Determination of Simvastatin by Voltammetry Method at Screen-Printed Electrode Modified by Graphene Oxide Nanosheets and Sodium Dodecyl Sulfate

An accurate, rapid, simple, and novel technique was developed to determine simvastatin (SMV). In this research, a screen-printed electrode (SPE) was deposited with graphene oxide (GO) and sodium dodecyl sulfate (SDS), respectively. For the first time, the handmade modified SPE measured the SMV by differential pulse voltammetry (DPV) with high sensitivity and selectivity. The results of cyclic voltammetry indicated the oxidation irreversible process of SMV. Various parameters (pH, concentration, scan rate, support electrolyte) were performed to optimize the conditions for the determination of SMV. Under the optimum experiment condition of 0.1 M KNO3 as support electrolyte and pH 7.0, the linear range was achieved for SMV concentration from 1.8 to 36.6 µM with a limit of detection (LOD), and a limit of quantitation (LOQ) of 0.06 and 1.8 µM, respectively. The proposed method was successfully utilized to determine SMV in tablets and urine samples with a satisfactory recovery in the range of 96.2 to 103.3%.

Rapid Simultaneous Determination of 11 Synthetic Cannabinoids in Urine by Liquid Chromatography-Triple Quadrupole Mass Spectrometry

Synthetic cannabinoids are a series of synthetic substances that mimic the effects of natural cannabinoids and produce a much stronger toxicity than natural cannabinoids, which have become the most abused family of new psychoactive substances. A solid-phase extractive-liquid chromatography-triple quadrupole/linear ion trap mass spectrometry method was developed to determine 11 synthetic cannabinoids in rat urine. The factors affecting recovery were optimized, and Oasis HLB was selected to extract synthetic cannabinoids simultaneously. The results showed that the linear correlation coefficients of the synthetic cannabinoids ranged from 0.993 to 0.999, and the limit of quantitation ranged from 0.01 to 0.1 ng/mL, and the spiked recoveries ranged from 69.90% to 118.39%. This method has the advantages of good purification ability, simple operation, and good reproducibility, and can be used for the high sensitivity analysis of various synthetic cannabinoids in urine.

Bacterial Detection and Recovery From Poultry Litter

The level of pathogens in poultry litter used for raising broiler chickens is critical to the overall health of a broiler chicken flock and food safety. Therefore, it is imperative that methods used for determining bacterial concentration in litter are accurate and reproducible across studies. In this perspective, we discuss the shortcomings associated with current methods used for bacterial quantification and detection from litter and assess the efficacy of one method for pathogen and commensal (Campylobacter, Salmonella, Escherichia coli, and Enterococcus spp.) recovery. The limit of quantitation and detection for this method differed between pathogens, and the recovery rate (∼138–208%) was higher for Salmonella, E. coli, and Enterococcus compared to Campylobacter (24%). Our results suggest that pathogen recovery from litter is highly variable and pathogen concentrations need to be reported in dry weight before comparisons can be made between studies.

HPLC determination of Escitalopram in tablet dosage forms

Purpose: A simple, specific, precise, and accurate reversed phase liquid chromatographic (RP-LC) method has been developed for the determination of Escitalopram in tablet dosage form. Methods: The chromatographic separation was achieved on a LiChrosorb C18, 250 mm x 4.6 mm, 5 μm column at a detector wavelength of 270 nm and a flow rate of 1.0 ml/min. The mobile phase was composed of methanol, acetonitrile (70:30 v/v). The retention time of Escitalopram was 5.49 min. The method was validated for the parameters like specificity, linearity, precision, accuracy, limit of quantitation and limit of detection. Results: The method was found to be specific as no other peaks of impurities and excipients were observed. The square of correlation coefficient (R2) was 0.9999 while relative standard deviations were found to be <2.0%. Conclusion: The proposed RP-LC method can be applied for the routine analysis of commercially available formulations of Escitalopram.

Eco-Friendly, Simple, Fast, and Sensitive UPLC-MS/MS Method for Determination of Pexidartinib in Plasma and Its Application to Metabolic Stability

Pexidartinib is the first drug approved by the U.S. Food and Drug Administration specifically to treat the rare joint tumor tenosynovial giant cell tumor. In the current study, a validated, selective, and sensitive UPLC-MS/MS assay was developed for the quantitative determination of pexidartinib in plasma samples using gifitinib as an internal standard (IS). Pexidartinib and IS were extracted by liquid-liquid extraction using methyl tert-butyl ether and separated on an acquity BEH C18 column kept at 40 °C using a mobile phase of 0.1% formic acid in acetonitrile: 0.1% formic acid in de-ionized water (70:30). The flow rate was 0.25 mL/min. Multiple reaction monitoring (MRM) was operated in electrospray (ESI)-positive mode at the ion transition of 418.06 > 165.0 for the analyte and 447.09 > 128.0 for the IS. FDA guidance for bioanalytical method validation was followed in method validation. The linearity of the established UPLC-MS/MS assay ranged from 0.5 to 1000 ng/mL with r > 0.999 with a limit of quantitation of 0.5 ng/mL. Moreover, the metabolic stability of pexidartinib in liver microsomes was estimated.

