Simultaneous LC–MS–MS determination of cyclosporine A, tacrolimus, and sirolimus in whole blood as well as mycophenolic acid in plasma using common pretreatment procedure

Bogusz, M; Enazi, Eid Al; Hassan, Huda; Abdel-Jawaad, Jamil; Ruwaily, Jamal Al; Tufail, Mohammed Al

doi:10.1016/j.jchromb.2006.12.048

Cited by 76 publications

(45 citation statements)

References 23 publications

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“…This matrix effect could be explained by the presence of undetectable co-eluting compounds with the analytes in the post-extraction sample and, in the case of tissues, also the PBS used to homogenize the samples. Bogusz et al found a signal suppression caused primarily by zinc sulfate used in deproteinizing solution [26]. However, in the present method CyA diluted in extraction solution was evaluated and showed higher peak intensity than that obtained from blank-processed samples spiked with the drug.…”

Section: Recovery and Matrix Effectmentioning

confidence: 55%

“…It was observed that an aliquot of 10% trichloroacetic acid aqueous solution improved protein precipitation. This led to a reduction in the organic solvent volumes needed to precipitate proteins reported by other authors (methanol with zinc sulfate or acetonitrile) [7,9,18,25,26], enabling the direct injection of the final supernatant for analysis and consequently improved the lower limit of quantification. The use of trichloroacetic acid as precipitation reagent has not been previously published in CyA detection methods.…”

Section: Sample Preparationmentioning

confidence: 99%

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Ultra high performance liquid chromatography–tandem mass spectrometry method for cyclosporine a quantification in biological samples and lipid nanosystems

Guada

Imbuluzqueta

Mendoza

et al. 2013

Journal of Chromatography B

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Cyclosporine A (CyA) is an immunosuppressant cyclic undecapeptide used for the prevention of organ transplant rejection and in the treatment of several autoimmune disorders. An ultra high performance liquid chromatography-tandem mass spectrometry method (UHPLC-MS/MS) to quantify CyA in lipid nanosystems and mouse biological matrices (whole blood, kidneys, lungs, spleen, liver, heart, brain, stomach and intestine) was developed and fully validated.Chromatographic separation was performed on an Acquity UPLC ® BEH C18 column with a gradient elution consisting of methanol and 2 mM ammonium acetate aqueous solution containing 0.1% formic acid at a flow rate of 0.6 mL/min. Amiodarone was used as internal standard (IS). Retention times of IS and CyA were 0.69 min and 1.09 min, respectively. Mass spectrometer operated in electrospray ionization positive mode (ESI+) and multiple reaction monitoring (MRM) transitions were detected, m/z 1220.69→1203.7 for CyA and m/z 646→58 for IS. The extraction method from biological samples consisted of a simple protein precipitation with 10% trichloroacetic acid aqueous solution and acetonitrile and 5 µL of supernatant were directly injected into the UHPLC-MS/MS system. Linearity was observed between 0.001 µg/mL-2.5 µg/mL (r ≥ 0.99) in all matrices. The precision expressed in coefficient of variation (CV) was below 11.44% and accuracy in bias ranged from −12.78% to 7.99% including methanol and biological matrices. Recovery in all cases was above 70.54% and some matrix effect was observed. CyA was found to be stable in post-extraction whole blood and liver homogenate samples exposed for 6 h at room temperature and 72 h at 4 o C. The present method was successfully applied for quality control of lipid nanocarriers as well as in vivo studies in BALB/c mice.

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Section: Recovery and Matrix Effectmentioning

confidence: 55%

Section: Sample Preparationmentioning

confidence: 99%

Ultra high performance liquid chromatography–tandem mass spectrometry method for cyclosporine a quantification in biological samples and lipid nanosystems

Guada

Imbuluzqueta

Mendoza

et al. 2013

Journal of Chromatography B

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“…Liquid-liquid and solid-phase extractions are usually the most effective approaches, but they are expensive and time consuming (Earla et al, 2012). The elimination of water-soluble inorganic metallic substances such as phosphates, sodium, and sulfates from plasma is important in ESI LC-MS/MS analysis to reduce ion suppression (Bogusz et al, 2007;Clavijo et al, 2009). In addition, the pH of the reconstitution solution and mobile phase is very important to achieve maximum chromatographic peak separation, resolution, reliability, ionization, and reproducibility.…”

