An analytical “quality by design” approach in RP-HPLC method development and validation for reliable and rapid estimation of irinotecan in an injectable formulation

Bhaskaran, Navya Ajitkumar; Kumar, Lalit; Reddy, M. Sreenivasa; Pai, Girish K

doi:10.2478/acph-2021-0008

Cited by 37 publications

(21 citation statements)

References 23 publications

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“…For estimating the limits of detection and quantification, the method reported by Bhaskaran et al [ 46 ] was used based on equations: LOD = 3.3 σ/s and LOQ = 10 σ/s, where, σ is SD of y-intercepts of the regression line and s is the slope of the calibration line. LODs were reported to be 0.075 and 0.134, while LOQs were calculated to be 0.248 and 0.448 µg/mL for both XIP and VAL, respectively (Table 7 ) showing that the proposed method is highly sensitive and being applicable for future bioequivalence studies where it is mandatory to detect small drug concentrations in plasma.…”

Section: Resultsmentioning

confidence: 99%

Quality by design approach for development and validation of a RP-HPLC method for simultaneous estimation of xipamide and valsartan in human plasma

et al. 2022

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A new rapid, simple, and sensitive RP-HPLC method was carried out through applying Quality by Design approach for determination of xipamide and valsartan in Human plasma. Fractional factorial design was used for screening of four independent factors: pH, flow rate, detection wavelength, and % of MeOH. Analysis of variance (ANOVA) confirmed that flow rate and % of MeOH were only significant. Chromatographic conditions optimization was carried out through using central composite design. Method analysis was performed using BDS Hypersil C8 column (250 × 4.6 mm, 5 μm) and an isocratic mobile phase of MeOH and 0.05 M KH2PO4 buffer pH 3 (64.5:35.5, v/v) at 1.2 mL/min flow rate with UV detection at 240 nm and 10 μL injection volume. According to FDA guidelines, the method was then validated for the determination of the two drugs clinically in human plasma in respect of future pharmacokinetic and bioequivalence simulation studies. The standard curve was linear in the concentration range of 5–100 µg/mL for both drugs, with a determination coefficient (R2) of 0.999. Also, the average recoveries lied within the range from 99.89 to 100.03%. The proposed method showed good predictability and robustness.

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Section: Resultsmentioning

confidence: 99%

Quality by design approach for development and validation of a RP-HPLC method for simultaneous estimation of xipamide and valsartan in human plasma

et al. 2022

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“…The concentration at which the signal-to-noise ratio of 3:1 is produced is termed as LOD, whereas the concentration at which the signal-to-noise ratio of 10:1 is produced with less than 10% RSD ( n = 3) is termed as LOQ. The following formula was used for examining the LOD and LOQ for both the analytes: LOD = 3 . 3σ / s LOQ = 10 0.25em σ / s where σ stands for the standard deviation of y -intercepts of the regression line, and s stands for the slope obtained from the calibration curve. , …”

Section: Methodsmentioning

confidence: 99%

Rapid Analytical Method Development and Validation of RP-HPLC Method for the Simultaneous Estimation of Exemestane and Genistein with Specific Application in Lipid-Based Nanoformulations

Sharma

Gupta

et al. 2023

ACS Omega

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Exemestane (EXE), an irreversible aromatase inhibitor, is employed as a therapy for hormone-dependent breast cancer. Several studies have also established the budding effects of genistein (GEN) in various types of cancer such as breast, prostate, as well as skin due to its feeble estrogenic and anti-estrogenic properties. Considering the promising benefits of GEN, it was combined with EXE to accomplish superior therapeutic efficiency with fewer side effects. The quantification of the exact concentration of EXE and GEN when delivered as a combination would be required for which HPLC method was developed and validated. For this purpose, the C18 ODS column having dimensions of 150 × 4.6 mm, 5 μm, using mobile phase A as methanol:water (35:15, v/v), with formic acid (0.01%), and B as acetonitrile (in the ratio of A:B−−30:70 v/v) at a flow rate of 1 mL/min was commonly used. The Box− Behnken design was chosen as our experimental model, and the interactions among the independent and dependent variables were analyzed. Parameters like linearity, system suitability, specificity, precision (intra-and interday), robustness, ruggedness, LOD (limit of detection), and LOQ (limit of quantification) were selected for the validation of our proposed method. EXE and GEN were eluted individually at 245 and 270.5 nm, respectively, while both of the agents were determined simultaneously at 256 nm, showing retention time as 2.10 and 1.67 min, respectively, and the calibration plot was observed to be linear in the range of 5−110 μg/mL. Hence, the method that we developed and validated was found to be suitable for the identification of both the drugs simultaneously in combination and in our in-house-developed nanoformulation.

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“…Where 'SD a ' is the standard deviation of the y-intercept and 'm' is the slope of the calibration curve. 15,16…”

Section: Lod and Loqmentioning

confidence: 99%

Development and Validation of RP-HPLC Method for Quantification of Total, Free and Entrapped Ritonavir in Lipid Nanocarriers and Drug content of Film Coated Fixed Dose Formulation

Jitta¹,

Bhaskaran²,

Kumar³

et al. 2022

Ind. J. Pharm. Edu. Res

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Aim:The current study was aimed to develop and validate a simple isocratic, precise, sensitive, accurate and robust reverse phase HPLC analytical method for the quantification of total, free and entrapped ritonavir in lipid nanocarriers and drug content of the filmcoated fixed-dose formulation. Materials and Methods: The method was developed by using Inertsil ODS-3V C 18 column as stationary phase, orthophosphoric acid (OPA) in water (pH 3.0) and acetonitrile as mobile phase. Further, the method was validated following ICH Q2(R1) guidelines. Ritonavir loaded lipid nanocarriers were developed using hot-emulsion and probe-sonication method. A solid phase extraction (SPE) method was developed for the separation of free and entrapped ritonavir. Total ritonavir was extracted from lipid nanocarriers (LNCs) and film-coated tablets using methanol and analyzed with validated method. Results: The responses were found to be linear and precise over a range of 0.25 µg/mL to 16 µg/mL. The limit of detection (LOD) and limit of quantification (LOQ) of the RP-HPLC method were found to be 14.06 ng/mL and 42.60 ng/mL, respectively which emphasizes the sensitivity of the method. The recovery of ritonavir from LNCs was found to be within 3% of the total drug present in LNCs. Similar, amount of drug recovery was found from assay of marketed formulation i.e., > 97%. Conclusion: The SPE method is capable of separating free and entrapped ritonavir from LNCs. The developed HPLC method is sensitive, robust, economical and gives high recovery. The developed HPLC method can also be employed for routine quantitative analysis of ritonavir in bulk formulation.

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An analytical “quality by design” approach in RP-HPLC method development and validation for reliable and rapid estimation of irinotecan in an injectable formulation

Cited by 37 publications

References 23 publications

Quality by design approach for development and validation of a RP-HPLC method for simultaneous estimation of xipamide and valsartan in human plasma

Quality by design approach for development and validation of a RP-HPLC method for simultaneous estimation of xipamide and valsartan in human plasma

Rapid Analytical Method Development and Validation of RP-HPLC Method for the Simultaneous Estimation of Exemestane and Genistein with Specific Application in Lipid-Based Nanoformulations

Development and Validation of RP-HPLC Method for Quantification of Total, Free and Entrapped Ritonavir in Lipid Nanocarriers and Drug content of Film Coated Fixed Dose Formulation

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