Determination of Fluoxetine in Human Plasma by Liquid Chromatography–Mass Spectrometry and Its Application

Abstract

A rapid, simple, and specific liquid chromatography–electrospray ionization–mass spectrometric method has been developed and validated for the determination of fluoxetine in human plasma. The method was validated with a linear range of 0.5–100 ng mL^?1, and the lowest limits of quantification were 0.5 ng mL^?1 for fluoxetine. The extraction efficiencies were about 65% and recoveries of method were in the range of 94.0–97.5%. The intraday relative standard deviation (RSD) was less than 11% and interday RSD was within 12%. The method has been successfully applied to the evaluation of pharmacokinetics and bioequivalence of fluoxetine.     

Determination of Pesticides in Carrots by Gas Chromatography–Mass Spectrometry

ABSTRACT

A sensitive and selective method was developed to determine pesticides in carrots by gas chromatography–mass spectrometry following the development of an optimized extraction procedure. The method was validated for 30 organochlorine pesticides for gas chromatography with electron capture detection obtaining limit of detection from 0.18 to 0.92?µg/kg except for cis- and trans-permenthrin. Twenty-six carrot samples were analyzed and six pesticides were detected. The results compared with the accepted maximum residue levels in correlation to crop origin.     

Preliminary Characterization of the Composition and Phenolic Fragmentation of Olive Byproducts by Gas Chromatography–Mass Spectrometry and High-Performance Liquid Chromatography–Tandem Mass Spectrometry

Olive waste is a potential resource due to its rich variety of biologically active compounds. To investigate chemical components of olive waste, the selected samples were extracted using ultrasound assisted enzyme hydrolysis and petroleum ether, ethyl acetate and n-butyl alcohol were used to obtain a series of solvent extracts. Gas chromatography–mass spectrometry analysis showed hydrocarbons, esters, acids, alcohols, and ketones present in the extracts. Some fatty acids were considered to be predominant; it is noteworthy that phenolic compounds were detected in the ethyl acetate extract fraction. Furthermore, the primary phenolic compounds were also determined by high-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry. The possible fragmentation patterns have been proposed in positive and negative ion modes; the main fragment ions were observed from the loss of methyl, hydroxyl, or carboxyl groups. The compounds showed different fragmentation ions types in both positive and negative ionization modes and gave structural information on the main phenolic compounds in olive waste. The results of this study may be used to identify valuable active compounds and guide commercial applications of olive waste.     

Application of Thin-Layer Chromatography and Gas Chromatography—Mass Spectrometry for Evaluation of the Chemical Stability of Hexyl Nicotinate

JPC – Journal of Planar Chromatography – Modern TLC - In this study, thin-layer chromatography with densitometry and gas chromatography—mass spectrometry (GC—MS) were used...     

Phytochemical Study of the Composition of the Unsaponifiable Fraction of Various Vegetable Oils by Gas Chromatography–Mass Spectrometry

Journal of Analytical Chemistry - We developed a method for quantitatively analyzing some components of the unsaponifiable fraction of edible oils and validated its characteristics. The component...     

Determination of Preservatives in Water-Based Adhesives by Gas Chromatography–Mass Spectrometry

This study establishes an analytical method for the determination of eighteen preservatives in water-based adhesives. The method was based on liquid–liquid extraction by methyl tertiary-butyl ether and subsequent determination by gas chromatography–mass spectrometry. Experimental conditions (instrumental parameters, extraction solvent, extraction mode, dispersant volume, and extraction time) were optimized and validated. When the method was applied to water-based adhesives, the limits of detection and recovery were 2.29–17.59 milligrams per kilogram and 85.7 ? 93.9 percent, respectively, and the repeatability was below 5 percent for all analytes. None of the analytes were found in five cigarette adhesives.     

