A dispersive solid-phase extraction method based on a new sorbent has been performed on plasma and wastewater samples to determine metoprolol by high-performance liquid chromatography–tandem mass spectrometry. In this study, the analyte was adsorbed from the samples onto microcrystalline cellulose as a green and efficient sorbent and then eluted for use in the determination step. In the mass spectrometer, the analyte was detected in the positive mode and selectivity of the analysis was increased by sequential mass analysis through multiple reaction monitoring. All of the effective parameters in the extraction of metoprolol from plasma and wastewater were optimized. Under optimal conditions the method was linear in the ranges of 1–1,000 and 0.1–1,000 ng/ml in plasma and wastewater samples, respectively. The detection limits of the method were 0.30 and 0.03 ng/ml in plasma and wastewater samples, respectively. The data showed that the method provides low detection limit, wide linear range, good precision and high extraction recovery. Finally several plasma and wastewater samples were successfully analyzed using the method. The use of a small amount of a green and inexpensive sorbent and a low volume of plasma without the need for further pretreatment steps are the main advantages of the method. 相似文献
A new method for extraction and analysis of acetone in human urine based on headspace solid phase microextraction using a
mixture of activated carbon and zeolite as sorbents in a PVC matrix coated on a silver wire and its application to the determination
of ketone bodies is described. Unlike commercial fibers, which are coated on fused silica, the coating adheres strongly to
the silver wire and is thermally stable up to 250 °C. After optimization of coating composition and microextraction conditions
the fiber was used for the analysis of acetone in human urine. 相似文献
Summary In this study, a rapid and efficient semi-micro extraction procedure is presented for the extraction of some higher n-alkanes
from water and soil samples. In the case of water samples n-hexane was used as the organic phase in a phase volume ratio (volume
of aqueous phase/volume of organic phase) higher than 285, while in the case of soil samples, extraction with n-hexane was
carried out in the presence of an excess of 2 M NaCl solution. The extraction rate from soil samples is very high and is better
than Soxhlet extraction, comparable with supercritical fluid extraction. High preconcentration factor in water samples allows
the limits of detection to be in the ng.mL−1 level with the use of gas chromatographic analysis. Flame ionization detector was used for monitoring the analytes. The obtained
recoveries of all studied compounds from both water and soil samples are higher than 90%. This method was successfully used
to determine some n-alkanes in municipal wastewater and contaminated soil. 相似文献
High performance liquid chromatography (HPLC) and gas chromatography (GC) are introduced for analysis of polymer lubricants
(stearamide, oleamide and erucamide). In the HPLC method, a reverse phase octadecylsilane (ODS) column along with acetonitrile/methanol
(60:40) as a mobile phase were used. Detection of analytes was performed by a UV detector at 202 nm. The analysis time was
less than 8 min. In the GC method, polar capillary column and flame ionization detector (FID) were used for separations and
detection, respectively. The analysis time by GC was longer than HPLC and was about 30 min. Limits of detection, linear range
and repeatability of both methods are similar, but determination of oleamide in real samples by HPLC method is difficult due
to complexity of the initial part of HPLC chromatogram in polyethylene samples. That problem is not observed in the GC method.
Detection limits in both methods for all analytes are lower than 0.003% which are much lower than the amount of lubricants
in commercial polymers (0.05–0.2%). 相似文献
A simple and rapid solid-phase microextraction (SPME) method is presented based on activated charcoal–PVC fiber for determination of some organophosphorus pesticides from aqueous samples in direct mode SPME. After optimization of the experimental variables affecting SPME of the target compounds from aqueous solutions, the proposed method was applied to determine pesticides in fruit juice. The analytes in this procedure were preconcentrated for 15 min on the SPME fiber and subsequently desorbed by heating the fiber at 200 °C for 5 min in the GC injection port. Separation was on a capillary column GC followed by flame ionization detection. Recoveries of the pesticides studied in aqueous samples ranged 42%–63% and repeatability for all analytes was < 9% for a single fiber. Fiber-to-fiber reproducibility was < 18%. 相似文献
In this two‐part report, the efficiency of rice bran in removal of heavy metals such as cadmium, lead, zinc, nickel, copper and iron(III) from aqueous solution is investigated. The different experimental conditions such as pH, temperature, volume of solution, bran amount, particle size, exchange time, stirring speed, etc. are studied, and the optimum conditions are selected in part 1 of this series of reports. The efficiency of bran in removal of heavy metals is presented with and without treatments. For treatment, heat or acid, alkali and salt solutions were used. The results obtained show that after treating with saturated sodium chloride solution, its efficiency for Ni2+ and Zn2+ improves. At pH 5, all studied cations have recoveries more than 93% (lead and cadmium 100%). The exchange speed is very high and has preference over the classical ion exchangers. 相似文献
An inside-needle extraction method was developed through thermal polymerization of atrazine-molecularly imprinted polymer (MIP) on the internal surface of a stainless steel hollow needle, which was oxidized and silylated. The fabricated coating (MIP layer) for the needle was durable and showed very good chemical and thermal stability. It could be mounted on a glass syringe and be directly coupled with gas chromatographic (GC) systems. The parameters being effective on the coating and extraction processes, namely nature of oxidizing agent, silylation time, nature and amount of porogen, template-to-MIP components ratio, polymerization time and temperature, sample volume, flow rate, pH and ionic strength of the sample were investigated and optimized. The extraction needle showed high selectivity as well as a great extraction capacity for triazines. The extraction of atrazine, simazine, cyanazine, ametryn, prometryn and terbutryn using the fabricated extraction needle and followed by GC analysis resulted in detection limits of 2.6, 21, 24, 32, 38 and 42 ng mL−1, respectively. The fabricated needle proved to be applicable to the analysis of real samples by comparing the results obtained for non-spiked and spiked samples of grape juice, tap water and groundwater.