Article of the Year 2020
Studies on Adsorption of Fluorescein Dye from Aqueous Solutions Using Wild HerbsRead the full article
International Journal of Analytical Chemistry publishes research reporting new experimental results and chemical methods, especially in relation to important analytes, difficult matrices, and topical samples.
Chief Editor, Professor Charles L. Wilkins, is a Distinguished Professor of Chemistry and Biochemistry at the University of Arkansas, USA. His research focuses on the development of novel analytical chemistry instrumentation and analysis paradigms.
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Antioxidant Activity In Vitro Guided Screening and Identification of Flavonoids Antioxidants in the Extract from Tetrastigma hemsleyanum Diels et Gilg
This study aimed to investigate the extract with high antioxidant activity of Tetrastigma hemsleyanum Diels et Gilg and identify the antioxidant components in vitro. α, α-Diphenyl-β-picrylhydrazyl (DPPH) radical assay, Trolox equivalent antioxidant capacity (TEAC) assay, ferric reducing antioxidant power (FRAP), and hydroxyl radical scavenging method were used to screen the extract with high antioxidant activity. The antioxidant capacity of the extracts was evaluated by the free radical scavenging ability of DPPH. The ability of extracts to scavenge 2, 2’-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) free radical was evaluated by TEAC assay. The FRAP method was used to evaluate the ability of extracts to reduce Fe3+. The ability to scavenge hydroxyl radicals produced by the interaction of hydrogen peroxide and Fe2+ was measured by monitoring the change in the absorbance of the reaction mixture at 536 nm. Then, high-performance liquid chromatography-DPPH (HPLC-DPPH) and HPLC-hydroxyl radical scavenging methods were used to screen the antioxidant components in the extract. The molecular weight of the above antioxidant components was investigated using the qualitative analytical method of high-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (HPLC-Q-TOF LC/MS). Based on the concentrations of the samples (0.2–4 mg/mL), the DPPH free radical scavenging ability, ABTS+ free radical scavenging ability, hydroxyl free radical scavenging ability, and Fe3+ reducing ability of the ethyl acetate extract (EAE) were stronger than that of the crude extract (CE), petroleum ether extract (PEE), and n-butanol extract (BE). The EAE has higher antioxidant activity than CE, PEE, and BE. Six antioxidant components, rutin, quercetin, isoquercetin, astragalin, kaempferol, and kaempferol-3-o-rutoside, were identified in the EAE.
Simultaneous Determination of Amphenicols and Metabolites in Animal-Derived Foods Using Ultrahigh-Performance Liquid Chromatography-Tandem Mass Spectrometry
Amphenicols are widely used to prevent and treat animal diseases. However, amphenicol residues accumulate in livestock and poultry and harm consumers. We hypothesized that one can combine solid-phase extraction (SPE) with ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) to simultaneously determine amphenicols and metabolites in pork, beef, lamb, chicken, and their products and meet government regulations for maximum residue limits. We extracted crude samples with ethyl acetate and ammonia water (98:2, v/v), purified the samples with a CNW Si SPE column, defatted the samples with acetonitrile-saturated n-hexane, and then determined the resulting analytes by UHPLC-MS/MS. The limit of detection of the analytes in livestock and poultry meat was 0.03–1.50 μg/kg, and the limit of quantification was 0.05–5.00 μg/kg. Measured chloramphenicol, thiamphenicol, and florfenicol concentrations were linear over the range 0.50–50 μg/kg; and the florfenicol amine concentration was linear over the range 5.00–200 μg/kg (all with correlation coefficients >0.9990). The recovery of the spiked samples was between 72% and 120%. The intraday relative standard deviation (RSD) ranged from 1% to 9%, and the interday RSD ranged from 1% to 12%. Based on the above results, the current method is sensitive, accurate, and reproducible with the detection limits being well below the maximum residue limits as per Chinese standard GB 31650-2019, and thus, our research hypothesis could be confirmed.
Optimization of Residual Hexane in Edible Oils Analysis Using Static Headspace Gas Chromatography
This study aims to determine the residual hexane in four edible oils in Malaysia using a simple, rapid, and automated method in order to improve the efficiency and productivity of the analysis. Gas chromatography (GC/FID) equipped with a headspace autosampler (HS-20) was used to perform the analysis. Incubation time for each injection was successfully optimized from one hour to 30 minutes (50% reduction) compared to the official AOCS method Ca 3b-87. Out of the four tested edible oils, only the hexane residues detected in sunflower oil exceeded the maximum residue limit (MRL) set by the European Union regulation. Significant difference of the results obtained between large calibration range (0–938 mg kg−1) and small calibration range (0–68 mg kg−1) suggests that there is a need to use a lower standard calibration concentration to avoid misinterpretation of analysis results. Method validation applies to the technical hexane; 2-methylpentane, 3-methylpentane, cyclohexane, and methylcyclopentane, the signal-to-noise (S/N), as well as the limit of quantification (LoQ) values was found to be 218.20, 221.45, 746.37, 97.37 and 0.85, 0.84, 0.25, 1.93 mg kg−1, respectively. Good linearity, repeatability, and low carryover of this method have provided an alternative way to analyze the content of the residual hexane in edible oils in a more efficient manner. Current study might provide a fundamental reference for the improvement of the AOCS official Ca 3b-87 method for determination of hexane residues in fats and oils analysis in the future.
