Journal of Pharmaceutical Analysis

JPA Prize in 2014

2015, 5(4)

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Abstract:

Application of analytical instruments in pharmaceutical analysis

2015, 5(4): Ⅰ-Ⅳ.

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Abstract:

Quantitative bioanalytical and analytical method development of dibenzazepine derivative, carbamazepine: A review☆

Prasanna A. Datar

2015, 5(4): 213-222. doi: 10.1016/j.jpha.2015.02.005

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Abstract:
Bioanalytical methods are widely used for quantitative estimation of drugs and their metabolites in physiological matrices. These methods could be applied to studies in areas of human clinical pharma-cology and toxicology. The major bioanalytical services are method development, method validation and sample analysis (method application). Various methods such as GC, LC-MS/MS, HPLC, HPTLC, micellar electrokinetic chromatography, and UFLC have been used in laboratories for the qualitative and quan-titative analysis of carbamazepine in biological samples throughout all phases of clinical research and quality control. The article incorporates various reported methods developed to help analysts in choosing crucial parameters for new method development of carbamazepine and its derivatives and also enu-merates metabolites, and impurities reported so far.

Development and validation of a GC-FID method for quantitative analysis of oleic acid and related fatty acids☆

Honggen Zhang, Zhenyu Wang, Oscar Liu

2015, 5(4): 223-230. doi: 10.1016/j.jpha.2015.01.005

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Abstract:
Oleic acid is a common pharmaceutical excipient that has been widely used in various dosage forms. Gas chromatography (GC) has often been used as the quantitation method for fatty acids normally requiring a derivatization step. The aim of this study was to develop a simple, robust, and derivatization-free GC method that is suitable for routine analysis of all the major components in oleic acid USP-NF (United States Pharmacopeia-National Formulary) material. A gas chromatography-flame ionization detection (GC-FID) method was developed for direct quantitative analysis of oleic acid and related fatty acids in oleic acid USP-NF material. Fifteen fatty acids were separated using a DB-FFAP (nitroterephthalic acid modified polyethylene glycol) capillary GC column (30 m × 0.32 mm i.d.) with a total run time of 20 min. The method was validated in terms of specificity, linearity, precision, accuracy, sensitivity, and robustness. The method can be routinely used for the purpose of oleic acid USP-NF material analysis.

Fabrication of multiwalled carbon nanotube-surfactant modified sensor for the direct determination of toxic drug 4-aminoantipyrine☆

Jayant I. Gowda, Arunkumar T. Buddanavar, Sharanappa T. Nandibewoor

2015, 5(4): 231-238. doi: 10.1016/j.jpha.2015.01.001

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A multi-walled carbon nanotube (MWCNT)-cetyltrimethylammonium bromide (CTAB) surfactant composite modified glassy carbon electrode (GCE) was developed as a novel system for the determination of 4-aminoantipyrine(AAP). The oxidation process was irreversible over the pH range studied and exhibited a diffusion controlled behavior. All experimental parameters were optimized. The combination of MWCNT-CTAB endows the biosensor with large surface area, good biological compatibility, electricity and stability, high selectivity and sensitivity. MWCNT-CTAB /GCE electrode gave a linear response for AAP from 5.0 × 10-9 to 4.0 × 10-8 M with a detection limit of 1.63 × 10-10 M. The modified electrode showed good selectivity against interfering species and also exhibited good reproducibility. The present electrochemical sensor based on the MWCNT-CTAB/GCE electrode was applied to the determination of AAP in real samples.

Simultaneous determination of four Sudan dyes in rat blood by UFLC-MS/MS and its application to a pharmacokinetic study in rats☆

Hao Zhu, Yijun Chen, Changshun Huanga, Yangyang Han, Yiwei Zhang, Shucan Xie

2015, 5(4): 239-248. doi: 10.1016/j.jpha.2015.03.001

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A rapid and sensitive method based on ultrafast liquid chromatography-tandem mass spectrometry was developed and validated for simultaneous determination of Sudan Ⅰ, Sudan Ⅱ, Sudan Ⅲ, and Sudan Ⅳ levels in rat whole blood. Cleanert C18 mixed-mode polymeric sorbent was used for effective solid-phase extraction cleanup. Separation was carried out on a reversed-phase C18 column (100 mm × 2.1 mm, 1.8 μm) using 0.1% (v/v) formic acid in water/0.1% (v/v) formic acid in acetonitrile as the mobile phase in gradient elution. Quantification was performed by an electrospray ionization source in the positive multiple reaction monitoring mode using D5-Sudan I as the internal standard. Calibration curves showed good linearity between 0.2 and 20.0 μg/L, with correlation coefficients higher than 0.9990. The average recovery rates were between 93.05% and 114.98%. The intra- and inter-day relative standard deviations were within 6.2%. The lower limit of quantification was 0.2 μg/L. All the analytes were found to be stable in aseries of stability studies. The proposed method was successfully applied to a pharmacokinetic study of four Sudan dyes after oral administration to rats.

