Pressurized liquid extraction followed by liquid chromatography with tandem mass spectrometry to determine pharmaceuticals in mussels

Salicylic acid is an emerging environmental contaminant, usually found at ng/L concentrations in natural waters. Its quantification usually involves liquid chromatography-tandem mass spectrometry, which requires complex and costly instrumentation as well as time-consuming sample pretreatment, typically involving large solvent volumes. In this work, sequential injection chromatography was exploited to develop a fast, green, cost-effective, and highly sensitive procedure for fluorimetric determination of salicylic acid in natural waters. Analyte preconcentration directly on the chromatographic column (on-column preconcentration) was exploited to improve detectability, yielding an enrichment factor of 122 (1.75 mL of sample) and takes only 8.5 min per determination. A detection limit of 20 ng/L, a linear response range from 0.06 to 5.00 μg/L, coefficients of variation lower than 3.0% (n = 10), and recoveries within 86 and 114% were estimated. The procedure was applied for the analyses of freshwater samples and results agreed with those obtained by liquid chromatography-tandem mass spectrometry at the 95% confidence level. The proposed procedure encompasses in-line concentration, isolation/separation, and detection, without the need for sample clean-up, thus minimizing the consumption of organic solvents and risk of analyte losse. K E Y W O R D Sgreen analytical chemistry, on-column preconcentration, sequential injection chromatography, solid-phase extraction, spectrofluorimetry 1232

Section: Introductionmentioning

confidence: 99%

Exploitation of a short monolithic column for in‐line separation and preconcentration: Environmental friendly determination of the emerging pollutant salicylic acid in natural waters

Souza

Sasaki

Rocha

2020

“…It is clear that the choice of an appropriate and selective samplepreparation procedure is essential for accurate determination of these drugs [3][4][5][6][7]. SPME is a sample-preparation method that has been applied to a range of applications such as environmental, industrial, clinical, forensic, drug and food analysis [8][9][10].…”

Section: Introductionmentioning

confidence: 99%

“…Microextraction procedures are widely used as sample preparation for drug separation from matrices where potentially interfering sample components coexist. It is clear that the choice of an appropriate and selective sample‐preparation procedure is essential for accurate determination of these drugs . SPME is a sample‐preparation method that has been applied to a range of applications such as environmental, industrial, clinical, forensic, drug and food analysis .…”

Section: Introductionmentioning

confidence: 99%

Ultrasound‐assisted magnetic dispersive solid‐phase microextraction: A novel approach for the rapid and efficient microextraction of naproxen and ibuprofen employing experimental design with high‐performance liquid chromatography

Ghorbani

Chamsaz

Rounaghi

2016

A simple, rapid, and sensitive method for the determination of naproxen and ibuprofen in complex biological and water matrices (cow milk, human urine, river, and well water samples) has been developed using ultrasound-assisted magnetic dispersive solid-phase microextraction. Magnetic ethylendiamine-functionalized graphene oxide nanocomposite was synthesized and used as a novel adsorbent for the microextraction process and showed great adsorptive ability toward these analytes. Different parameters affecting the microextraction were optimized with the aid of the experimental design approach. A Plackett-Burman screening design was used to study the main variables affecting the microextraction process, and the Box-Behnken optimization design was used to optimize the previously selected variables for extraction of naproxen and ibuprofen. The optimized technique provides good repeatability (relative standard deviations of the intraday precision 3.1 and 3.3, interday precision of 5.6 and 6.1%), linearity (0.1-500 and 0.3-650 ng/mL), low limits of detection (0.03 and 0.1 ng/mL), and a high enrichment factor (168 and 146) for naproxen and ibuprofen, respectively. The proposed method can be successfully applied in routine analysis for determination of naproxen and ibuprofen in cow milk, human urine, and real water samples.

“…SA (and its salicylate anion) is the principal metabolite of ASA and it is the pharmacologically active substance in food and biological samples [6]. Many chromatographic methods including CE [7], LC-UV [8,9], and LC-MS/MS [10][11][12][13] have been proposed for the analysis of SA in food and biological samples. The residues present in food samples are usually at extremely low concentrations with complex and multicomponent matrixes.…”

Section: Introductionmentioning

confidence: 99%

“…SPE is an effective technique to isolate and preconcentrate compounds of interest from the sample matrix. Various SPE sorbents for off‐line processing have been reported , including strong anion‐exchange sorbent, hydrophilic–lipophilic balance sorbent (the sorbent of which is a microporous copolymer made from a balanced ratio of two monomers including hydrophilic and lipophilic ones) and the C 18 sorbent. Off‐line SPE is a multi‐step process that requires conditioning of the SPE cartridge, addition of an extract, rinsing, and elution of the analytes.…”

Section: Introductionmentioning

confidence: 99%

Poly[(2‐(acryloyloxy) ethyl]trimethylammonium chloride‐co‐ethylene dimethacrylate monolith on‐line solid‐phase extraction coupled with liquid chromatography and tandem mass spectrometry for the fast determination of salicylic acid in foodstuffs

Wang

et al. 2018

We report the fabrication of an anion-exchange monolithic column in a stainless-steel chromatographic column (10 mm × 2.1 mm i.d.) using [2-(acryloyloxy) ethyl]trimethylammonium chloride as the monomer and ethylene dimethacrylate as the crosslinker. The prepared monolith was developed as the adsorbent for the on-line solid-phase extraction of salicylic acid in various animal-origin foodstuffs combined with liquid chromatography and tandem mass spectrometry. The monolith was characterized by using Fourier transform infrared spectroscopy, scanning electron microscopy, nitrogen adsorption analysis, and elemental analysis. Potential factors affecting the on-line solid-phase extraction and liquid chromatography with tandem mass spectrometry analysis were studied in detail. Under the optimized conditions, the total analysis time including cleanup and liquid chromatography with tandem mass spectrometry separation was 17 min. The developed method gave the linear range of 15-750 μg/kg, detection limits (S/N = 3) of 5 μg/kg, and quantification limits (S/N = 10) of 15 μg/kg. The recoveries obtained by spiking 10, 20, and 100 μg/kg of salicylic acid in the animal-origin food samples were in the range of 85.2-98.4%. In addition, the monolith was stable enough for 550 extraction cycles with the precision of peak area ≤11.6%.