Evaluation of Analytical Performances of Magnetic Force-Assisted Electrochemical Sandwich Immunoassay for the Quantification of Carcinoembryonic Antigen

Carcinoembryonic antigen (CEA) is a biomarker indicated in different cancers, targeted for quantitative analysis via immunoassay. Here we introduce a new technique called magnetic force-assisted electrochemical sandwich immunoassay (MESIA) for determination of CEA level in a drop of human serum using a fully automated point-of-care testing (POCT) device. The analytical performances of the assay are assessed based on precision, accuracy, limit of blank (LoB), limit of detection (LoD) and limit of quantitation (LoQ), linearity, Hook effect, interference, cross-reactivity, and method comparison following the guidelines of the Clinical Laboratory Standards Institute (CLSI). The LoD is 0.50 ng/ml. A linear relationship is shown in the range of 0.5–200 ng/ml. A high dose effect is not seen up to approximately 500,000 ng/ml. The recovery range is from 94.7 to 108.9%. The %CV of run-to-run and within-lab variations are less than 2.04 and 4.41% across the CEA concentrations, respectively, whereas reproducibility is 4.45–6.24%. Method comparison shows that the assay correlates well with the reference device (R2 = 0.9884). The assay demonstrates acceptable precision, accuracy, LoB, LoD and LoQ, hook effect, linearity, interference, cross-reactivity, and high correlation with its reference device. Thus, the system is suitable for the quantification of CEA in clinical practices with a POCT manner.

Determination of Oxaliplatin by a UHPLC-MS/MS Method: Application to Pharmacokinetics and Tongue Tissue Distribution Studies in Rats

Oxaliplatin (OXP), a third-generation platinum-based chemotherapy drug, was often indirectly analyzed via total platinum by an ICP-MS because it was difficult to directly quantify using an LC-MS/MS method, due to its instability, bad column separability and severe MS signal inhibition. Here, we developed and validated a specific, sensitive and reproducible LC-MS/MS method for the quantification of OXP itself in rat plasma and tongue tissue on a SCIEX 4000 QTRAP® MS/MS system equipped with a Phenomenex Lux 5u Cellulose-1 column (250 × 4.6 mm, 5 μm). This method was validated at the lower limit of detection (LOD) and the lower limit of quantitation (LLOQ) of 5 ng/mL and 10 ng/mL, with linearity of 10–5000 ng/mL (r2 > 0.99) and 10–2500 ng/mL (r2 > 0.99), in rat plasma and tongue homogenates, respectively. The intra- and inter-day precision (CV%) and accuracy (RE%) were within 15% for LLOQ, low-, medium- and high-quality control samples. The mean extraction recoveries were around 50% and 80% for plasma and tongue homogenates, respectively. This assay was successfully applied to pharmacokinetics study following intravenous administration of OXP, as well as tongue tissue distribution after 1 h and 4 h of a novel oral mucosal patch application.

Stability Indicating HPTLC Method for Simultaneous Determination of Amlodipine Besylate and Lisinopril in Combined Dose Tablet Formulation

A combined dose tablet formulation containing Amlodipine besylate and Lisinopril is used for the treatment of essential hypertension. The present study reports development and validation of stability indicating high performance thin layer chromatographic method for simultaneous estimation of these drugs in combined dose tablet formulation. The two drugs were satisfactorily resolved on aluminum plates precoated with silica gel 60F254 using n-butanol : methanol: ammonia (4:4:1 v/v/v) as mobile phase. The Rf value for lisinopril and amlodipine besylate were 0.27±0.02 and 0.62±0.02, respectively. Densitometric evaluation of the separated bands was performed at 215nm. The calibration curves for lisinopril and amlodipine besylate were found to be linear in the concentration range of 1000-6000ng/band. The method was validated as per ICH guidelines for accuracy, precision, robustness, specificity, limit of detection and limit of quantitation. Statistical analysis proves that the method is suitable for simultaneous analysis of Lisinopril and Amlodipine besylate in pharmaceutical formulation without any interference from the excipients/degradant. The developed method offers several advantages such as sensitive, rapid, cost effective and less time consuming as compared to the reported methods. As the method could effectively separate the drugs from its degradation products, it can be employed as a stability indicating method.

Comparative between Ammonia Ion Selective Electrode and Dye Binding Method to study effect of Processing Methods on Protein Content of Plain Yogurt

In this study, two analytical methods were used to determinate the protein, the ammonia ion selective electrode method and dye binding method using orange G and the spectrophotometer at λmax 478 nm by determining the linearity, accuracy, precision, limit of detection and limit of quantitation of each. In comparison, the dye binding method was chosen for its accuracy, repeatability, sensitivity (LOD, LOQ) and speed of performance. After that, it was applied to samples of prepared plain yogurt to study effect of different properties (source, heat treatment and type) of used milk on protein content of plain yogurt.

Characterization of handmade Nepali paper as a platform for paper analytical device to determine anti-diabetic drug

The COVID-19 pandemic has highlighted the need of eco-friendly and locally or distributed manufacturing of diagnostic and safety products. Here, we characterized five handmade papers for their potential application to make paper analytical device (PADs). The handmade papers were made from locally available plant fiber using eco-friendly method. Thickness, grammage, and apparent density of the paper samples ranged from 198 μm to 314 μm, 49 g/m2 to 117.8 g/m2, and 0.23 to 0.39 g/cm3, respectively. Moisture content, water filtration and wicking speed ranged from 5.2% to 7.1%, 35.7 to 156.7, and 0.062 to 0.124 mms-1, respectively. Further, water contact angle and porosity ranged from 76˚ to 112˚ and 79% to 83%, respectively. The best paper sample one was chosen to fabricate PADs which were used for the determination of metformin. The metformin assay on PADs followed linear range from 0.0625 to 0.5 mg/mL. The assay had limit of detection and limit of quantitation of 0.05 mg/mL and 0.18 mg/mL respectively. The new method was used to test metformin samples (n=20) collected from local pharmacies. The average amount of metformin concentration in samples was 465.6 ± 15.1mg/tablet. Three samples did not meet the regulatory standards. When compared with spectrophotometric method, PADs assay correctly predicted 18 out of 20 samples. The PADs assay on handmade paper may provide a low-cost and easy-to-use system to screening the quality of drugs and other point-of-need applications.