Electrospun Membrane for the Extraction of Acrylamide in Pet Food Samples
A simple microextraction procedure was developed using an electrospun nanostructured membrane to determine acrylamide in pet food samples. Polyvinyl chloride, polyvinyl alcohol, and polyvinyl alcohol/hydroxyethyl cellulose electrospun membranes were prepared and investigated as a sorbent to extract acrylamide. The characterization of the synthesized electrospun membrane was accomplished using field-emission scanning electron microscopy (FESEM). FESEM images showed uniform morphology and beadless nanofibers. Quantification was done by high-performance liquid chromatography with ultraviolet detection. A series of microextraction parameters were optimized before quantitative analysis of dry pet food samples. The calibration curve exhibited good linearity with a correlation coefficient of 0.996 across a 1–100 μg/kg concentration range. The recovery of acrylamide for pet food samples spiked with 5 and 10 μg/kg was in the range of 79.6–113.9 (n = 3). The intraday precision of the method was less than 12% for three replicated real spiked samples at the 5 μg/kg level. The results demonstrated that the electrospun nanostructured membrane has good extraction selectivity and minimal matrix effect with an enrichment factor of 180-fold.
Determination of Dabigatran Concentration in Human Plasma and Breast Milk
Venous thromboembolism (VTE) is an important cause of death following childbirth. Dabigatran etexilate can be a useful prophylaxis in susceptible women during the postpartum period. However, it is not clear whether dabigatran is excreted into breast milk in amounts which can be harmful to the suckling baby. We have developed an accurate, sensitive, and specific assay for the quantitation of dabigatran in both human plasma and breast milk. This is particularly useful for the determination of the extent by which dabigatran is secreted into breast milk in relation to its systemic availability. Dabigatran was enriched from both matrices using solid-phase extraction prior to separation on a C8-RPLC column and detection using SRM on a QqTrap mass spectrometer. The assay was validated for specificity, sensitivity, linearity, precision, accuracy, and stability of the analyte in human plasma and breast milk. The lower limit of detection for dabigatran was 20 pg/ml in plasma and 75 pg/ml in breast milk. This assay will aid future studies for the measurement of dabigatran concentrations in human breast milk to help determine if dabigatran etexilate can safely be administered to breast-feeding women.
Formulation and development of Serratiopeptidase enteric coated tablets and analytical method validation by UV Spectroscopy
Serratiopeptidase (SRP) is a proteolytic enzyme that emerged as one of the most potent anti-inflammatory and analgesic drugs. The purpose of the present study was to formulate and evaluate enteric-coated tablets for SRP and investigate their stability using a simple and validated analytical method by ultraviolet (UV) spectroscopy. The colloidal silicon dioxide (2.50%), sodium starch glycolate (3.44%), and crospovidone (2.50%) were used as appropriate excipients for the development of core part of tablets. To protect the prepared tablets from acidic environment in the stomach, white shellac, castor oil, HPMC phthalate 40, and ethyl cellulose were used. The seal coating and enteric coating attained were 2.75% and 6.74%, respectively. SRP was found to be linear at 265 nm in the concentration range of 25–150 µg/mL. The results revealed that our developed method was linear (R2 = 0.999), precise (RSD % = 0.133), and accurate (% recovery = 99.96–103.34). The formulated SRP tablets were found to be stable under accelerated conditions as well as under room temperature for 6 months (assay %: >97.5%). The in vitro drug release study demonstrated that enteric-coated tablets were able to restrict SRP release in both acidic environments: 0.1 N HCl and simulated gastric fluid (pH 1.2). Moreover, at 60 minutes, the formulated SRP tablets revealed 13.0% and 8.98% higher drug release in phosphate buffer (pH 6.8) and simulated intestinal fluid (pH 6.8), respectively, compared to the marketed tablet formulation. This study concludes that enteric-coated tablets of SRP with higher drug release in the intestine can be prepared and examined for their stability using validated analytical technique of UV spectroscopy.