Determination of free (unconjugated) amphetamine-type stimulants in urine samples by dispersive liquid–liquid microextraction and gas chromatography coupled to mass spectrometry (DLLME-GC-MS)

2016 ◽  
Vol 125 ◽  
pp. 230-235 ◽  
Author(s):  
Ricardo Leal Cunha ◽  
Wilson Araujo Lopes ◽  
Pedro Afonso P. Pereira
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Urine Samples ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

scholarly journals Determination of Non-Steroidal Anti-Inflammatory Drugs in Animal Urine Samples by Ultrasound Vortex-Assisted Dispersive Liquid–Liquid Microextraction and Gas Chromatography Coupled to Ion Trap-Mass Spectrometry

2020 ◽  
Vol 10 (16) ◽  
pp. 5441 ◽  
Author(s):  
Pasquale Avino ◽  
Ivan Notardonato ◽  
Sergio Passarella ◽  
Mario Vincenzo Russo
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Analytical Method ◽  
Ion Trap ◽  
Urine Samples ◽  
Ion Trap Mass Spectrometry ◽  
Inflammatory Drugs ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

A low solvent consumption method for the determination of non-steroidal anti-inflammatory drugs (NSAIDs) in animal urine samples is studied. The NSAIDs were extracted with CH2Cl2 by the ultrasound vortex assisted dispersive liquid–liquid microextraction (USVA-DLLME) method from urine samples, previously treated with β-glucuronidase/acrylsulfatase. After centrifugation, the bottom phase of the chlorinated solvent was separated from the liquid matrix, dried with Na2SO4, and derivatized with N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) + trimethylchlorosilane (TMCS) (99 + 1). After cooling at room temperature, the solution was concentrated under nitrogen flow, and 1 µL of solution was analyzed in gas chromatography/ion trap-mass spectrometry (GC-IT-MS). The enrichment factor was about 300–450 times and recoveries ranged from 94.1 to 101.2% with a relative standard deviation (RSD) of ≤4.1%. The USVA-DLLME process efficiency was not influenced by the characteristics of the real urine matrix; therefore, the analytical method characteristics were evaluated in the range 1–100 ng mL−1 (R2 ≥ 0.9950). The limits of detection (LODs) and limits of quantification (LOQs) were between 0.1 and 0.2 ng mL−1 with RSD ≤4.5% and between 4.1 and 4.7 ng mL−1 with RSD ≤3.5%, respectively, whereas inter- and intra-day precision was 3.8% and 4.5%, respectively. The proposed analytical method is reproducible, sensitive, and simple.

Determination of UV-327 and its metabolites in human urine using dispersive liquid-liquid microextraction and gas chromatography-tandem mass spectrometry

2021 ◽  
Vol 13 (35) ◽  
pp. 3978-3986
Author(s):  
Corinna Fischer ◽  
Thomas Göen
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Tandem Mass Spectrometry ◽  
Human Urine ◽  
Tandem Mass ◽  
Extraction Solvent ◽  
Chromatography Tandem Mass Spectrometry ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

A method is presented for the extraction of the UV stabilizer UV-327 and its metabolites from urine with acetonitrile (disperser solvent) and chloroform (extraction solvent), followed by instrumental analysis of the trimethylsilylated analytes.

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