Optimization of an HPLC-PDA analytical method for therapeutic monitoring of oral busulfan in hematopoietic stem cell transplant patients
Autor(a) principal: | |
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Data de Publicação: | 2021 |
Outros Autores: | , , , , , , , , |
Tipo de documento: | Artigo |
Idioma: | por |
Título da fonte: | Research, Society and Development |
Texto Completo: | https://rsdjournal.org/index.php/rsd/article/view/15864 |
Resumo: | The study aims to develop activities for therapeutic monitoring of oral busulfan in patients undergoing heterologous stem-cell transplantation (HSCT) through the identification and determination of plasma busulfan. It was used HPLC-PDA Shimadzu C18 column (150 mm x 4 mm), methanol/water/acetonitrile (65:20:15, v/v/v), flow rate 1 mL min-1, UV λ=276 nm, analysis time 17 min; derivatization with sodium diethylcarbamate, extraction with ethyl acetate; linear calibration curve over the range of 200-5000 ng ml-1. The average relative recovery of the controls was 89% ± 0.04 (QCH=86%; QCM=87%; QCL=93%), and the internal standard (IS) was 74%±0.47. The mean absolute recovery of the controls was 114±0.03% (QCH=111%, QCM=118%; QCL=113%), and the IS was 102±2.5%. The lower limits of detection and quantification obtained were respectively 200 ng ml-1 and 40 ng.mL-1. The linearity was evaluated by calibration curve (200-5000 ng.mL-1) (r=0.998, r=0.994, r=0.998). The repeatability (intracorrida) resulted in 1.25% -11.25% and intermediate precision (intercorrida) resulted in 2.17% -10.71%. The accuracy was found to be 89.61% -102.18%. The short-term stability of the solutions and samples extracted was 6.25% and 3.18% for QCL, 7.54% and 2.4% for QCH, and 4.13% and 13.17% for IS, respectively. The stability of freeze-thaw cycles extracted samples and the solutions was 3.64% and 2.53% for QCL, 9.09% and 5.65% and QCH to 4.82% and 10.32% for IS, respectively. It was concludefd that it was possible to describe a technique for determining the busulfan in plasma by HPLC-PDA, settling their validation parameters for therapeutic drug monitoring purposes. |
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Optimization of an HPLC-PDA analytical method for therapeutic monitoring of oral busulfan in hematopoietic stem cell transplant patientsOptimización de un método analítico HPLC-PDA para la monitorización terapéutica de busulfán oral en pacientes con trasplante de células madre hematopoyéticasOtimização de método analítico em HPLC-PDA para monitoração terapêutica do bussulfano oral em pacientes transplantados de células-tronco hematopoiéticasBusulfanHPLCTherapeutic drug monitoring.BusulfánHPLCMonitorización terapéutica. HPLCBusulfanoMonitoramento de medicamentos.The study aims to develop activities for therapeutic monitoring of oral busulfan in patients undergoing heterologous stem-cell transplantation (HSCT) through the identification and determination of plasma busulfan. It was used HPLC-PDA Shimadzu C18 column (150 mm x 4 mm), methanol/water/acetonitrile (65:20:15, v/v/v), flow rate 1 mL min-1, UV λ=276 nm, analysis time 17 min; derivatization with sodium diethylcarbamate, extraction with ethyl acetate; linear calibration curve over the range of 200-5000 ng ml-1. The average relative recovery of the controls was 89% ± 0.04 (QCH=86%; QCM=87%; QCL=93%), and the internal standard (IS) was 74%±0.47. The mean absolute recovery of the controls was 114±0.03% (QCH=111%, QCM=118%; QCL=113%), and the IS was 102±2.5%. The lower limits of detection and quantification obtained were respectively 200 ng ml-1 and 40 ng.mL-1. The linearity was evaluated by calibration curve (200-5000 ng.mL-1) (r=0.998, r=0.994, r=0.998). The repeatability (intracorrida) resulted in 1.25% -11.25% and intermediate precision (intercorrida) resulted in 2.17% -10.71%. The accuracy was