<![CDATA[Current Pharmaceutical Analysis (Volume 20 - Issue 1)]]> https://www.benthamscience.com/journal/32 RSS Feed for Journals | BenthamScience EurekaSelect (+https://www.benthamscience.com) 2024-02-19 <![CDATA[Current Pharmaceutical Analysis (Volume 20 - Issue 1)]]> https://www.benthamscience.com/journal/32 <![CDATA[Preface]]>https://www.benthamscience.com/article/1385882024-02-19 <![CDATA[A Review on N-nitrosamine Impurity]]>https://www.benthamscience.com/article/1374122024-02-19 <![CDATA[Evaluation of the Quality of Water Samples Purified by Compounding Pharmacies in Brazil]]>https://www.benthamscience.com/article/1370642024-02-19Background: Highly purified water is essential for the production of pharmaceuticals, directly impacting the quality and safety of the final product.

Methods: In this work, we studied the physicochemical and microbiological quality of 1477 purified water samples from 25 compounding pharmacies in Southeast Brazil. To the best of our knowledge, this is the most comprehensive study on the quality of water purified in Brazil. It was observed that 47.7% of the samples were purified by reverse osmosis, 39.9% by distillation and 12.4% by deionization. Of the total, 10.63% presented one or more non-compliances. Amongst the three purification processes, the amount of non-compliance was found to be 8.9% for reverse osmosis, 10.9% for deionization, and 12.4% for distillation.

Results: It was therefore concluded that reverse osmosis is advantageous. However, even the advantageous reverse osmosis process showed contamination by viable bacteria, total and faecal coliforms/ E. coli, and Pseudomonas aeruginosa.

Conclusion: Quantitative data showed that all purification processes significantly reduced the conductivity and pH values of the input water. However, conductivity values above the limits and several other non-compliances were found after purification by all processes, which points to the need for additional studies on improvements in purification processes adopted by compounding pharmacies in Brazil.

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<![CDATA[Determination of Ketamine, Fluoroketamine, Norketamine, and 2-Norfluoro-ketamine in Urine using Ultra-performance Liquid Chromatography-tandem Mass Spectrometry]]>https://www.benthamscience.com/article/1378902024-02-19Objective: This study aimed to establish a simple, reliable, and sensitive method for detecting ketamine, fluoroketamine, and their metabolites in urine using UPLC-MS/MS.

Methods: The chromatographic separation was performed on UPLC BEH C18 (50 mm × 2.1 mm, 1.7 μm) at a column temperature of 40°C. The mobile phase consisted of 0.1% formic acid aqueous solution and acetonitrile, with a flow rate set at 0.4 mL/min, following a specific elution procedure. A urine sample was treated with acetonitrile, and midazolam was used as an internal standard. Multiple reaction monitoring was used for quantitative analysis.

Results: Ketamine, fluoroketamine, norketamine, and 2-norfluoro-ketamine exhibited linearity in urine (r>0.99) within the concentration range of 5-2000 ng/mL. Intra-day and inter-day precisions were 9% or less and 12% or less, respectively. The accuracy ranged from 92 to 107%. Mean recoveries were above 76%. The measured matrix effect was between 85 and 104%.

Conclusion: This simple, reliable, and sensitive PLC-MS/MS method was successfully developed to determine ketamine, fluoroketamine, and their metabolite in rat urine.

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<![CDATA[Molecular Absorption Scanning and Assay of Serotonin Reception Inhibitor Antidepressant Drugs]]>https://www.benthamscience.com/article/1374142024-02-19Background: Spectrophotometric techniques are based on the absorption of electromagnetic energy by the molecules of the substance analyzed and can be applied to drug analysis.

Objective: This study has been proposed to carry out molecular absorption scanning and assay in the ultraviolet region of generic antidepressant drugs of the serotonin reuptake inhibitor class produced by three Brazilian laboratories, addressing the importance of good manufacturing practices, drug quality control, and the use of qualitative and quantitative analytical techniques.

Methods: The physicochemical analyses were performed in a Marte Científica (580 UVP) UV-Vis spectrophotometer, and the result was evaluated according to the acceptance interval described in the Brazilian Pharmacopoeia.

Results: When calculating the dosage of the fluoxetine hydrochloride sample, the value of 90.95% was obtained and, therefore, the drug was approved for the dosage test. The dosage test for the drugs, citalopram hydrobromide and sertraline hydrochloride, was also approved, obtaining values of 102.4% and 98.2%, respectively.

Conclusion: The results presented provide future perspectives regarding the rigor of the need for good drug handling practices, maintenance and qualification of quality control laboratory equipment, and the guarantee of validation of analytical methodologies used in the pharmaceutical industries, contributing to the improvement of the quality of production and pharmaceutical products analysis.

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<![CDATA[Isocratic RP-HPLC Method Development, Validation, and Optimization of BCS-II in Bulk and Dosage Form]]>https://www.benthamscience.com/article/1378942024-02-19Background: Previous studies of dextromethorphan hydrobromide basically worked on simultaneous research with other compounds. So, the development of a novel method using the isocratic elution mode is needed.

Objective: For the detection of dextromethorphan hydrobromide (DXM) in diverse matrices, a straightforward, accurate, and sensitive reversed-phase HPLC technique using a Waters 2487 Dual λ Absorbance detector has been designed and validated.

Methods: In this experimental work, utilizing methanol/pH 3.0 potassium dihydrogen phosphate buffer (70:30, v/v) as the mobile phase, the separation was completed in 7 minutes on a C-18 HPLC column (4.6 cm length, 4.6 mm internal diameter; 5 μm particle size) utilizing an isocratic elution mode, flow rate of 1.0 mL/min, and UV-detection at 278 nm. Integration of the chromatography response was carried out using Empower 2.4 software.

