Solid-phase Microextraction of Volatile Polar Compounds in Water

A methodology for automated headspace solid-phase microextraction for the trace analysis of pharmaceutical process-related toxic impurities such as benzyl chloride, triethyl amine, chloroethyl methyl ether, N-methylmorpholine, and N-methylpyrrolidinone by gas chromatography and flame ionization detection is reported. Carboxen/ polysiloxane/divinylbenzene fiber showed excellent sensitivity towards these analytes compared to direct injection and the highest sensitivity among the commercial SPME fibers evaluated in this study. However, a profound effect of competition for the available adsorption sites was observed on the Carboxen/PDMS/DVB fiber. The effects of extraction parameters such as extraction time, temperature, agitation rate, and headspace volume were studied. The influence of the addition of inorganic salt on the analyte extraction efficiency was also investigated. The sensitivity of method extended to the sub-ppm level with acceptable precision and accuracy. The linearity of the method covered one order of magnitude. The narrower linear dynamic range is attributed largely to the limited number of adsorption sites on the Carboxen/PDMS/DVB fiber.

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Determination of pharmaceutical process impurities by solid phase microextraction gas chromatography

Frost

Hussain

Raghani³

2003

J of Separation Science

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Optimization of solid-phase microextraction using Taguchi design to quantify trace level polycyclic aromatic hydrocarbons in water

et al. 2012

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This article introduces a simple, rapid, and reliable solid-phase microextraction (SPME) method coupled with GC-MS for the quantitative determination of 16 polycyclic aromatic hydrocarbons in water. In this study, the Taguchi experimental design was used to optimize extraction conditions of polycyclic aromatic hydrocarbons using SPME method to obtain highly enriched analytes. Consequently, quantitative determination of polycyclic aromatic hydrocarbons in water was achieved by GC-MS technique. The selected parameters affecting enrichment of polycyclic aromatic hydrocarbons were sample extraction time, stirring speed, temperature, ionic strength, and pH. The study revealed that optimal operating conditions were found to be 90-min extraction time, 1400 rpm stirring speed, and 60°C sample temperature. The effect of ionic strength and pH were shown to be insignificant. Optimized conditions were also reevaluated by placing the 16 polycyclic aromatic hydrocarbons into several subgroups based on their molecular weight. The extraction efficiency of polycyclic aromatic hydrocarbons with low molecular weight was shown to be a function of only the extracting temperature. Satisfactory results were obtained for linearity (0.983-0.999), detection limits (2.67-18.02 ng/L), accuracy (71.2-99.3%), and precision (4.3-13.5%). The optimum conditions reported by other design approaches were evaluated and generalized optimum conditions were suggested.

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Analysis of pesticides volatilised from plants and soil by headspace solid-phase microextraction and gas chromatography

Castro¹,

Pérez²,

Sánchez‐Brunete³

et al. 2001

Chromatographia

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Gas ch romatog ra phy SPME Pesticides Plants and soil SummaryPesticides volatilised from plants and soil were determined by headspace SPME and gas chromatography with electron-capture and mass spectrometric detection. SPME analyses were carried out with polydimethylsiloxane (PDMS) and polyacrylate (PA) fibres. A mixture of endosulfan, chlorpyrifos, hndane and pendimethalin was used in these assays. Fortified soil and plant samples were maintained at 30 ~ for 2 h and 1 h, respectively, before SPME sampling. Pesticides were extracted by SPME by inserting the sheathed fibre through the cap and exposing it to the headspace for 1 h.GC-ECD analysis was performed after thermal desorption of pesticides from the fibre for 5 minutes. Pesticide identily was confirmed by mass spectrometry operating in the electron impact mode (El). The SPME fibres assayed gave good results, the response obtained with the PDMS fibre being somewhat belter in the concentration range studied. Detection limits for the compounds studied varied from 1 to 8 ng L 1.

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Solid-phase Microextraction of Volatile Polar Compounds in Water

Cited by 14 publications

References 18 publications

Determination of pharmaceutical process impurities by solid phase microextraction gas chromatography

Determination of pharmaceutical process impurities by solid phase microextraction gas chromatography

Optimization of solid-phase microextraction using Taguchi design to quantify trace level polycyclic aromatic hydrocarbons in water

Analysis of pesticides volatilised from plants and soil by headspace solid-phase microextraction and gas chromatography

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