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A sensitive, heart-cutting, two-dimensional liquid chromatography–tandem mass spectrometry method for the determination of mometasone furoate in human plasma: Application for a bioequivalence study in nasal spray formulations

Yang Leting, Yang Hongyi, Xie Huiru, Liu Hui, He Gangmin, Zhong Wenjing, Wang Ling

Acta Chromatographica

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2024

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Vol. 36, no. 1

14--22

EN

We developed and validated a sensitive, heart-cutting, two-dimensional liquid chromatography–tandem mass spectrometry (2D-LC‒MS/MS) method to determine the concentration of mometasone furoate in human plasma after nasal spray administration. Isotopically labeled mometasone furoate-13¹³C,d₆ was used as an internal standard (IS). Plasma samples were prepared using a solid-phase extraction (SPE) method. With this 2D-LC strategy, the analytes were trapped in the first dimension (1D) column, and only judiciously selected portions of the 1D effluent were transferred to the second dimension (2D) column for further separation to obtain high-resolution information. MS/MS quantification was performed in positive ionization mode via multiple-reaction monitoring (MRM). This analytical method was fully validated according to related regulatory guidance, and the results showed that the method is robust and sensitive enough for pharmacokinetic investigation of mometasone furoate with satisfactory linearity from 0.25 to 30 pg mL⁻¹. This method was successfully applied to a bioequivalence (BE) study of mometasone furoate aqueous nasal sprays in healthy volunteers.

2

Development and validation of a rapid and sensitive LC-MS/MS method for the determination of aripiprazole in human plasma: Application to a bioequivalence study

Patel D. S., Sharma N., Patel M. C., Patel B. N., Shrivastav P. S., Sanyal M.

Acta Chromatographica

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2014

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Vol. 26, no. 2

203--227

EN

A rapid, selective, and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay has been proposed for the determination of aripiprazole in human plasma. The analyte and propranolol as internal standard (IS) were extracted from 200 μL of human plasma via liquid-liquid extraction using methyl tert-butyl ether under alkaline conditions. The best chromatographic separation was achieved on an Aquasil C18 (100 × 2.1 mm, 5 μm) column using methanol-deionized water containing 2 mM ammonium trifluoroacetate and 0.02% formic acid (65:35, v/v) as the mobile phase under isocratic conditions. Detection of analyte and IS was done by tandem mass spectrometry, operating in positive ion and multiple reaction monitoring (MRM) acquisition mode. The method was fully validated for its selectivity, interference check, sensitivity, carryover check, linearity, precision and accuracy, reinjection reproducibility, recovery, matrix effect, ion suppression/enhancement, stability, ruggedness, and dilution integrity. The assay was linear over the concentration range of 0.10–100 ng mL -1 for aripiprazole. The intra-batch and inter-batch precision (%CV) was ≤4.8%, while the mean extraction recovery was >96% for aripiprazole across quality control levels. The method was successfully applied to a bioequivalence study of 10 mg aripiprazole orally disintegrating tablet formulation in 27 healthy Indian subjects under fasting and fed condition. The reproducibility in the measurement of study data was demonstrated by reanalysis of 260 incurred samples.

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Development and validation of a sensitive LC-MS/MS method for determination of valacyclovir in human plasma: Application to a bioequivalence study

Konda R. K., Chandu B. R., Challa B. R., Chandrasekhar K. B.

Acta Chromatographica

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2013

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Vol. 25, no. 4

669--686

EN

A simple, sensitive, and highly specific method has been developed for determination of valacyclovir (VL) in human plasma. The analytical procedure involves a solid-phase extraction method using Valacyclovir-D8 (VLD8) as an internal standard. Chromatographic separation was carried out on a reversed phase Zorbax, SB C18, 4.6 × 75 mm, 3.5μm column. Valacyclovir and Valacyclovir-D8 were detected with proton adducts at m/z 325.2 → 152.0 and 333.3 → 152.0 in multiple reaction monitoring (MRM) positive mode. The method was linear over the concentration range of 0.5–700.0 ng mL -1. The limit of detection (LOD) and limit of quantification (LOQ) for valacyclovir were 0.2 pg mL -1 and 0.5 ng mL -1, respectively. The method was shown to be precise with the average within-run and between-run variations of 0.7 to 3.5% and 3.1 to 4.7%, respectively. The average within-run and between-run accuracies of the method throughout its linear range were 96.7 to 97.9 and 94.7 to 97.3%, respectively. The mean recoveries of valacyclovir and Valacyclovir-D8 from human plasma by the developed method were 99.17 ± 10.78% and 110.84 ± 8.74%, respectively. The method was successfully applied in bioequivalence study with 20 healthy male volunteers under fasting condition.