Section: Discussionmentioning

confidence: 99%

“…By considering these factors, we have validated a novel, rapid, and robust ESI-LC-MS/MS assay that uses a hydrophilic-lipophilic balance SPE cartridge to analyze rhesus plasma. In this method, we used 1 ml of methanol followed by water, which is simpler and faster than the previously reported methods (Bogusz et al, 2007;Clavijo et al, 2009). In previously described methods, a higher amount of solvents was used followed by additional washing steps that also contained ammonium hydroxide, dichloromethane, and isopropanol.…”

Section: Discussionmentioning

confidence: 99%

Enhanced Methamphetamine Metabolism in Rhesus Macaque as Compared with Human: An Analysis Using a Novel Method of Liquid Chromatography with Tandem Mass Spectrometry, Kinetic Study, and Substrate Docking

Earla

Kumar²,

Wang

et al. 2014

Drug Metab Dispos

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Methamphetamine (MA), which remains one of the widely used drugs of abuse, is metabolized by the cytochrome P450 (P450) family of enzymes in humans. However, metabolism of methamphetamine in macaques is poorly understood. Therefore, we first developed and validated a very sensitive liquid chromatography with tandem mass spectrometry (LC-MS/MS) method using solid phase extraction of rhesus plasma with a lower limit of quantitation at 1.09 ng/ml for MA and its metabolites, 4-hydroxy methamphetamine (4-OH MA), amphetamine (AM), 4-OH amphetamine (4-OH AM), and norephedrine. We then analyzed plasma samples of MA-treated rhesus, which showed >10-fold higher concentrations of AM (∼29 ng/ml) and 4-OH AM (∼28 ng/ml) than MA (∼2 ng/ml). Because the plasma levels of MA metabolites in rhesus were much higher than in human samples, we examined MA metabolism in human and rhesus microsomes. Interestingly, the results showed that AM and 4-OH AM were formed more rapidly and that the catalytic efficiency (V max /K m ) for the formation of AM was ∼8-fold higher in rhesus than in human microsomes. We further examined the differences in these kinetic characteristics using three selective inhibitors of each human CYP2D6 and CYP3A4 enzymes. The results showed that each of these inhibitors inhibited both D-and L-MA metabolism by 20%-60% in human microsomes but not in rhesus microsomes. The differences between human and rhesus CYP2D6 and CYP3A4 enzymes were further assessed by docking studies for both d and l-MA. In conclusion, our results demonstrated an enhanced MA metabolism in rhesus compared with humans, which is likely to be caused by differences in MA-metabolizing P450 enzymes between these species.

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“…Therapeutic monitoring of immunosuppressive drugs is performed routinely with immunological or chromatographic procedures (35,(55)(56)(57). The most commonly used immunosuppressive drugs for maintenance therapy are cyclosporin A, sirolimus, tacrolimus and everolimus (Table 1- …”

Section: Determination Of Cyclosporin a Sirolimus Tacrolimus And Evmentioning

confidence: 99%

Development of Reference Measurement Procedures with LC-MS in Clinical Chemistry

Magdolna¹

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Simultaneous LC–MS–MS determination of cyclosporine A, tacrolimus, and sirolimus in whole blood as well as mycophenolic acid in plasma using common pretreatment procedure

Cited by 76 publications

References 23 publications

Ultra high performance liquid chromatography–tandem mass spectrometry method for cyclosporine a quantification in biological samples and lipid nanosystems

Ultra high performance liquid chromatography–tandem mass spectrometry method for cyclosporine a quantification in biological samples and lipid nanosystems

Enhanced Methamphetamine Metabolism in Rhesus Macaque as Compared with Human: An Analysis Using a Novel Method of Liquid Chromatography with Tandem Mass Spectrometry, Kinetic Study, and Substrate Docking

Development of Reference Measurement Procedures with LC-MS in Clinical Chemistry

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