found to be 89.61% -102.18%. The short-term stability of the solutions and samples extracted was 6.25% and 3.18% for QCL, 7.54% and 2.4% for QCH, and 4.13% and 13.17% for IS, respectively. The stability of freeze-thaw cycles extracted samples and the solutions was 3.64% and 2.53% for QCL, 9.09% and 5.65% and QCH to 4.82% and 10.32% for IS, respectively. It was concludefd that it was possible to describe a technique for determining the busulfan in plasma by HPLC-PDA, settling their validation parameters for therapeutic drug monitoring purposes.Se optimizó un método para la monitorización plasmática de busulfán en pacientes sometidos a trasplante de células madre hematopoyéticas (TCMH). HPLC-PDA Shimadzu, columna C18 (150 mm x 4 mm), metanol/agua/acetonitrilo (65:20:15, v/v/v), se usó un flujo de 1 ml min-1; UV λ = 276 nm, tiempo de análisis 17 min; derivatización con dietilcarbamato de sodio, extracción con acetato de etilo; curva de calibración lineal de 200-5000 ng.mL-1. La recuperación relativa de los controles fue de 89% ± 0,04 (CQA = 86%; CQM = 87%; CQB = 93%) y la del EI (estándar interno) fue de 74% ± 0,47. La recuperación absoluta de los controles fue 114% ± 0.03 (CQA = 111%; CQM = 118%; CQB = 113%), y la del EI fue 102% ± 2.5. Los límites inferiores de cuantificación y detección obtenidos fueron, respectivamente, 200 ng.mL-1 y 40 ng.mL-1. La linealidad se analizó mediante la curva de calibración (200–5000 ng.mL-1) (r = 0,998). La repetibilidad (intra-análisis) fue de 1,25% -11,25% y la precisión intermedia (entre análisis), 2,17% -10,71%. La precisión encontrada fue de 89,61% -102,18%. La estabilidad a corto plazo de las muestras y soluciones extraídas fue de 6.25% y 3.18% para CQB, 7.54% y 2.4% para CQA y 13.17% y 4.13% para EI, respectivamente. La estabilidad de los ciclos de congelación y descongelación de las muestras y soluciones extraídas fue de 3.64% y 2.53% para CQB, 9.09% y 5.65% para CQA y 10.32% y 4.82% para EI, respectivamente. Así, fue posible validar una técnica para la determinación de busulfán en plasma por HPLC-PDA, adecuada para monitorización terapéutica de los pacientes.Otimizou-se método para monitoração plasmática de bussulfano em pacientes submetidos a transplante de células-tronco hematopoiéticas (TCTH). Utilizou-se HPLC-PDA Shimadzu, coluna C18 (150 mm x 4 mm), metanol/água/acetonitrila (65:20:15, v/v/v), fluxo 1 mL min-1; UV λ = 276 nm, tempo de análise de 17 min; derivatização com dietilcarbamato de sódio, extração com acetato de etila; curva de calibração linear de 200-5000 ng mL-1. A recuperação relativa dos controles foi de 89%±0,04 (CQA = 86%; CQM = 87%; CQB = 93%) e a do PI (padrão interno) foi de 74%±0,47. A recuperação absoluta dos controles foi de 114%±0,03 (CQA = 111%; CQM = 118%; CQB = 113%), e a do PI foi de 102%±2,5. Os limites inferiores de quantificação e detecção obtidos foram, respectivamente, de 200 ng mL-1 e 40 ng mL-1. A linearidade foi analisada pela curva de calibração (200–5000 ng.mL-1) (r = 0,998). A repetibilidade (intracorrida) foi de 1,25%-11,25%, e a precisão intermediária (intercorrida), 2,17%-10,71%. A exatidão encontrada foi de 89,61%-102,18%. A estabilidade de curta duração de amostras extraídas e das soluções foi de 6,25% e 3,18% para CQB, 7,54% e 2,4% para CQA e 13,17% e 4,13% para PI, respectivamente. A estabilidade de ciclos de congelamento e descongelamento de amostras extraídas e das soluções foi de 3,64% e 2,53% para CQB, 9,09% e 5,65% para CQA e 10,32% e 4,82% para PI, respectivamente. Desta forma, foi possível validar uma técnica para determinação do bussulfano em plasma por HPLC-PDA, adequada à monitorização terapêutica de pacientes.Research, Society and Development2021-06-07info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersionapplication/pdfhttps://rsdjournal.org/index.php/rsd/article/view/1586410.33448/rsd-v10i6.15864Research, Society