Characterization of Oil by Micro-Solid-Phase Extraction and Gas Chromatography–Mass Spectrometry

Micro-solid-phase extraction is reported for the preparation of Bohai crude oil for the determination of hydrocarbons by gas chromatography-mass spectrometry. The operational parameters were optimized. Micro-solid-phase extraction provided higher quantities of low-molecular weight components than conventional liquid chromatography. The concentrations of high-molecular weight n-alkanes, polycyclic aromatic hydrocarbons, and their alkylated homologs obtained were comparable by micro-solid-phase extraction and liquid chromatography. The diagnostic ratios also indicated that there were no significant differences between these methods. Therefore, micro-solid-phase extraction with gas chromatography–mass spectrometry is recommended for the characterization of spilled oil.     

Novel Sampling for the Determination of Naphthalene in Air by Gas Chromatography–Mass Spectrometry

Here are reported two new sampling method approaches for the determination of naphthalene in ambient air for concentrations from 0.25 to 18.7?µg/L. The first method used for gas phase naphthalene analysis produced an average recovery of 88.8% and the second method using headspace sampling produced an average recovery of 93.8%. The second method showed better recovery than the former, so it was used for subsequent comparative gas-phase determination of naphthalene. The second method was validated at various naphthalene concentrations and humidity using a naphthalene gas generator to produce various naphthalene standards and a naphthalene-monitoring instrument. The naphthalene concentrations generated using the gas generator and determined second sampling method with gas chromatography–mass spectrometry (GC–MS) were compared to the sensor measurements and were in good agreement. In summary, the sampling methods presented provided reliable gas-phase naphthalene determination when coupled with GC–MS.     

Determination of Herbicides in Corn Flour by Novel Extraction and Gas Chromatography–Mass Spectrometry

A simple and efficient procedure was developed to determine eight herbicides in corn flour by gas chromatography–mass spectrometry in selected ion-monitoring mode. Samples were prepared with a modified, quick, easy, rapid, effective, rugged, and safe procedure. The type and volume of extraction solvent, type and amount of adsorbent, and time of sonication were optimized. The protocol method was rigorously verified. The mean recoveries were from 85 to 108% at various fortification levels with relative standard deviations below 15% and limits of quantification from 4 to 48?ng g^?1. The method was used to determine herbicides in corn flour.     

Determination of Toluene and Ethanol in Urine by Headspace and Cryotrapping Gas Chromatography–Mass Spectrometry

Toluene is the major volatile organic compound found in glue and is often used as a hallucinogenic for abusers. Use with alcohol increases the risk of adverse effects from toluene exposure. In this study, a headspace and cryotrapping gas chromatography–mass spectrometry method was developed and validated for the determination of toluene and ethanol in urine. Experimental and instrumental variables were investigated to optimize the method for sensitivity. Excess sodium sulfate was used as the salting-out reagent before the headspace protocol. Linear least squares regression with a 1/x weighting factor was used to construct calibration curves from 0.002 to 0.4?µg?mL^?1 for toluene and 10 to 2000?µg?mL^?1 for ethanol. The correlation coefficients exceeded 0.9993. The limits of detection were 0.0005?µg?mL^?1 for toluene and 0.21?µg?mL^?1 for ethanol. Intraday and interday precisions were within 5.4 and 11.5%, while intraday and interday accuracies were between ?11.3 to ?4.0% and ?11.0 to 1.2%, respectively. The method validation results for selectivity and stability were satisfactory. The validation results were used to estimate the expanded uncertainty and the contribution of individual steps in the method for the quantification of toluene and ethanol. The relative expanded uncertainties were 14.1% for toluene and 4.6% for ethanol.     

Determination of δ-Hexadecanesultone in Anionic Surfactants and Detergents by Gas Chromatography–Mass Spectrometry

Journal of Analytical Chemistry - A method is proposed for the determination of sultones in the anionic surfactant sodium α-olefin sulfonate (AOS Na) and products based on this surfactant. The...     

