Development and Validation of an LC-MS/MS Method for Simultaneous Determination of Short Peptide-Based Drugs in Human Blood Plasma

A novel HPLC-ESI-MS/MS method for simultaneous gonadotropin-releasing hormone (GnRH) analogs and somatostatin analog quantitation was developed and validated. The developed method was successfully applied to pharmacokinetic studies. The sample preparation process included solid-phase extraction (SPE...

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Main Authors: Elizaveta N. Fisher, Evgeny S. Melnikov, Vladimir Gegeckori, Natalya V. Potoldykova, Dmitry V. Enikeev, Kirill A. Pavlenko, Snezana Agatonovic-Kustrin, David W. Morton, Galina V. Ramenskaya
Format: Article
Language:English
Published: MDPI AG 2022-11-01
Series:Molecules
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Online Access:https://www.mdpi.com/1420-3049/27/22/7831
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author Elizaveta N. Fisher
Evgeny S. Melnikov
Vladimir Gegeckori
Natalya V. Potoldykova
Dmitry V. Enikeev
Kirill A. Pavlenko
Snezana Agatonovic-Kustrin
David W. Morton
Galina V. Ramenskaya
author_facet Elizaveta N. Fisher
Evgeny S. Melnikov
Vladimir Gegeckori
Natalya V. Potoldykova
Dmitry V. Enikeev
Kirill A. Pavlenko
Snezana Agatonovic-Kustrin
David W. Morton
Galina V. Ramenskaya
author_sort Elizaveta N. Fisher
collection DOAJ
description A novel HPLC-ESI-MS/MS method for simultaneous gonadotropin-releasing hormone (GnRH) analogs and somatostatin analog quantitation was developed and validated. The developed method was successfully applied to pharmacokinetic studies. The sample preparation process included solid-phase extraction (SPE). Effective chromatographic separation of the analytes and internal standard (dalargin) was achieved with a C18 column, using a gradient elution with two mobile phases: 0.1% <i>v</i>/<i>v</i> formic acid (aqueous solution) and 0.1% <i>v</i>/<i>v</i> formic acid (acetonitrile solution). The linearity of the method was demonstrated within a concentration range of 0.5–20 ng/mL, with correlation coefficients between 0.998–0.999 for goserelin, buserelin, triptorelin, and octreotide, respectively. The relative standard deviation (RSD, %) values for method accuracy and precision did not exceed 20% at the lower level of quantitation (LLOQ) or 15% at other concentration levels.
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spelling doaj.art-cdcb27d8246044f597f639ff206915f72023-11-24T09:21:54ZengMDPI AGMolecules1420-30492022-11-012722783110.3390/molecules27227831Development and Validation of an LC-MS/MS Method for Simultaneous Determination of Short Peptide-Based Drugs in Human Blood PlasmaElizaveta N. Fisher0Evgeny S. Melnikov1Vladimir Gegeckori2Natalya V. Potoldykova3Dmitry V. Enikeev4Kirill A. Pavlenko5Snezana Agatonovic-Kustrin6David W. Morton7Galina V. Ramenskaya8I.M. Sechenov First MSMU of the Ministry of Health of the Russian Federation, Sechenov University, 8, Trubetskaya Street, 119991 Moscow, RussiaI.M. Sechenov First MSMU of the Ministry of Health of the Russian Federation, Sechenov University, 8, Trubetskaya Street, 119991 Moscow, RussiaI.M. Sechenov First MSMU of the Ministry of Health of the Russian Federation, Sechenov University, 8, Trubetskaya Street, 119991 Moscow, RussiaInstitute for Urology and Reproductive Health, I.M. Sechenov First MSMU of the Ministry of Health of the Russian Federation, Sechenov University, 8, Trubetskaya Street, 119991 Moscow, RussiaInstitute for Urology and Reproductive Health, I.M. Sechenov First MSMU of the Ministry of Health of the Russian Federation, Sechenov University, 8, Trubetskaya Street, 119991 Moscow, RussiaMoscow Clinical Scientific Center, 86, Shosse Enthuziastov, 111123 Moscow, RussiaI.M. Sechenov First MSMU of the Ministry of Health of the Russian Federation, Sechenov University, 8, Trubetskaya Street, 119991 Moscow, RussiaI.M. Sechenov First MSMU of the Ministry of Health of the Russian Federation, Sechenov University, 8, Trubetskaya Street, 119991 Moscow, RussiaI.M. Sechenov First MSMU of the Ministry of Health of the Russian Federation, Sechenov University, 8, Trubetskaya Street, 119991 Moscow, RussiaA novel HPLC-ESI-MS/MS method for simultaneous gonadotropin-releasing hormone (GnRH) analogs and somatostatin analog quantitation was developed and validated. The developed method was successfully applied to pharmacokinetic studies. The sample preparation process included solid-phase extraction (SPE). Effective chromatographic separation of the analytes and internal standard (dalargin) was achieved with a C18 column, using a gradient elution with two mobile phases: 0.1% <i>v</i>/<i>v</i> formic acid (aqueous solution) and 0.1% <i>v</i>/<i>v</i> formic acid (acetonitrile solution). The linearity of the method was demonstrated within a concentration range of 0.5–20 ng/mL, with correlation coefficients between 0.998–0.999 for goserelin, buserelin, triptorelin, and octreotide, respectively. The relative standard deviation (RSD, %) values for method accuracy and precision did not exceed 20% at the lower level of quantitation (LLOQ) or 15% at other concentration levels.https://www.mdpi.com/1420-3049/27/22/7831LC-ESI-MS/MSpeptide drugsGnRH analogssomatostatin analoguesolid-phase extraction
spellingShingle Elizaveta N. Fisher
Evgeny S. Melnikov
Vladimir Gegeckori
Natalya V. Potoldykova
Dmitry V. Enikeev
Kirill A. Pavlenko
Snezana Agatonovic-Kustrin
David W. Morton
Galina V. Ramenskaya
Development and Validation of an LC-MS/MS Method for Simultaneous Determination of Short Peptide-Based Drugs in Human Blood Plasma
Molecules
LC-ESI-MS/MS
peptide drugs
GnRH analogs
somatostatin analogue
solid-phase extraction
title Development and Validation of an LC-MS/MS Method for Simultaneous Determination of Short Peptide-Based Drugs in Human Blood Plasma
title_full Development and Validation of an LC-MS/MS Method for Simultaneous Determination of Short Peptide-Based Drugs in Human Blood Plasma
title_fullStr Development and Validation of an LC-MS/MS Method for Simultaneous Determination of Short Peptide-Based Drugs in Human Blood Plasma
title_full_unstemmed Development and Validation of an LC-MS/MS Method for Simultaneous Determination of Short Peptide-Based Drugs in Human Blood Plasma
title_short Development and Validation of an LC-MS/MS Method for Simultaneous Determination of Short Peptide-Based Drugs in Human Blood Plasma
title_sort development and validation of an lc ms ms method for simultaneous determination of short peptide based drugs in human blood plasma
topic LC-ESI-MS/MS
peptide drugs
GnRH analogs
somatostatin analogue
solid-phase extraction
url https://www.mdpi.com/1420-3049/27/22/7831
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