolute areas of each marker from each matrix with each fibre; (ii) intra-fibre repeatability of the total absolute areas of the markers of each matrix obtained with each fibre of each set; (iii) inter-fibre intermediate precision of the total absolute areas of the markers of each matrix obtained with all fibres of each set; and (iv) analysis of variance by one-way ANOVA with Fisher and Tukey tests. The influence of the number of analyses on fibre effectiveness (fibre life-time) was studied by linear regression analysis (LRA). The results proved that HS-SPME can successfully be used for routine control analysis of aromatic ad medicinal plants since both types of fibres showed good repeatability and intermediate precision of analytes recovery and consistency over time. Unlike data previously reported by other authors, CAR/DVB/PDMS coated fibres gave better results than those coated with PDMS. The fibre-life seemed mainly to be influenced by the number and conditions of samplings and nature of the matrix investigated.

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“…The use of sol-gel with SPME was first reported by Chong et al [136] which resulted with higher thermal stability (> 320 °C) for SPME-GC analysis. After that, many synthesized different sol-gel phase chemistry such as the incorporation of polyethylene glycol [137], various crown ethers [138][139][140][141][142][143], and amino [144] groups to achieve high selectivity for the analytes of interest in various applications.…”

Section: Sol-gel Technologymentioning

confidence: 99%

Evaluation of Non-Contact Sampling and Detection of Explosives using Receiver Operating Characteristic Curves

Young¹

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Preparation and characteristics of sol–gel-coated calix[4]arene fiber for solid-phase microextraction

Cited by 105 publications

References 41 publications

A solid-phase microextraction fiber coated with diglycidyloxycalix[4]arene yields very high extraction selectivity and sensitivity during the analysis of chlorobenzenes in soil

A solid-phase microextraction fiber coated with diglycidyloxycalix[4]arene yields very high extraction selectivity and sensitivity during the analysis of chlorobenzenes in soil

Reliability of fibres in solid-phase microextraction for routine analysis of the headspace of aromatic and medicinal plants

Evaluation of Non-Contact Sampling and Detection of Explosives using Receiver Operating Characteristic Curves

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