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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MDPI AG
2022-11-01
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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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issn | 1420-3049 |
language | English |
last_indexed | 2024-03-09T18:08:18Z |
publishDate | 2022-11-01 |
publisher | MDPI AG |
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series | Molecules |
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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