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A validated ultraperformance liquid chromatography-tandem mass spectrometry (UPLC–MS/MS) method was developed for the first-ever simultaneous analysis of neratinib, curcumin and internal standard (imatinib) using acetonitrile as the liquid–liquid extraction medium. On a BEH C18 (100 mm × 2.1 mm, 1.7 μm) column, the analytes were separated isocratically using acetonitrile (0.1% formic acid):0.002M ammonium acetate. The flow rate was set at 0.5 mL.min−1. The authors utilized multiple reaction monitoring-based transitions for the precursor-to-product ion with m / z 557.099 → 111.928 for neratinib, m / z 369.231 → 176.969 curcumin and m / z 494.526 → 394.141 for imatinib during the study. Validation of the method as per United States Food and Drug Administration requirements for linearity (5–40 ng mL−1), accuracy and precision, stability, matrix effect, etc. were investigated and were observed to be acceptable. Afterward, we evaluated the method for establishing its greenness profile by using two greenness assessment tools and found it green. Overall, a reliable green UPLC–MS/MS method was devised and used to estimate neratinib and curcumin in human plasma simultaneously. [ABSTRACT FROM AUTHOR]

For the quantification of resveratrol (RV) in the Wistar rat skin, an ultra-performance liquid chromatography-mass spectrometric (UPLC–MS/MS) method was developed and validated on ACQUITY UPLC BEH C18 column (1.7 μm). The mobile phase ratio of methanol (A) and 2% formic acid (B) (ratio 10: 90% v/v, 80: 20 v/v) at isocratic elution with flow rate 0.3 mL/min, and run time 3 min was used for analysis. In addition, the use of multiple reaction monitoring (MRM)/ES+ mode to detect the analytes and to track parents to daughter ion transition of 229.17 > 107.04 m/z (time scan 3 min, retention time 1.48) for RV and curcumin as an internal standard shows 369.16 > 176.93m/z (scan time is 2.80 min, retention time is 1.11), respectively. Linearity was observed in the range of 2.5 to 2,000 ng/mL (R2 = 0.987). Precision and accuracy on rat skin were within the acceptability range (RE%: ±15; RSD%: ±15). Moreover, it showed a good percentage recovery and found within acceptance limit 90–110%. Lower limit of detection and quantitation for the method observed to be 2.5 and 20 ng.mL−1, respectively. Method application indicated successful determination of dermatokinetics parameters of RV from lipospheres gel and suspension in the rats. [ABSTRACT FROM AUTHOR]

A chemometrics-oriented green ultra-performance liquid chromatography-mass spectrometry/mass spectrometry method was developed and validated for the first-time simultaneous estimation of capecitabine (CAP) and lapatinib (LPB) along with imatinib (as internal standard (IS)) in rat plasma. Analytes were extracted using ethyl acetate as the liquid–liquid extraction media. In the pre-development phase, principles of analytical eco-scale were used to confirm method greenness. Subsequently, vital method variables, influencing method robustness and performance, were optimized using a chemometrics-based quality-by-design approach. Chromatography was achieved on a BEH C18 (100 × 2.1 mm, 1.7 μm) using isocratic flow (0.5 mL.min −1 ) of mobile phase acetonitrile (0.1% formic acid):0.002 M ammonium acetate in water as the mobile phase. The mass spectrometric detections were carried out in multiple reaction monitoring modes with precursor-to-product ion transitions with m/z 360.037 → 244.076 for CAP, m/z 581.431 → 365.047 LPB and m/z 494.526 → 394.141 for IS. The bioanalytical method validation studies were performed, ensuring regulatory compliance. Linearity (r 2 > 0.99) over analyte concentrations ranging from 5 and 40 ng.mL −1 was observed, while acceptable values were obtained for all other validation parameters. In a nutshell, a robust and green bioanalytical method was developed and applied for the simultaneous estimation of two anticancer agents from rat plasma. [ABSTRACT FROM AUTHOR]

