ABSTRACT
In this work, an ordered mesoporous carbon (OMC)/Nafion coated fiber for solid-phase microextraction (SPME) was prepared and used as the working electrode for electro-enhanced SPME (EE-SPME) of amphetamines. The EE-SPME strategy is primarily based on the electro-migration and complementary charge interaction between fiber coating and ionic compounds. Compared with traditional SPME, EE-SPME exhibited excellent extraction efficiency for amphetamine (AP) and methamphetamine (MA) with an enhancement factor of 7.8 and 12.1, respectively. The present strategy exhibited good linearity for the determination of AP and MA in urine samples in the range of 10-1000ngmL(-1) and 20-1000ngmL(-1), respectively. The detection limits were found to be 1.2ngmL(-1) for AP and 4.8ngmL(-1) for MA. The relative standard deviations were calculated to be 6.2% and 8.5% for AP and MA, respectively. Moreover, the practical application of the proposed method was demonstrated by analyzing the amphetamines in urine and serum samples with satisfactory results.
Subject(s)
Amphetamines/blood , Amphetamines/urine , Chromatography, Gas/methods , Solid Phase Microextraction/methods , Carbon , Electrochemical Techniques , Humans , Limit of Detection , Linear Models , Reproducibility of ResultsABSTRACT
Single-drop microextraction (SDME) coupled with gas chromatography-flame ionization detector (GC-FID) was developed for the extraction and determination of aromatic amines (AAs) in environmental water samples. A silicon tube was introduced for the SDME procedure by inserting it into the needle of the micro-injector. In this manner, a large volume of extractant is allowed to be suspended for the extraction, leading to the enhancement of method sensitivity and reproducibility. Extraction parameters which control the performance of SDME such as the type of microextraction solvent and volume, sample pH, ionic strength and extraction time were investigated and optimized. Under the optimized conditions, the SDME-GC method exhibited good linearity from 0.5 to 50 µg mL(-1) for aniline and 4-methylaniline and 0.1 to 50 µg mL(-1) for N-methylaniline and N, N-diethylaniline. The enrichment factors were calculated to be 42-509. The SDME-GC method was performed for the determination of AAs in environmental water samples including drinking, lake and sea water, and excellent recoveries and relative standard deviations (RSD values) ranging from 79.5 to 122.7% and 3.2 to 13.3%, respectively, were obtained. The results demonstrated that SDME-GC is a rapid, simple and effective sample preparation method and could be successfully applied for the determination of AAs in environmental water samples.
ABSTRACT
In this work, oriented ZnO nanorods (ZNRs) were in situ hydrothermally grown on a porous polyaniline (PANI) film to function as a solid-phase microextraction (SPME) coating. Scanning electron microscopy (SEM) study revealed that the majority of oriented ZNRs grew from pores of PANI matrix, which protected the ZNRs from easily peeling off during operation. Furthermore, in this process, a thin layer of PANI was found to cover the ZNRs, which can enlarge the effective surface area of the composite coating. This ZNRs/PANI composite coating combined the merits of both ZNRs and PANI and, thus, has several advantages over that of sole PANI film and ZNRs coating such as improved extraction efficiency for benzene homologues, enhanced mechanical stability and longer service life (over 150 cycles of SPME-GC operation). Coupled with gas chromatography-flame ionization detector (GC-FID), the optimized SPME-GC-FID method was used for the analysis of six benzene homologues in water samples. The calibration curves were linear from 1 to 1000µgL(-1) for each analyte, and the limits of detection were between 0.001 and 0.024µgL(-1). Single fiber repeatability and fiber-to-fiber reproducibility were in the range of 1.3-6.8% and 5.3-11.2%, respectively. The spiked recoveries at 100 and 5µgL(-1) for three environmental water samples were in the range of 79.8-115.4% and 73.7-117.4%, respectively.
