Journal of Pharmacetical and Cosmetic Control

Development of a method for simultaneous quantification of five phosphodiesterase type 5 (PDE-5) in postmortem blood samples by liquid chromatography tandem mass spectrometry

2025-04-11T10:16:10+00:00

This study developed a method for the simultaneous qualitative and quantitative analysis of five selective phosphodiesterase type 5 (PDE-5) inhibitors, including sildenafil, tadalafil, vardenafil, avanafil, and thiosildenafil, in postmortem blood samples using liquid chromatography-mass spectrometry (LC-MS/MS). This method is developed based on current FDA guidelines. Results: Isotopes Warfarin-d5 was used as internal standard. The procedure for samples treatment was simple with the value of recovery being higher than 85 % and repeatability being lower than 15.0 %. The experimental results showed that the limit of detection (LOD) of the analytes ranged from 0.02 to 0.03 ng/mL. The linearity of the method was in the range of 1 ng/mL to 250 ng/mL with a good correlation coefficient (R2) from 0.9989 to 0.9993.

Validating the procedure for detecting Mycoplasma in culture of cell lines at the National Institute of Drug Quality Control using the MycoAlert™ PLUS kit.

2025-04-11T10:35:34+00:00

Validation of the MycoAlert™ PLUS kit for detecting Mycoplasma contamination in Vero 76 and L929 cell cultures was conducted at the National Institute of Drug Quality Control. The study assessed system suitability, specificity, and repeatability of the method, demonstrating its effectiveness in detecting Mycoplasma in these cell lines. Results confirmed the kit’s reliability and suitability for routine monitoring of cell cultures. These findings support the integration of the MycoAlert™ PLUS kit into quality control protocols, ensuring contamination-free cell culture processes.

Determination of coumatetralyl and bromadiolone in human blood by liquid chromatography mass spectrometry

2025-04-11T10:42:29+00:00

In this study, a specific, sensitive and reliable liquid chromatography tandem mass spectrometry (LC-MS/MS) has been established for the simultaneous quantification of coumatetralyl and bromadiolone in whole blood. The method involves a liquid-liquid extraction with ethyl acetate. Multiple-reaction monitoring (MRM) was used for the monitoring of negative ions for the detection of analysed compounds. Warfarin-d5 was used as an internal standard (IS). Linearity was observed for each analyte in blood ranging from 0.5 to 100 ng/mL, with correlation coefficients over 0.99 . The limit of detection (LOD) was 0.04 ng/mL for coumatetralyl and 0.05 ng/mL for bromadiolone. The intra-day and inter-day precision values were < 15 %, and accuracies ranged from 83.4 % to 109.0 %. This method was applied to analyze twenty whole blood samples of twenty people who were suspected of having been poisoned by these compounds.

Development and validation a LC-MS/MS method for simultaneous quantitation of amlodipin, perindopril and its active metabolite perindoprilat in human plasma

2025-04-11T10:51:32+00:00

A fast, simple, high throughput and specific method using ultra performance liquid chromatography tandem mass spectrometry was developed for simultaneous quantitation of amlodipine, perindopril and its active metabolite perindoprilat in human plasma. The Sciex Qtrap 6500+ UHPLCMS/MS was operated under the multi reaction-monitoring (MRM) mode using positive electrospray ionization technique. Amlodipine, perindopril, perindoprilat and internal standards were extracted from human plasma by protein precipitation technique using methanol. The samples were chromatographed on a C18 column (dimention 50 x 2,1 mm, particle 1,9 μm) with a gradient elution at a flow rate of 0.3 ml/min using 0.1 % formic acid in water – methanol. The calibration curves were found to be linear in the range 0.15 to 15 ng/ml, 1.25 to 125 ng/ml and 0.2 to 20 ng/ml for amlodipine, perindopril and perindoprilat, respectively, with mean correlation coefficient of > 0.99 for all analysis. The accuracy was within 85 % - 115.0 % and the precision was less than 15 %. Total run time was 4.5 min. This method can be used for BA-BE studies of amlodipine and perindopril combination preparations.

Determination of residual erythromycin antibiotic in lyophilized measles vaccine by liquid chromatography mass spectrometry.

2025-04-11T11:11:07+00:00

A simple and sensitive method was developed for determination of residual erythromycin in lyophilized measles vaccine using liquid chromatography tandem mass spectrometry (LC-MS/MS). Erythromycin was extracted from vaccine with methanol. Liquid chromatography was performed on an Acquity BEH-C18; (100 x 2,1 mm; 1,7 μm) column with gradient program of 0.1 % aqueous solution of formic acid and acetonitrile containing 0.1 % formic acid as mobile phase at flow rate of 0.2 mL per minute, temperature: 400C. The Waters Xevo TQD UPLC-MS/MS was operated under the multiple-reaction monitoring (MRM) mode using the ESI+ mode with transitions at (m/z) 734.5 → 157.9 and 734.5 → 576.4. The method was validated for the specificity, linear range, precision, accuracy, LOD and LOQ. The validation results showed that the method was suitable for determination of residual erythromycin in lyophilized measles vaccine.

Study on extraction, isolation and purification of β-ecdysteron from Cyanotis arachnoidea extract for reference standard establishment.

2025-04-11T11:24:41+00:00

In Vietnam and China, Radix Achyranthis bidentatae has been widely used as a traditional herbal. With reference to the quality of Radix Achyranthis bidentatae, its content of β-ecdysteron quantified by HPLC/DAD is specified to be not less than 0.03 %. For the quality control of Radix Achyranthis bidentatae, the establishment of β-ecdysteron as an affordable-price reference standard is prerequisite in Vietnam. In this study, 1.1 g of β-ecdysteron was isolated and purified from 500 g of Cyanotis arachnoidea Extract. The structure of β-ecdysteron was confirmed by 1H, 13C-NMR, HR-MS, IR, UV-VIS…, as compared to the corresponding spectra of β-ecdysteron reference standard. The content of β-ecdysteron in our purified samples was determined to be 92.4 % by HPLC-DAD analysis.