Neratinib, a tyrosine kinase inhibitor, was very recently approved by USFDA in 2017 as an anticancer drug to treat of HER2 positive breast cancers. The present work provides an account on the development of a validated bioanalytical UPLC–MS/MS method for quantification of neratinib and internal standard (imatinib) in rat plasma and tissue homogenates. A UPLC having a 100 mm C18 column (1.7 μm sized particles) was used with acetonitrile (0.1% formic acid): 2 mMol of ammonium acetate in water (pH 3.5) as the mobile phase. An efficient chromatographic separation was performed and detection was achieved by monitoring precursor-to-product ion transitions with m/z 557.29 → 112.06 for neratinib and m/z 494.43 → 294.17 for IS. The method demonstrated excellent linearity in the spiked plasma drug concentrating ranging between 1 and 800 ng.mL−1 (r2 = 0999), with lower limit of quantification (LLOQ) was observed at 1 ng.mL−1. Intra-assay and inter-assay precision relative standard deviations were found to be within 6.58. Mean extraction recovery for neratinib and IS were 99.44 and 99.33%, while matrix effect for neratinib and IS was ranging between −4.35 and − 3.66%, respectively. Overall, the method showed successful applicability in pharmacokinetic analysis of pure various formulations in Wistar rat plasma. [ABSTRACT FROM AUTHOR]

Borage oil that is extracted from (Borago officinalis Linn.) is a well-known medicinal plant having various medicinal benefits. In this work, an affordable, simple, reliable, rapid and easily accessible high-performance thin-layer chromatography (HPTLC) method was developed for the estimation of gamma-linolenic acid (GLA) in borage oil. HPTLC method employs thin-layer chromatography (TLC) aluminum plates precoated with silica gel (G60F254) as the stationary phase, and the mixture of hexane:toulene:glacial acetic acid (3:7:1, v/v/v) was used as the mobile phase. Densitometric analysis of the TLC plates was carried out at 200 nm. The developed method showed well-resolved spots with retention factor (R f) value of 0.53 ± 0.04 for GLA. Various experimental conditions like saturation time for chamber, solvent phase migration and width of the band were studied intensely for selecting the optimum conditions. The method validation was performed for parameters like linearity, accuracy, specificity and precision. The values of limit of detection and limit of quantification for GLA were found to be 0.221 and 0.737 μg/band, respectively. In nutshell, the developed HPTLC method was found to be highly sensitive for the estimation of GLA in the herbal oil samples and formulations. [ABSTRACT FROM AUTHOR]

The present study described the development of a reversed-phase liquid chromatographic method for the estimation of abiraterone acetate by Quality by Design (QbD) approach. Using an isocratic solvent system for the mobile phase, the chromatographic estimation of analyte was performed on a Hypersil BDS C18 column using mobile phase mixture containing acetonitrile and water with pH adjusted with 0.1% v/v orthophosphoric acid (15:85%v/v ratio), flow rate 1.0 mL.min−1 and detection at 250 nm using photodiode array detector. Systematic development of the chromatographic method was carried out by factor screening using a half-factorial design which suggested organic modifier (%), flow rate (mL.min−1) and autosampler temperature (°C) as influential variables. Further, the method was optimized by Box–Behnken design and trials performed were evaluated for the area under peak, retention time, theoretical plate count and tailing factor as the responses. Validation of the developed method showed good linearity, accuracy, precision and sensitivity. Evaluation of the stability-indicating profile of the method using forced degradation studies revealed the formation of a possible degradation product under acidic and alkaline conditions, while no such degradation product peaks were observed under the oxidative environment. Overall, the study construed the successful development of HPLC assay method for pharmaceutical applications. [ABSTRACT FROM AUTHOR]

Borage oil that is extracted from (Borago officinalis Linn.) is a well-known medicinal plant having various medicinal benefits. In this work, an affordable, simple, reliable, rapid and easily accessible high-performance thin-layer chromatography (HPTLC) method was developed for the estimation of gamma-linolenic acid (GLA) in borage oil. HPTLC method employs thin-layer chromatography (TLC) aluminum plates precoated with silica gel (G60F254) as the stationary phase, and the mixture of hexane:toulene:glacial acetic acid (3:7:1, v/v/v) was used as the mobile phase. Densitometric analysis of the TLC plates was carried out at 200 nm. The developed method showed well-resolved spots with retention factor (Rf) value of 0.53 ± 0.04 for GLA. Various experimental conditions like saturation time for chamber, solvent phase migration and width of the band were studied intensely for selecting the optimum conditions. The method validation was performed for parameters like linearity, accuracy, specificity and precision. The values of limit of detection and limit of quantification for GLA were found to be 0.221 and 0.737 μg/band, respectively. In nutshell, the developed HPTLC method was found to be highly sensitive for the estimation of GLA in the herbal oil samples and formulations., (© The Author(s) 2021. Published by Oxford University Press. All rights reserved. For permissions, please email: journals.permissions@oup.com.)