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Znowelizowana wytyczna European Medicines Agency na temat badań równoważności biologicznej

Bogiel M.

Chemik

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2011

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Vol. 65, nr 2

115-120

PL

1 sierpnia 2010 r. weszła w życie znowelizowana wytyczna EMA dotycząca badań równoważności biologicznej produktów leczniczych – Guideline on the investigation of bioequivalence. Zastąpiła ona obowiązującą od 2002 r. wytyczną: Note for guidance on the investigation of bioavailability and bioequivalence. Wejście w życie znowelizowanej wytycznej jest ważnym i szeroko komentowanym wydarzeniem dla przemysłu farmaceutycznego, jak i dla osób i instytucji zaangażowanych w prace nad badaniami równoważności biologicznej. Najbardziej istotne zmiany w znowelizowanej wersji wytycznej dotyczą modelu badania (m.in. wprowadzenie tzw. twostage design), zasadności wyboru oznaczanej substancji (metabolity, enancjomery), kryteriów akceptacji statystycznej dla uznania równoważności oraz warunków odstąpienia od badań in vivo (biowaivers, bracketing approach). Zostały one omówione w artykule.

EN

An amended EMA Guideline on the investigation of bioequivalence of medicinal products became effective on the 1st of August 2010. It replaced a previous one, effective since 2002: Note for guidance on the investigation of bioavailability and bioequivalence. The coming into force of the revised guideline was an important and widely discussed event for the pharmaceutical industry, as well as for the people and institutions engaged in the work on the investigation of bioequivalence. The most significant changes in the amended guideline pertain to the model of studies (introduction of the so-called two-stage design, among others), justification of the selection of the substance determined (metabolites, enantiomers), criteria of statistical acceptance of bioequivalence and conditions for exempting in vivo studies (biowaivers, bracketing approach). These are discussed in the paper.

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An LC-MS/MS-ESI method for the quantification of betamethasone in bioequivalence studies

Teixeira L. S, Mundim I. M, Souza W. C, Ramos D. R, Bellorio K. B, Rezende K. R

Acta Chromatographica

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2011

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Vol. 23, no. 3

415--428

EN

A simple, sensitive, and rapid liquid chromatography-mass detection (LC-MS/MS) method for the analysis of betamethasone (BET) from intramuscular injection of phosphate and dipropionate BET produgs was developed for bioequivalence studies in human plasma. The calibration curve was linear over the range of concentrations (0.5–50.0 ng mL-1; r2 = 0.99), showing a very high sensitivity without interferences at the retention times of BET (0.8 min) and the internal standard (IS) triamcinolone acetonide (0.95 min). Both drug (D) and IS were extracted from human plasma by liquid-liquid extraction, showing average recovery values of 94.0 and 98.9%, respectively. Within- and between-run precision studies demonstrated a variation coefficient <10% at all tested concentrations. Therefore, our analytical method proved to be validated according to the worldwide-accepted FDA guidelines and successfully applied for bioequivalence studies of parenteral formulations containing BET dipropionate (5 mg mL−1) and BET sodium phosphate (2 mg mL-1).

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Analysis of lovastatin in human plasma by liquid chromatography coupled with tandem mass spectrometry

Yu X. R., Song M., Hang T. J., Wen A. D.

Acta Chromatographica

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2008

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Vol. 20, no. 3

399-410

EN

A sensitive and selective liquid chromatographic tandem mass spectrometric (LC-MS-MS) method for analysis of lovastatin in human plasma has been developed and validated. Ethyl acetate extraction was used for plasma sample preparation and simvastatin was used as internal standard. Chromatographic separation was achieved on a C 18 column by isocratic elution with 83:17:0.1 ( v/v ) methanol-2 µM aqueous sodium acetate-formic acid as mobile phase, delivered at 1.0 mL min -1. MS-MS detection was performed using positive electrospray ionization and multiple-reaction monitoring with argon for collision-induced dissociation. Calibration plots were generated over the concentration range 0.05 to 20 ng mL -1 (r > 0.999) with a lower limit of quantification (LLOQ) of 0.05 ng mL -1. Intra and inter-day precision and accuracy were determined at four different concentrations, 0.05, 0.5, 2.0, and 10.0 ng mL -1, and precision ranged from 0.4 to 11.4% with the deviation always less than 15% ( n = 5). Extraction recoveries were from 86.8 to 94.1% for lovastatin and approximately 88.0% for simvastatin. The validated method was successfully applied to a bioequivalence study of two lovastatin tablets in 20 healthy volunteers.

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Badania równoważności biologicznej odtwórczych preparatów farmaceutycznych

Kobylińska K.

Przemysł Chemiczny

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2002

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T. 81, nr 5

311-313