and Development; Vol. 10 No. 6; e48110615864Research, Society and Development; Vol. 10 Núm. 6; e48110615864Research, Society and Development; v. 10 n. 6; e481106158642525-3409reponame:Research, Society and Developmentinstname:Universidade Federal de Itajubá (UNIFEI)instacron:UNIFEIporhttps://rsdjournal.org/index.php/rsd/article/view/15864/14319Copyright (c) 2021 Cristiane Effting; Fernando Gomes Ferreira Oliveira; Iram Moreira Mundim; Alessandro de Carvalho Cruz; Andryne Rego Rodrigues; Caroline Rego Rodrigues; Jerônimo Raimundo de Oliveira-Neto; Marianna Medeiros Barros da Cunha; Adriano de Moraes Arantes; Luiz Carlos da Cunhahttps://creativecommons.org/licenses/by/4.0info:eu-repo/semantics/openAccessEffting, Cristiane Oliveira, Fernando Gomes Ferreira Mundim, Iram Moreira Cruz, Alessandro de CarvalhoRodrigues, Andryne Rego Rodrigues, Caroline Rego Oliveira-Neto, Jerônimo Raimundo de Cunha, Marianna Medeiros Barros da Arantes, Adriano de Moraes Cunha, Luiz Carlos da2021-06-10T22:51:46Zoai:ojs.pkp.sfu.ca:article/15864Revistahttps://rsdjournal.org/index.php/rsd/indexPUBhttps://rsdjournal.org/index.php/rsd/oairsd.articles@gmail.com2525-34092525-3409opendoar:2024-01-17T09:36:35.414966Research, Society and Development - Universidade Federal de Itajubá (UNIFEI)false |
dc.title.none.fl_str_mv |
Optimization of an HPLC-PDA analytical method for therapeutic monitoring of oral busulfan in hematopoietic stem cell transplant patients Optimización de un método analítico HPLC-PDA para la monitorización terapéutica de busulfán oral en pacientes con trasplante de células madre hematopoyéticas Otimização de método analítico em HPLC-PDA para monitoração terapêutica do bussulfano oral em pacientes transplantados de células-tronco hematopoiéticas |
title |
Optimization of an HPLC-PDA analytical method for therapeutic monitoring of oral busulfan in hematopoietic stem cell transplant patients |
spellingShingle |
Optimization of an HPLC-PDA analytical method for therapeutic monitoring of oral busulfan in hematopoietic stem cell transplant patients Effting, Cristiane Busulfan HPLC Therapeutic drug monitoring. Busulfán HPLC Monitorización terapéutica. HPLC Busulfano Monitoramento de medicamentos. |
title_short |
Optimization of an HPLC-PDA analytical method for therapeutic monitoring of oral busulfan in hematopoietic stem cell transplant patients |
title_full |
Optimization of an HPLC-PDA analytical method for therapeutic monitoring of oral busulfan in hematopoietic stem cell transplant patients |
title_fullStr |
Optimization of an HPLC-PDA analytical method for therapeutic monitoring of oral busulfan in hematopoietic stem cell transplant patients |
title_full_unstemmed |
Optimization of an HPLC-PDA analytical method for therapeutic monitoring of oral busulfan in hematopoietic stem cell transplant patients |
title_sort |
Optimization of an HPLC-PDA analytical method for therapeutic monitoring of oral busulfan in hematopoietic stem cell transplant patients |
author |
Effting, Cristiane |
author_facet |
Effting, Cristiane Oliveira, Fernando Gomes Ferreira Mundim, Iram Moreira Cruz, Alessandro de Carvalho Rodrigues, Andryne Rego Rodrigues, Caroline Rego Oliveira-Neto, Jerônimo Raimundo de Cunha, Marianna Medeiros Barros da Arantes, Adriano de Moraes Cunha, Luiz Carlos da |
author_role |
author |
author2 |
Oliveira, Fernando Gomes Ferreira Mundim, Iram Moreira Cruz, Alessandro de Carvalho Rodrigues, Andryne Rego Rodrigues, Caroline Rego Oliveira-Neto, Jerônimo Raimundo de Cunha, Marianna Medeiros Barros da Arantes, Adriano de Moraes Cunha, Luiz Carlos da |
author2_role |
author author author author author author author author author |
dc.contributor.author.fl_str_mv |
