Original Article
STABILITY INDICATING LC–ESI-MS/MS METHOD DEVELOPMENT AND VALIDATION FOR THE
QUANTITATION OF LURBINECTEDIN IN BIOLOGICAL MATRICES
MANTRAVADI ANUSHA, RAMREDDY GODELA
*
, KUMAR SHIVA GUBBIYAPPA
Department of Pharmaceutical Analysis, GITAM School of Pharmacy, GITAM Deemed to be Univeristy, Rudraram, Patancheru, Telangana,
India
*
Corresponding author: Ramreddy Godela;
*
Email: rgodela@gitam.edu
Received: 24 Dec 2024, Revised and Accepted: 11 Jun 2025
ABSTRACT
Objective: A new and validated liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and used for the
quantitative analysis of the anticancer drug Lurbinectedin in plasma samples.
Methods: Liquid-liquid extraction method was used to extract the Lurbinectedin from plasma, and Ledipasvir was used as an internal standard (IS),
Chromatographic separation of Lurbinectedin was accomplished with Zorbax SB-C18 column (250 mm×4.6 mm, 5 μm) using a mobile phase
comprises of 0.1% v/v formic acid and acetonitrile (10:90, v/v) pumped at a flow rate of 0.80 ml/min. The total run time for Lurbinectedin and
internal standard elution was 3.5 min. The linearity was attained for a concentration range of 1.50–5000 ng/ml with a correlation coefficient (r²) of
0.9994 by the optimized method. The lower limit of quantification (LLOQ) was established at 1.50 ng/ml, which resembles the sensitivity of the
method toward Lurbinectedin.
Results: The method showed high accuracy, ranging from 95.31% to 104.06% of nominal values, with intra-and inter-day precision within a 4.32%
coefficient of variance (%CV). Matrix effects at the low-quality control (LQC) level varied between 94.25% and 104.85% (%CV: 4.61), while at the
high-quality control (HQC) level, they ranged from 94.62% to 103.88% (%CV: 4.02). The mean recovery across all control standards was 95.58%.
Conclusion: Stability assessments confirmed the robustness of the method. The developed LC-MS/MS approach is reliable for routine bioanalytical
applications, including quality control, pharmacokinetic studies, and bioequivalence assessments of Lurbinectedin in biological matrices.
Keywords: Lurbinectedin, LC-ESI-MS/MS, Bioanalytical method, Precision, Sensitivity, Zorbax SB-C18 column
© 2025 The Authors. Published by Innovare Academic Sciences Pvt Ltd. This is an open access article under the CC BY license (https://creativecommons.org/licenses/by/4.0/)
DOI: https://dx.doi.org/10.22159/ijap.2025v17i5.53562 Journal homepage: https://innovareacademics.in/journals/index.php/ijap
INTRODUCTION
A DNA alkylating medication known as Lurbinectedin has been
investigated for potential use in treating many cancers, including
CLL (fig. 1), mesothelioma, breast cancer, and SCLC. The anticancer
chemical Ecteinascidin (trabectedin) is derived from the marine
tunicate Ecteinascidia turbinata. The primary change is that
Lurbinectedin is more effective against tumors than trabectedin due
to the substitution of a tetrahydro β‐carboline for
tetrahydroisoquinoline [1].
As it binds to guanine residues in the DNA's minor groove, it
generates adducts that cause the DNA helix to bend toward the
major groove. A cascade of events begins at this step, altering the
function of transcription factors and decreasing the efficacy of DNA
repair pathways. Ultimately, this leads to cell death by breaking
double-stranded DNA. It also inhibits RNA-polymerase-II activity,
nucleotide transfer inhibits EWS-FL11 protein expression, and
inhibits human monocyte activity and macrophage entrance into
tumor tissue, among other mechanisms [2].
Strong DNA attachment is the mechanism by which Lurbinectedin
exerts its chemotherapeutic action, causing DNA strand breakage
and cell death [3]. Because Lurbinectedin has been associated with
myelosuppression, patients using this medication should have
cytopenias monitored carefully. Verify that the platelet count is
more than 100,000/mm3 and the neutrophil count is greater than
1,500 cells/mm3 prior to beginning therapy. If the neutrophil count
falls below 500 cells/mm3, it may be prudent to consider
administering granulocyte colony-stimulating factor (G-CSF).
Lurbinectedin has also been associated with liver damage. During
and after therapy, it is important to monitor liver function tests.
Delaying, reducing, or discontinuing treatment entirely may be
necessary depending on the severity of the hepatotoxicity [4-6].
There are just two published protocols on LCMS/MS in the literature
on Lurbinectedin [7, 8]. Nicholas et al. developed a method having a
calibration curves displayed good linearity over 0.1 to 50 ng/ml for
lurbinectedin and 0.5 to 20 ng/ml for the metabolites. This method has
poor recovery results with a 12.9% error [7]. Andel et al. developed a
method having linearity up to 100 ng/ml [8]. The method was linear
over 0.1–100 ng/ml and 1–1000 ng/ml in plasma and urine,
respectively, with accuracies and precisions within ±15% (20% for
LLOQ) and below 15% (20% for LLOQ), respectively. The fields of
pharmacodynamics, forensics, and pharmacokinetics studies require
specific methods with good recovery values. Hence, there is a need for
an LC-MS/MS approach to studying human K2 EDTA plasma.
Fig. 1: Chemical structure of lurbinectedin
MATERIALS AND METHODS
Reagent chemicals
Hetero Pharmaceuticals of Hyderabad, India, supplied the Ledipasvir
(with a purity level of 99.52 percent). The drug Lurbinectedin was
sourced from Selleck Chemicals in Houston, Texas, USA. Plasma from
the Vivekananda Blood Bank in Hyderabad, India, which is devoid of
drugs and contains the anticoagulant K2-EDTA, was obtained. The
International Journal of Applied Pharmaceutics
ISSN- 0975-7058 Vol 17, Issue 5, 2025