Development and Validation of LC-MS/MS Method for the Simultaneous Determination of Quinine and Doxycycline in Pharmaceutical Formulations

Abstract

A fast, sensitive, and specific liquid chromatography-tandem mass spectrometry (LC-MS=MS) method was developed and validated for the simultaneous determination of quinine and doxycycline in pharmaceutical formulations. The LC-MS=MS method was carried out on a Sun Fire Waters C 18 column (50 mm  3.0 mm I.D.) and the mobile phase consisted of acetonitrile:0.1% formic acid (75:25, v=v), run at a flow rate of 0.45 mL=min (split 1:3). The injection volume was 10 mL for both standard and samples. The triple quadrupole mass spectrometer equipped with an electrospray source in positive mode (ESþ) was set up in multiple reaction monitoring mode (MRM), monitoring the transitions of 325.0 > 307.0 and 445.0 > 428.1, for quinine and doxycycline, respectively. The total analysis time was 2 min and the method was linear in the concentration range of 10-1500 ng=mL for both compounds. Method validation investigated parameters such as the specificity, linearity, precision, accuracy, and robustness, giving results within the acceptable range. Moreover, the proposed method was successfully applied for determination of quinine and doxycycline in nanocapsule formulations to support the quality control.

Determination of thirteen antibiotics in drug products – A new LC-MS/MS tool for screening drug product quality

“…The importance of the LC-MS/MS technique in pharmaceutical, forensic, proteomic, biological and environmental studies are well acknowledged. [26][27][28][29][30] There are reports of LC-MS/MS methods for identication and quan-tication of medicines, but most of these describe methods dealing with biological and environmental matrices 26,[28][29][30] and not meant to be used as screening tool for the quality of antimicrobial pharmaceutical products. In this regard, the LC-MS/ MS technique, which is capable of identifying and quantifying multiple chemical compounds, becomes a viable alternative.…”

Haemolysis Effect Estimation of Doxycycline Hyclate 150 mg Delay Release Tablet in Bio-analysis (Human Plasma) by Liquid Chromatography-Tandem Mass Spectrometry

“…The injection volume was 10 µL for both standard and samples. The triple quadruple mass spectrometer equipped with an electro spray source in positive mode (ES+) was set up in Multiple Reactions Monitoring mode (MRM), monitoring the transitions of 325.0>307.0 and 445.0>428.1, for quinine and Doxycycline, respectively [4].…”

Delapril and Manidipine Measurements by Liquid Chromatography—Tandem Mass Spectrometry in a Pharmaceutical Formulation

“…Moreover, as a consequence of the mass selectivity, it was expected that the time for method development and sample turnover could be significantly reduced. [16][17][18][19] the fixed oral combination of DEL and MAN is commercially available, but, at present, there is no published Lc-MS/MS method for the quantitative analysis of the drugs in the finished product. thus, the aim of the present study was to develop and validate a specific and sensitive high-throughput Lc-MS/MS method for the simultaneous determination of DEL and MAN in solid pharmaceutical dosage forms, establishing a comparison with a validated Lc-uV and micellar electrokinetic chromatography (MEKc) 20 methods and contributing to the research of advantageous alternative techniques for the Qc of pharmaceutical formulations.…”