QUANTITATION OF CARVEDILOL OXIDATIVE METABOLITES IN HUMAN PLASMA USING LIQUID CHROMATOGRAPHY TANDEM MASS SPECTROMETRY

INDIAN DRUGS ◽  
2012 ◽  
Vol 49 (02) ◽  
pp. 37-44
Author(s):  
J Valarmathy ◽  
◽  
T. Sudha ◽  
K. L. Kumar ◽  
S. L Joshua
Keyword(s):  
Human Plasma ◽  
Room Temperature ◽  
Plasma Sample ◽  
Liquid Extraction ◽  
Liquid Liquid Extraction ◽  
Chromatography Tandem Mass Spectrometry ◽  
Oxidative Metabolites ◽  
Liquid Chromatography Tandem Mass ◽  
Assay Precision

A sensitive and efficient method was developed for the determination of carvedilol and its metabolite in human plasma by LC-MS/MS. Plasma samples were hydrolysed with beta-glucuronidase and the target compounds were extracted with liquid liquid extraction using diethyl ether in dichloro methane as solvent. The extracts were completely derivatized and analysed by LC-MS/MS. The linearity of the assay ranges from 0.250 ng/mL to 200.0 ng/mL for carvedilol and from 0.500 ng/mL to 30.0 ng/mL for 4-hydroxy carvedilol. The absolute recovery of carvedilol and its metabolite added to blank plasma sample was 70.28 82.90%. The reproducibility was from 0.96 to 8.28 for the intraday assay and from 1.65 to 6.09 for the interday assay precision. Repetitive thawing and freezing did not have an affect on metabolite through a minimum of three cycles. Thawed samples remaining in plasma for 4h before extraction were with 5% of theoretical value. Stability of the extracted samples on the auto sampler at room temperature was evaluated for 34 h and was observed to with in 12% of a fresh analytical sample for 4 hydroxy carvedilol. The proposed LC-MS/MS method was effective for the determination of carvedilol and it metabolite in human plasma.

scholarly journals Determination of Eight Coccidiostats in Eggs by Liquid–Liquid Extraction–Solid-Phase Extraction and Liquid Chromatography–Tandem Mass Spectrometry

Molecules ◽  
2020 ◽  
Vol 25 (4) ◽  
pp. 987 ◽  
Author(s):  
Bo Wang ◽  
Jianyu Liu ◽  
Xia Zhao ◽  
Kaizhou Xie ◽  
Zhixiang Diao ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Solid Phase ◽  
Liquid Extraction ◽  
Tandem Mass ◽  
Liquid Liquid Extraction ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

A method for the simultaneous determination of robenidine, halofuginone, lasalocid, monensin, nigericin, salinomycin, narasin, and maduramicin residues in eggs by liquid chromatography–tandem mass spectrometry (LC–MS/MS) was developed. The sample preparation method used a combination of liquid–liquid extraction (LLE) and solid-phase extraction (SPE) technology to extract and purify these target compounds from eggs. The target compounds were separated by gradient elution using high-performance liquid chromatography (HPLC) and ultra-performance liquid chromatography (UPLC). Tandem mass spectrometry was used to quantitatively and qualitatively analyze the target compounds via electrospray ionization (ESI+) and multiple reaction monitoring mode. The HPLC–MS/MS and UPLC–MS/MS methods were validated according to the requirements defined by the European Union and the Food and Drug Administration. The limits of detection and limits of quantification of the eight coccidiostats in eggs were 0.23–0.52 µg/kg and 0.82–1.73 µg/kg for HPLC–MS/MS, and 0.16-0.42 µg/kg and 0.81-1.25 µg/kg for UPLC–MS/MS, respectively. The eggs were spiked with four concentrations of the eight coccidiostats, and the HPLC–MS/MS and UPLC–MS/MS average recoveries were all higher than 71.69% and 72.26%, respectively. Compared with the HPLC–MS/MS method, utilizing UPLC–MS/MS had the advantages of low reagent consumption, a short detection time, and high recovery and precision. Finally, the HPLC–MS/MS and UPLC–MS/MS methods were successfully applied to detect eight coccidiostats in 40 eggs.

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