Simultaneous on-line extraction and analysis of sirolimus (rapamycin) and ciclosporin in blood by liquid chromatography–electrospray mass spectrometry

Kirchner, Gabriele I.; Vidal, Christian; Jacobsen, Wolfgang; Franzke, Anke; Hallensleben, Katrin; Christians, Uwe; Sewing, Karl–Friedrich

doi:10.1016/s0378-4347(98)00463-0

Cited by 56 publications

(46 citation statements)

References 28 publications

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“…Compared to previously described methods, the combination of LC-tandem MS technology with on-line solid phase extraction enables quantification of sirolimus with a considerably shorter hands-on time (23) and running time (18). Thus, this method could be applied to large series of clinical samples.…”

Section: Discussionmentioning

confidence: 99%

“…Due to the poor UV-absorption of sirolimus, quantification using UV-detection is cumbersome and highly efficient sample clean-up is necessary (12)(13)(14)(15) phy with single-stage detection by mass spectrometry (LC-MS) overcomes the poor UV-absorption of the sirolimus molecule but requires also efficient chromatographic separation due to the limited specificity of this detection principle (16)(17)(18)(19)(20). In contrast, liquid chromatography-tandem mass spectrometry (LC-tandem MS) (syn.…”

Section: Introductionmentioning

confidence: 99%

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Quantification of Sirolimus by Liquid Chromatography-Tandem Mass Spectrometry Using On-Line Solid-Phase Extraction

Vogeser¹,

Fleischer²,

Meiser³

et al. 2002

Clinical Chemistry and Laboratory Medicine

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Quantification of the new immunosuppressant sirolimus (syn. rapamycin; Rapamune ® ) in whole blood by chromatography is essential for its clinical use since no immunoassay is available although monitoring is mandatory. Here we report on a rapid and convenient liquid chromatography (LC)-tandem mass spectrometry method and describe our practical experience with its routine use.Whole blood samples were hemolyzed and deproteinized using an equal volume (150 µl) of a mixture of methanol/zinc sulfate solution containing the internal standard desmethoxy-rapamycin. After centrifugation, the clear supernatants were submitted to an on-line solid-phase extraction procedure using the polymeric Waters Oasis HLB ® material, with elution of the extracts onto the analytical column in the back-flush mode by column switching. For analytical chromatography a RP-C18 column was used with 90/10 methanol/2 mM ammonium acetate as the mobile phase. A 1:10 split was used for the transfer to the mass spectrometer, a Micromass Quattro LC-tandem mass spectrometry system equipped with a Z-spray ® source and used in the positive electrospray ionization mode. The following transitions were recorded: sirolimus, 931>864 m/z, and desmethoxy-rapamycin (I.S.), 901>834 m/z. The analytical running time was 5 min, including on-line extraction.The method has a linear calibration curve (r>0.99; range 1.6-50 µg/l) and is rugged and precise with monthly CVs <7% at a sirolimus concentration of 13.1 µg/l in routine use; the instrumentation proved to be reliable and required minimal maintenance. Clin Chem Lab Med 2002; 40(1):40-45

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Section: Discussionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Quantification of Sirolimus by Liquid Chromatography-Tandem Mass Spectrometry Using On-Line Solid-Phase Extraction

Vogeser¹,

Fleischer²,

Meiser³

et al. 2002

Clinical Chemistry and Laboratory Medicine

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“…589 The sensitivity and selectivity provided by MS helped to ease sample preparation in clinical chemistry laboratories. Column-switching systems coupling the extraction support to the chromatographic column before MS detection were also used for the analysis of sirolimus [598][599][600][601][602][603][604][605][606][607][608][609][610][611] and everolimus 598,599,602,603,[605][606][607]609,[612][613][614] in whole blood. LLE 615 or SPE 616 on 96-well plates constitutes another approach for sample preparation automatisation.…”

Section: Mtor Inhibitorsmentioning

confidence: 99%

Antineoplastic drugs and their analysis: a state of the art review

Guichard

Guillarme

Bonnabry

et al. 2017

Analyst

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The number of patients suffering from cancer is constantly increasing and, consequently, the number of different chemotherapy treatments administered is increasing. Given the high reactivity and toxicity of antineoplastic drugs, analytical methods are required in all pharmaceutical fields, from drug development to their elimination in wastewater; including formulation quality control, environment and human exposure and therapeutic drug monitoring. The aim of this paper is to provide an overview of the analytical methods available for the determination of antineoplastic drugs in different matrices such as pharmaceutical formulations, biological and environmental samples. The applicability and performance of the reported methods will be critically discussed, with focus on the most commonly used antineoplastic drugs. Only conventional compounds and small molecules for targeted therapy will be considered in the present review.

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“…Several HPLC methods with ultraviolet (UV) detection or mass spectrometry (MS) are available for measurement of SRL and SDZ-RAD individually (10 -16 ), and liquid chromatography (LC) methods using MS or tandem MS allow simultaneous measurement of these compounds in combination with other immunosuppressants (17)(18)(19)(20)(21)(22). The purported advantage of LC-MS methods over LC-UV methods is the ability to monitor multiple drugs within the same analytical run.…”

Section: Simultaneous Measurement Of Sirolimus and Everolimus In Wholmentioning

confidence: 99%

Simultaneous Measurement of Sirolimus and Everolimus in Whole Blood by HPLC with Ultraviolet Detection

Khoschsorur

2005

Clinical Chemistry

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146 -254 g/L. As long as more valid data are lacking, serum concentrations of 146 -254 g/L can be considered as a preliminary target range for TDM of aripiprazole. Moreover, it should be stressed that because pure and authentic reference materials for aripiprazole and its metabolite were not available, the accuracy of the method described here remains uncertain.We thank Sandra Heller for skillful technical assistance. Note Added in Proof:The manufacturer (Bristol-Myers Squibb) has subsequently provided us with pure aripiprazole. We prepared samples containing 50, 250, 500, and 1000 g/L and assayed them with our method. The results obtained were 49, 240, 488, and 995 g/L.References

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Simultaneous on-line extraction and analysis of sirolimus (rapamycin) and ciclosporin in blood by liquid chromatography–electrospray mass spectrometry

Cited by 56 publications

References 28 publications

Quantification of Sirolimus by Liquid Chromatography-Tandem Mass Spectrometry Using On-Line Solid-Phase Extraction

Quantification of Sirolimus by Liquid Chromatography-Tandem Mass Spectrometry Using On-Line Solid-Phase Extraction

Antineoplastic drugs and their analysis: a state of the art review

Simultaneous Measurement of Sirolimus and Everolimus in Whole Blood by HPLC with Ultraviolet Detection

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