Effting, Cristiane Oliveira, Fernando Gomes Ferreira Mundim, Iram Moreira Cruz, Alessandro de Carvalho Rodrigues, Andryne Rego Rodrigues, Caroline Rego Oliveira-Neto, Jerônimo Raimundo de Cunha, Marianna Medeiros Barros da Arantes, Adriano de Moraes Cunha, Luiz Carlos da |
dc.subject.por.fl_str_mv |
Busulfan HPLC Therapeutic drug monitoring. Busulfán HPLC Monitorización terapéutica. HPLC Busulfano Monitoramento de medicamentos. |
topic |
Busulfan HPLC Therapeutic drug monitoring. Busulfán HPLC Monitorización terapéutica. HPLC Busulfano Monitoramento de medicamentos. |
description |
The study aims to develop activities for therapeutic monitoring of oral busulfan in patients undergoing heterologous stem-cell transplantation (HSCT) through the identification and determination of plasma busulfan. It was used HPLC-PDA Shimadzu C18 column (150 mm x 4 mm), methanol/water/acetonitrile (65:20:15, v/v/v), flow rate 1 mL min-1, UV λ=276 nm, analysis time 17 min; derivatization with sodium diethylcarbamate, extraction with ethyl acetate; linear calibration curve over the range of 200-5000 ng ml-1. The average relative recovery of the controls was 89% ± 0.04 (QCH=86%; QCM=87%; QCL=93%), and the internal standard (IS) was 74%±0.47. The mean absolute recovery of the controls was 114±0.03% (QCH=111%, QCM=118%; QCL=113%), and the IS was 102±2.5%. The lower limits of detection and quantification obtained were respectively 200 ng ml-1 and 40 ng.mL-1. The linearity was evaluated by calibration curve (200-5000 ng.mL-1) (r=0.998, r=0.994, r=0.998). The repeatability (intracorrida) resulted in 1.25% -11.25% and intermediate precision (intercorrida) resulted in 2.17% -10.71%. The accuracy was found to be 89.61% -102.18%. The short-term stability of the solutions and samples extracted was 6.25% and 3.18% for QCL, 7.54% and 2.4% for QCH, and 4.13% and 13.17% for IS, respectively. The stability of freeze-thaw cycles extracted samples and the solutions was 3.64% and 2.53% for QCL, 9.09% and 5.65% and QCH to 4.82% and 10.32% for IS, respectively. It was concludefd that it was possible to describe a technique for determining the busulfan in plasma by HPLC-PDA, settling their validation parameters for therapeutic drug monitoring purposes. |
publishDate |
2021 |
dc.date.none.fl_str_mv |
2021-06-07 |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/article info:eu-repo/semantics/publishedVersion |
format |
article |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
https://rsdjournal.org/index.php/rsd/article/view/15864 10.33448/rsd-v10i6.15864 |
url |
https://rsdjournal.org/index.php/rsd/article/view/15864 |
identifier_str_mv |
10.33448/rsd-v10i6.15864 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.none.fl_str_mv |
https://rsdjournal.org/index.php/rsd/article/view/15864/14319 |
dc.rights.driver.fl_str_mv |
https://creativecommons.org/licenses/by/4.0 info:eu-repo/semantics/openAccess |
rights_invalid_str_mv |
https://creativecommons.org/licenses/by/4.0 |
eu_rights_str_mv |
openAccess |
dc.format.none.fl_str_mv |
application/pdf |
dc.publisher.none.fl_str_mv |
Research, Society and Development |
publisher.none.fl_str_mv |
Research, Society and Development |
dc.source.none.fl_str_mv |
Research, Society and Development; Vol. 10 No. 6; e48110615864 Research, Society and Development; Vol. 10 Núm. 6; e48110615864 Research, Society and Development; v. 10 n. 6; e48110615864 2525-3409 reponame:Research, Society and Development instname:Universidade Federal de Itajubá (UNIFEI) instacron:UNIFEI |
instname_str |
Universidade Federal de Itajubá (UNIFEI) |
instacron_str |
UNIFEI |
institution |
UNIFEI |
reponame_str |
Research, Society and Development |
collection |
Research, Society and Development |
repository.name.fl_str_mv |
Research, Society and Development - Universidade Federal de Itajubá (UNIFEI) |
repository.mail.fl_str_mv |
rsd.articles@gmail.com |
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1797052749979844608 |