Bioanalysis of aminoglycosides using high-performance liquid chromatography

Aminoglycosides are broad-spectrum antibiotics used in the treatment of gram-negative bacterial infections. Due to their nephrotoxic and ototoxic potential (narrow therapeutic index), the use of aminoglycoside for clinical indications requires monitoring. The objective of this review was to identify relevant literature reporting liquid chromatographic methods for the bioanalysis of aminoglycosides in both preclinical and clinical settings/experiments. Data on liquid chromatographic methods were collected from articles in an online academic database (PubMed, Science Direct, Scopus, and Google Scholar). All 71 articles published from 1977 to 2020 were included in the review. Reversed-phase liquid chromatography was the most used method for the bioanalysis of aminoglycosides. Fluorescence or ultraviolet detection methods were mostly used from 1977 to 2002 (51 articles), while mass spectrometry was predominantly used as a detector from 2003 to 2020 (15 articles). Sixty-seven articles reported calibration ranges, which varied significantly for the various drugs assayed: some in the range of 0.1-0.5 ng/mL and others 1250-200000 ng/mL. Also, 61 articles reported R2 values (0.964-1.0) for almost all analytes under consideration. Sixty-three articles reported percent recoveries mostly between 61.0 % to 114.0 %, with only two articles reporting recoveries of 4.9 % and 36 %. Out of the 71 reviewed articles, 56 reported intermediate precision values ranging between 0.331 % to 19.76 %, which is within the acceptable limit of 20 %. This review will serve as a guide for research and/or routine clinical monitoring of aminoglycosides in biological matrices.

Evaluation of pesticide residues in commercial Swiss beeswax collected in 2019 using ultra-high performance liquid chromatographic analysis

The aim of this study was to determine residue levels of pesticides in Swiss commercial beeswax. Foundation samples were collected in 2019 from nine commercial manufacturers for analysis of 21 pesticides using ultra-high performance liquid chromatography. Individual samples showed the variability and residue ranges and pooled samples represented the average annual residue values of the Swiss production. In total, 17 pesticides were identified and 13 pesticides were quantified. They included 13 acaricides and/or insecticides, two fungicides as well as a synergist and a repellent. The means calculated from individual samples were similar to the average annual residue values for most tested pesticides. Mean values of 401, 236, 106 and 3 μg·kg−1 were obtained for the beekeeping-associated contaminants coumaphos, tau-fluvalinate, bromopropylate and N-(2,4-Dimethylphenyl)-formamide (DMF; breakdown product of amitraz), respectively. For the other pesticides, the mean values were 203 μg·kg−1 (synergist piperonyl butoxide), 120 μg·kg−1 (repellent N,N-Diethyl-3-methylbenzamide, DEET), 19 μg·kg−1 (chlorfenvinphos) and 4 μg·kg−1 ((E)-fenpyroximate), while the means for acrinathrin, azoxystrobin, bendiocarb, boscalid, chlorpyrifos, flumethrin, permethrin, propoxur and thiacloprid were below the limit of quantification (< LOQ). Individual samples contained from seven to 14 pesticides. The ranges of values for coumaphos and piperonyl butoxide (from 14 to 4270 μg·kg−1; from 6 to 1555 μg·kg−1, respectively) were larger as compared to the ranges of values for DEET and tau-fluvalinate (from < LOQ to 585 μg·kg−1; from 16 to 572 μg·kg−1, respectively). In conclusion, the most prominent contaminants were the pesticides coumaphos and tau-fluvalinate, which are both acaricides with previous authorization for beekeeping in Switzerland, followed by piperonyl butoxide, a synergist to enhance the effect of insecticides. Graphical abstract

Liquid chromatography-mass spectrometry method for isomer separation and detection of sugars, phophorylated sugars and organic acids v1

This standard operating procedure is used to achieve effective separation of a wide range of polar metabolites found in central carbon metabolism via a hybrid liquid chromatographic method (ion-exchange chromatography and hydrophilic interaction liquid chromatography (HILIC)) using an Intrada Organic Acid column (Imtakt) coupled with triple quadrupole mass spectrometry. This method gives improved resolution while showing enhanced sensitivity for the detection of low abundance phosphorylated sugars compared with standard HILIC methods.

Phytochemical Profile of Opuntia ficus-indica (L.) Mill Fruits (cv. ‘Orito’) Stored at Different Conditions

This research analyzed the phytochemical profile of prickly pear fruits from ‘Orito’ cultivar stored under cold conditions (2 °C, 85–90% RH) and shelf-life conditions at room temperature (stored at 20 °C for three days after cold storage) for 28 days, mimicking the product life cycle. A total of 18 compounds were identified and quantitated through HPLC-DAD-MS/MS (High-Performance Liquid Chromatographic -Diode Array Detector- Mass Spectrometry) analyses. Phenolic acids such as eucomic acid and betalains such as indicaxanthin were the predominant chemical families, and piscidic acid was the most abundant compound. During cold storage, the content of eucomic acid isomer/derivative and syringaresinol increased, and citric acid decreased, which could be caused by the cold activation of the phenylalanine ammonia-lyase (PAL) and polyphenol oxidase (PPO) enzymes. However, no significant differences were found in the content of these compounds during shelf-life storage. These results showed that ‘Orito’ fruit marketability would be possible up to 28 days after harvesting, retaining its profile, which is rich in bioactive compounds.

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 &lt;2.0%. Conclusion: The proposed RP-LC method can be applied for the routine analysis of commercially available formulations of Escitalopram.