Determination of Volatiles in Water Lily Flowers Using Gas Chromatography–Mass Spectrometry

Volatile organic compounds in the stamens, petals, and pistils of 56 water lily cultivars were determined by headspace solid-phase microextraction coupled with gas chromatography–mass spectrometry. The stamens released a majority of the volatiles. A total of 117 volatile organic compounds were determined. Alkanes and alkenes were the most abundant, followed by aldehydes and ketones. Cluster analysis was used to divide the cultivars into three subsets characterized by specific aromatic compounds and associated aromas. Discriminant analysis confirmed the results of the cluster analysis. Three tropical water lily cultivars Colorata, 34, and Ai Ji Bai and one hardy water lily cultivar Somptuosa had particularly high aromatic compound concentrations and are recommended to produce fragrant, colorful, and hardy specimens.     

Retention Time Locking in the Determination of Narcotic Drugs by Chromatography and Chromatography–Mass Spectrometry

The use of retention time locking (RTL) in the development of unified procedures for the detection and quantitative determination of drugs in biological fluids was considered. With consideration for the use of RTL, a chromatographic procedure with flame-ionization and mass-selective detection was developed for the detection and quantitative determination of opiates and their synthetic analogs; phenylalkylamine derivatives; cocaine; ketamine; and other narcotic drugs, their derivatives, and metabolites in urine. The analytical ranges for chromatography–mass spectrometry were 0.05–1000 and 0.005–1000 g/mL under the conditions of total ion current (TIC) scanning and selected ion monitoring (SIM), respectively. With flame-ionization detection (GC–FID), the analytical range was 0.5–1000 g/mL.     

Determination of Promedol (Trimeperidine) and Ketamine in Blood Using Gas Chromatography–Mass Spectrometry

A procedure was developed for the gas-chromatographic determination of promedol (trimeperidine) and ketamine in whole blood with mass-selective detection. The detection limit for trimeperidine and ketamine in blood is 0.05 g/mL. The analytical range is 0.1–5.0 g/mL. The maximum within-series errors in the determination of the studied compounds are no higher than 14.1% for concentrations of 0.10 g/mL and 7.47% for concentrations of 1.0 g/mL. The maximum between-series relative errors are 5.75% for concentrations of 0.10 g/mL and 2.7% for concentrations of 1.0 g/mL. The procedure can be used in toxicological and clinical analyses.     

Determination of α-Tocopherol in Olive Oil by Solid-Phase Microextraction and Gas Chromatography–Mass Spectrometry

Olive oil has great human health benefits and is an important component of the Mediterranean diet. Its quality, sensory attributes, and oxidative stability are linked to the presence of minor compounds. Vitamin E (α-tocopherol) is a key component in these properties. In this work, solid-phase microextraction coupled to gas chromatography–mass spectrometry was used for the determination of α-tocopherol in olive oil. The analytical performance of the method has been assessed in fortified olive oil with negligible vitamin E concentrations. The calibration curve was linear from 0.020 to 0.500?mg/g. The limits of detection and quantification were 0.006 and 0.021?mg/g, respectively. Intraday and interday relative standard deviations were 3.2 and 10.0, respectively, and were concentration independent. The method was used for the determination of α-tocopherol in virgin and extra virgin olive oil, reporting average concentrations of 0.044?±?0.03 and 0.200?±?0.05?mg/g, respectively. Overall, the method is simple, sensitive, rapid, and solvent free, and provided high recoveries of 97.7?±?3.1%. In addition, vitamin E stability in extra-virgin olive oil was characterized by a shelf-life study.     

Determination of Phthalate Esters in Textiles by Solid Phase Extraction and Gas Chromatography–Mass Spectrometry

A sensitive and rapid method was developed for the determination of seven phthalate esters in baby waterproof fabrics, decorated waterproof tarpaulins, and printed textiles by solid phase extraction followed by gas chromatography–mass spectrometry. The method showed good linearity with correlation coefficients between 0.9958 and 0.9999 and limits of quantification and detection from 23 to 274 micrograms per liter and 7 to 82 micrograms per liter, respectively. The maximum recoveries were between 96.2 and 100.9 percent with relative standard deviations from 1.06 to 6.87 percent. The protocol was applied to the determination of phthalate esters in textiles: the samples contained more than 0.1 percent phthalate esters, which exceed relevant standards.