Multi-spectroscopic investigation of the binding interaction of fosfomycin with bovine serum albumin☆

Manjunath D. Meti, Sharanappa T. Nandibewoor, Shrinivas D. Joshi, Uttam A. More, Shivamurti A. Chimatadar

2015, 5(4): 249-255. doi: 10.1016/j.jpha.2015.01.004

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Abstract:
The interaction between fosfomycin (FOS) and bovine serum albumin (BSA) has been investigated effectively by multi-spectroscopic techniques under physiological pH 7.4. FOS quenched the intrinsic fluorescence of BSA via static quenching. The number of binding sites n and observed binding constant KA were measured by the fluorescence quenching method. The thermodynamic parameters △G0, △H0 and △S0 were calculated at different temperatures according to the van't Hoff equation. The site of binding of FOS in the protein was proposed to be Sudlow's site I based on displacement experiments using site markers viz. warfarin, ibuprofen and digitoxin. The distance r between the donor (BSA) and acceptor (FOS) molecules was obtained according to the F?rster theory. The effect of FOS on the conformation of BSA was analyzed using synchronous fluorescence spectra (SFS), circular dichroism (CD) and 3D fluorescence spectra. A molecular modeling study further confirmed the binding mode obtained by the experimental studies.

Identification, synthesis and characterization of process related impurities of benidipine hydrochloride, stress-testing/stability studies and HPLC/UPLC method validations☆

Esen Bellur Atici, Bekir Karli?a

2015, 5(4): 256-268. doi: 10.1016/j.jpha.2015.02.001

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Abstract:
Benidipine hydrochloride, used as an antihypertensive agent and long-acting calcium antagonist, is synthesized for commercial use as a drug substance in highly pure form. During the synthetic process development studies of benidipine, process related impurities were detected. These impurities were identified, synthesized and characterized and mechanisms of their formation were discussed in detail. After all standardization procedures, they were used as reference standards for analytical studies. In addition, a separate HPLC method was developed and validated for detection of residual 1-benzylpi-peridin-3-ol (Ben-2), which is used during benidipine synthesis and controlled as a potential process related impurity. As complementary of this work, stress-testing studies of benidipine were carried out under specified conditions and a stability-indicating UPLC assay method was developed, validated and used during stability studies of benidipine.

Simultaneous quantitation of folic acid and 5-methyltetrahydrofolic acid in human plasma by HPLC-MS/MS and its application to a pharmacokinetic study☆

Xiao-Hong Zheng, Li-Yuan Jiang, Lan-Ting Zhao, Quan-Ying Zhang, Li Ding

2015, 5(4): 269-275. doi: 10.1016/j.jpha.2015.05.004

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Abstract:
A sensitive method based on high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed for the simultaneous determination of folic acid (FA) and its active metabolite, 5-methyltetrahydrofolic acid (5-M-THF), in human plasma. The analytes were extracted from plasma with methanol solution containing 10 mg/mL of 2-mercaptoethanol and 0.025% (v/v) ammonium hydroxide. FA and 5-M-THF were more stable after the addition of 2-mercaptoethanol and ammonium hydroxide in the sample preparation procedures of this study than they were in the previously published methods. Chromatographic separation was performed on a Hedera ODS-2 column using a gradient elution system of acetonitrile and 1 mM ammonium acetate buffer solution containing 0.6% formic acid as mobile phase. LC-MS/MS was carried out with an ESI ion-source and operated in the multiple reaction monitoring (MRM) mode. The assay was linear over the concentration ranges of 0.249-19.9 ng/mL for FA, and 5.05-50.5 ng/mL for 5-M-THF. The developed LC-MS/MS method offers increased sensitivity for quantification of FA and 5-M-THF in human plasma and was applicable to a pharmacokinetic study of FA and 5-M-THF.

2015 Vol. 5, No. 4