Comparison of extraction procedures for assessment of matrix effect for selective and reliable determination of atazanavir in human plasma by LC–ESI-MS/MS
“…The present work was executed using electrospray ionization (ESI) in the positive ionization mode as ATV, DRV, and RTV have several secondary amino groups which can be readily protonated. Q1 mass spectra of ATV, DRV, RTV, ATV-d6, DRV-d9, and RTV-d6 contained protonated precursor [M+H] + ions at m/z 705.2, 548.1, 721.3, 711.2, 557.1 and 727.4 respectively as reported in our previous work [13, 17, 21]. The most abundant and consistent product ions in Q3 mass spectra for ATV, DRV and RTV were observed at m/z 167.9, 392.0 and 296.3 by applying collision energy of 44, 17 and 20 eV respectively.…”
Section: Discussionsupporting
confidence: 61%
“…Based on our earlier work for ATV and RTV [13, 21], various combinations of organic solvents (methanol/acetonitrile) together with ammonium formate/formic acid buffer in the pH range 3.5–5.5 were tried. However, the run time was more than 4.0 min for baseline resolution of the analytes.…”
Objectives. HIV protease inhibitors are used in the treatment of patients suffering from AIDS and they act at the final stage of viral replication by interfering with the HIV protease enzyme. The paper describes a selective, sensitive, and robust method for simultaneous determination of three protease inhibitors atazanavir, darunavir and ritonavir in human plasma by ultra performance liquid chromatography-tandem mass spectrometry. Materials and Methods. The sample pretreatment consisted of solid phase extraction of analytes and their deuterated analogs as internal standards from 50 μL human plasma. Chromatographic separation of analytes was performed on Waters Acquity UPLC C18 (50 × 2.1 mm, 1.7 μm) column under gradient conditions using 10 mM ammonium formate, pH 4.0, and acetonitrile as the mobile phase. Results. The method was established over a concentration range of 5.0–6000 ng/mL for atazanavir, 5.0–5000 ng/mL for darunavir and 1.0–500 ng/mL for ritonavir. Accuracy, precision, matrix effect, recovery, and stability of the analytes were evaluated as per US FDA guidelines. Conclusions. The efficiency of sample preparation, short analysis time, and high selectivity permit simultaneous estimation of these inhibitors. The validated method can be useful in determining plasma concentration of these protease inhibitors for therapeutic drug monitoring and in high throughput clinical studies.
“…The present work was executed using electrospray ionization (ESI) in the positive ionization mode as ATV, DRV, and RTV have several secondary amino groups which can be readily protonated. Q1 mass spectra of ATV, DRV, RTV, ATV-d6, DRV-d9, and RTV-d6 contained protonated precursor [M+H] + ions at m/z 705.2, 548.1, 721.3, 711.2, 557.1 and 727.4 respectively as reported in our previous work [13, 17, 21]. The most abundant and consistent product ions in Q3 mass spectra for ATV, DRV and RTV were observed at m/z 167.9, 392.0 and 296.3 by applying collision energy of 44, 17 and 20 eV respectively.…”
Section: Discussionsupporting
confidence: 61%
“…Based on our earlier work for ATV and RTV [13, 21], various combinations of organic solvents (methanol/acetonitrile) together with ammonium formate/formic acid buffer in the pH range 3.5–5.5 were tried. However, the run time was more than 4.0 min for baseline resolution of the analytes.…”
Objectives. HIV protease inhibitors are used in the treatment of patients suffering from AIDS and they act at the final stage of viral replication by interfering with the HIV protease enzyme. The paper describes a selective, sensitive, and robust method for simultaneous determination of three protease inhibitors atazanavir, darunavir and ritonavir in human plasma by ultra performance liquid chromatography-tandem mass spectrometry. Materials and Methods. The sample pretreatment consisted of solid phase extraction of analytes and their deuterated analogs as internal standards from 50 μL human plasma. Chromatographic separation of analytes was performed on Waters Acquity UPLC C18 (50 × 2.1 mm, 1.7 μm) column under gradient conditions using 10 mM ammonium formate, pH 4.0, and acetonitrile as the mobile phase. Results. The method was established over a concentration range of 5.0–6000 ng/mL for atazanavir, 5.0–5000 ng/mL for darunavir and 1.0–500 ng/mL for ritonavir. Accuracy, precision, matrix effect, recovery, and stability of the analytes were evaluated as per US FDA guidelines. Conclusions. The efficiency of sample preparation, short analysis time, and high selectivity permit simultaneous estimation of these inhibitors. The validated method can be useful in determining plasma concentration of these protease inhibitors for therapeutic drug monitoring and in high throughput clinical studies.
“…To reduce the matrix influence, protein participation, solid phase extraction (SPE), liquid-liquid extraction, sample dilution or flow reduction are used for sample purification [24][25][26][27][28][29]. The matrix evaluation by Kittlaus et al [24] demonstrated the beneficial effect of multiple sequential sample preparation steps.…”
“…With many recognized advantages in terms of sensitivity, selectivity, and specificity, which allow for the analysis of trace amounts of target analytes in complex matrices, LC‐MS/MS technique has become a powerful analytical tool. However, owing to the presence of matrix effects in LC‐MS/MS analysis, an efficient sample cleanup procedure or suitable dilution is indeed necessary .…”
A novel, sensitive, and reliable LC-MS/MS method for multiresidue analysis of nine β-agonists (salbutamol, terbutaline, cimaterol, fenoterol, clorprenaline, ractopamine, tulobuterol, clenbuterol, and penbuterol) in four farm animal muscles was developed. Muscle matrix was extracted with acetonitrile-10% sodium carbonate solution, and then was subjected to cleanup using a SPE cartridge packed with new polymer synthesized in acetone. Chromatographic separation of the components was performed on a Luna C18 column using 0.1% of formic acid in water and acetonitrile. The mass spectrometer was operated in the positive electrospray mode. Good precision and accuracy were obtained for all analytes (except for fenoterol) at the spiked three levels of 1.0, 10, and 50 μg/kg. The decision limit and detection capability of nine β-agonists ranged from 0.04 to 0.18 and 0.15 to 0.69 μg/kg, respectively. The method developed was successfully applied to the monitoring of nine β-agonists in pork, beef, mutton, and chicken from Chinese markets.
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