Results: With an R2 of 0.9987, the current approach showed high linearity for DXM in the 10- 60 ppm range (retention time 4.281 ± 0.505 min). For DXM Hbr, the limits of detection (LOD & LOQ) were 10.633 μg/mL and 32.221μg/mL, respectively. Samples remained stable in the presence of the matrices without any apparent influence.

Conclusion: The novel approach, which used a straightforward liquid/liquid extraction procedure with recovery ranging from 100 ± 10 % performed by two different analytes, was accurate. The precision within and between days was ≤ 2.0% (RSD). The technique was proven to be reliable and repeatable, and it can be utilized with pharmacological (active ingredients, syrups) and also for biological (blood) matrices which can be used in future research work for bioanalytical method development such as pharmacokinetics studies.

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<![CDATA[Formulation, Analytical Method Development and Validation of an Emulsion of Multi-enzyme with Carminative Oils]]>https://www.benthamscience.com/article/1378892024-02-19Introduction: Indigestion leading to Flatulence is a common problem for infants, and tackling it is tedious for the parents. So, addressing the issue with an ideal formulation should likely have a combination of digestive enzymes and carminatives.

Methods: A formulation containing enzymes like Fungal Diastase (Amylase) and Papain (Protease) for the digestion of Carbohydrates and Protein, respectively, along with aromatic, volatile, carminative oils like Dill Oil, Anise Oil, and Caraway Oil can serve the purpose to mitigate problems associated with infant indigestion and flatulence with maximum compliance.

Results: The stability of multi-enzyme and analysis of carminative oil mixtures still need to be improved due to their inherent characteristics. Enzymes are very likely susceptible to changes in temperature and pH, while the solubility of carminative oils is minimal in the aqueous phase. Also, each enzyme is stable in different pH ranges. Nine emulsions were developed using a suitable buffer system and analyzed by HPLC method.

Conclusion: The optimum pH range was found, and analytical method validation was done for the method's accuracy, precision, and repeatability. The optimum pH was 6-6.5, and the active pharmaceutical ingredients (API) assay was found within the acceptable limit of NLT, 90% for enzymes and 90-110% for carminative oils.

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<![CDATA[Quality Evaluation of Banlangen Granule based on Bioassays of Anti-influenzal and Anti-inflammatory Effects]]>https://www.benthamscience.com/article/1374132024-02-19Objective: In order to control the quality better, this study aimed to develop two bioassay methods of Banlangen Granule (BLGG) based on its anti-influenza activity and antiinflammatory activity and to verify the necessity of established methods by relating the results tested by chemical methods.

Methods: First, the bioassay methods for determining the biopotency of the anti-influenza effect and anti-inflammatory activity were established and applied, taking neuraminidase and cyclooxygenase- 2 as disease targets, respectively. Secondly, the ultra-high-performance liquid chromatography coupled photo-diode array detector (UPLC-PDA) technique was used to perform fingerprints and quantify chemical compounds. Finally, the correlation analysis was performed on the results of bioassay methods and chemical methods to assist in choosing the effective quality markers for the BLGG.

Results: Two accurate, stable, and repeatable bioassay methods were developed and applied to the determination of 57 batches of samples. The chemical fingerprints and contents of seven quality compounds were obtained based on UPLC-PDA methods. From the results of correlation analysis, the highest intensity correlation between these quality markers was medium with a r=0.495 (P<0.01), which indicates the need for establishing a bioassay method for BLGG.

Conclusion: This present work illuminated that bioassay methods can be a great means to evaluate the quality of BLGG effectively and also provided a paradigm case for the quality control of other traditional Chinese medicine preparations.

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<![CDATA[Determination of Tyrosine Kinase Inhibitor Icotinib in Rat Plasma using UPLC-MS/MS and its Application <i>In vivo</i> Pharmacokinetic]]>https://www.benthamscience.com/article/1373592024-02-19Objective: The purpose of this study was to develop a UPLC-MS/MS method for the determination of icotinib concentrations in blood plasma.

Methods: For plasma sample preparation, protein precipitation with acetonitrile was utilized. Analytes were separated on a Kinetex C18 column using 10 mM ammonium acetate containing 0.2% formic acid and methanol (30:70) as the mobile phase, with a gradient flow rate ranging from 0.2 ml·min-1 to 0.4 ml·min-1. The total chromatographic analysis duration was 4.5 minutes. The UPLC system was connected to a mass spectrometer via an electrospray ionization (ESI) interface operated in positive ion mode. Mass monitoring was conducted in multiple reaction monitoring (MRM) modes, with precursor-to-product transitions being m/z 392.06→304.07 for icotinib and m/z 248.00→120.09 for the internal standard, tinidazole. This method has been used for a pharmacokinetic study in rats that were orally administered a single dose of 30 mg/kg icotinib.

Results: The assay showed good linearity over concentration ranges of 1-1000 ng/ml for icotinib, with the correlation coefficient exceeding 0.99. The lower limit of quantitation (LLOQ) was established at 1 ng/ml. Both intra- and inter-day precisions (RSD, %) were below 8.23%. The results demonstrated that stability, matrix effect, extraction recovery, carryover effect and dilution stability were all within the acceptable conditions. The primary pharmacokinetic parameters in SD rats after oral administration of icotinib (30 mg·kg-1) were as follows: t1/2 = (2.92 ± 0.87)h, Cmax = (2168.65 ± 268.72)ng/ml, Tmax = (0.70 ± 0.27)h, AUC=(9.69 ± 1.95)ug/mL•h, Vd = (14.51 ± 5.60)L, and CL = (3.19 ± 0.59)L/h.

Conclusion: A simple and sensitive UPLC-MS/MS method was developed and validated for the determination of icotinib in pharmacokinetic studies.

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