High-Performance Liquid Chromatographic Quantification of Busulfan in Human Serum after Fluorescence Derivatization by 2-Naphthalenethiol

Hara, Shuuji; Tsuchie, Masahiko; Tsujioka, Riko; Kimura, Masahiko; Fujii, Megumi; Kuroda, Takeshi; Ono, Nobufumi

doi:10.2116/analsci.16.287

Cited by 11 publications

(5 citation statements)

References 23 publications

Supporting

Mentioning

Contrasting

Unclassified

Order By: Relevance

“…Os valores de exatidão e precisão encontrados na literatura (Chow et al, 1997;Heggie et al, 1997;Peris et al, 1999;Bleyzac et al, 2000;Hara et al, 2000) assemelham-se aos dados obtidos no presente estudo (Tabela 2) e estão abaixo dos limites estabelecidos pela RE nº 899/2003, da ANVISA (Brasil, 2003), para métodos bioanalíticos (precisão até 20% para o LIQ e 15% para os demais pontos da curva de calibração, e exatidão de 80 a 120%). Com referência à mesma Resolução acrescenta-se, ainda, que o processo de validação preencheu todos os critérios de aceitação da curva de calibração, incluindo valores de precisão e de exatidão para cada ponto e o coeficiente de correlação linear, que deve ser igual ou superior a 0,98.…”

Section: Discussionunclassified

Otimização de método analítico em HPLC-PDA para monitoração terapêutica do bussulfano oral em pacientes transplantados de células-tronco hematopoiéticas

Effting

Oliveira²,

Mundim

et al. 2021

RSD

View full text Add to dashboard Cite

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.

show abstract

Section: Discussionunclassified

Otimização de método analítico em HPLC-PDA para monitoração terapêutica do bussulfano oral em pacientes transplantados de células-tronco hematopoiéticas

Effting

Oliveira²,

Mundim

et al. 2021

RSD

View full text Add to dashboard Cite

show abstract

“…Plasma sample preparation followed Hara's method [11]. 300 µL plasma standard or 100 µL patient plasma samples diluted with 200 µL water were spiked with 10 µL internal standard (20 µg/mL).…”

Section: Busulfan Hplc-flmentioning

confidence: 99%

“…The stability test and recovery of busulfan in plasma using ethyl acetate were not repeated since these studies were well established in references [11,13]. Linearity was assessed by weighted linear regression (1/conc.)…”

Section: Assay Partial Validationmentioning

confidence: 99%

“…Different analytical methods have been developed for busulfan measurement in plasma and other biological fluids, including GC and GC-MS [4][5][6][7], HPLC with UV detection [8][9][10], and with fluorescence detection [11,12] and LC-MS [13,14]. In the present study, we compared two published methods: (1) a rapid and accurate LC-MS assay with SIM mode, (2) a sensitive HPLC-FL assay using 2-naphthalenethiol derivatization for the busulfan quantitation.…”

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

Comparison of LC-MS Assay and HPLC Assay of Busulfan in Clinical Pharmacokinetics Studies

Lin¹,

Goodin²,

Strair³

et al. 2012

ISRN Analytical Chemistry

View full text Add to dashboard Cite

Busulfan is used in preparative regimens for bone marrow transplantation and timely busulfan plasma concentration reporting is critical for subsequent dose adjustment. We compared two sensitive methods for pharmacokinetics studies including LC-MS assay and HPLC precolumn derivatization assay. Chromatographic separation was performed on a Gemini C18column. Liquid-liquid extraction with ethyl acetate was used for plasma sample preparation. Busulfan and internal standard ([2H8]-busulfan) were detected as ammonium adducts at m/z 264.2 and 272.2 for LC-MS assay. For HPLC assay, the extraction from plasma was derivatized with 2-naphathalenethiol using synthesized internal standard (1,6-(methanesulfonyloxy)octane). The Ex and Em wavelength was 255 nm and 370 nm. The limit of detection was 15.6 ng/mL and 7.8 ng/mL for HPLC and LC-MS assay and good linearity ranging from 31.25–1000 ng/mL for HPLC and 15.6-1000 ng/mL for LC-MS assay. The intra and interday assay precision were less than 9.2% and 12.0% for LC-MS and HPLC assay. The pharmacokinetic parameters were estimated using noncompartmental pharmacokinetic model with WinNonlin. Busulfan AUClast showed an average difference of 0.7% between the two methods. The LC-MS method is accurate, reproducible, and requires less specimen, sample preparation and analysis time over the HPLC assay, making busulfan monitoring faster and easier in clinical practice.

show abstract

“…Prior to transplantation, the patient was given a 0.5-mg/kg oral test dose of BU, and blood samples were collected at 0, 1, 2, 4, and 6 hr after BU administration. Plasma concentration of BU was 1094 ng/mL, and then oral BU was then adjusted to 80% of the standard hematopoietic stem cell transplantation (HSCT) dose of 1 mg/kg BU every 6 hr for 4 days; this was based on the pharmacokinetic analysis to achieve a BU steady-state concentration of 850 ng/mL ± 5% [17].…”

Section: Case Reportmentioning

confidence: 99%

Conditioning with targeted busulfan for autologous peripheral blood stem cells transplantation for acute myelogenous leukemia in an XYY male

et al. 2004

View full text Add to dashboard Cite

We report herein a 19-year-old Japanese male with XYY syndrome who developed acute myelogenous leukemia. During three courses of cytotoxic chemotherapy, he suffered repeated hepatic and renal insufficiencies, possibly related to latent dysfunction from the XYY syndrome. The patient was treated with granulocyte colony-stimulating factor combined with etoposide, cytarabine, and busulfan (the latter adjusted to a targeting dose) followed by autologous peripheral blood stem cell transplantation. He had no severe regimen-related toxicities and is now free of leukemia. Am.

show abstract

High-Performance Liquid Chromatographic Quantification of Busulfan in Human Serum after Fluorescence Derivatization by 2-Naphthalenethiol

Cited by 11 publications

References 23 publications

Otimização de método analítico em HPLC-PDA para monitoração terapêutica do bussulfano oral em pacientes transplantados de células-tronco hematopoiéticas

Otimização de método analítico em HPLC-PDA para monitoração terapêutica do bussulfano oral em pacientes transplantados de células-tronco hematopoiéticas

Comparison of LC-MS Assay and HPLC Assay of Busulfan in Clinical Pharmacokinetics Studies

Conditioning with targeted busulfan for autologous peripheral blood stem cells transplantation for acute myelogenous leukemia in an XYY male

Contact Info

Product

Resources

About