Explore the vast range of titles available.

This article presents the first application of fully automated three-dimensional (3D) column-switching SPE–FIA–HPLC system for the characterization of lipids by a single injection. The whole system was designed and set up by modifying Agilent 1200 Series HPLC system in our laboratory. By using this system, a complete separation profile of the oil samples was achieved in a very short time period by using single injections. This approach was applied on vegetable oils which contains a large number of relatively high-class lipid components, such as TG, FFA, sterols, tocopherols, DG, ester and MG. In this part of the study, we focused on the optimization of evaporative light scattering detector (ELSD) by using an experimental design and RSM. Three experimental parameters were chosen as an independent variables which are the flow rate of mobile phase, nebulization temperature and evaporation temperature. A multivariate five level experimental design was used to establish a quadratic model as a functional relationship between the response values and independent variables. The optimal values of parameters were found to be a flow rate of 1.25 mL min⁻¹, nebulization temperature of 80 °C, and evaporation temperature of 40 °C. Regression analysis with an R ² values indicated as a satisfactory correlation between the experimental and predicted values. ANOVA test results were also illustrate that the models can be successfully used to predict the optimum parameters of ELSD. Thus, the proposed system is suitable for a large number of applications including research and development of new quality control and characterization methods for vegetable oils.

The long-term stability of drugs and metabolites of forensic interest in urine, and preventive measures against their decomposition have been investigated, with special attention to filtration sterilization. An aseptic urine collection kit, which was recently developed based on filtration sterilization, was utilized for the aseptic collection and storage of urine samples. For evaluating preservation measures, methamphetamine (MA), amphetamine (AP), nitrazepam (NZ), estazolam (EZ), 7-aminoflunitrazepam (7AF), cocaine (COC), and 6-acetylmorphine (6AM) were spiked into urine at 500 ng/mL each, and were monitored for 6 months at 25, 4, and −20 °C, after the addition of NaN 3 and/or filtration sterilization using the aseptic collection kit. In severely contaminated urine with bacteria, there were significant losses of 7AF and NZ, and slight decomposition of MA and AP at 25 °C. However, such degradation was successfully suppressed by the use of the kit, though the use of the kit and NaN 3 were preferred for 7AF. The kit was also effective in preventing the hydrolyses of COC and 6AM, while it was suggested that the common preservative NaN 3 can accelerate the hydrolysis of such ester-type drugs and metabolites.

Graphene oxide sheets fixed over silica particles (SiGO) and their modification functionalized with C18 and endcapped (SiGO-C18ec) have been reported as sorbents for extraction and analytical columns in LC. In this study, a SiGO column was selected as the extraction column and a SiGO-C18ec as the analytical column to study the applicability and limitations of a column-switching system composed exclusively of columns packed with graphene-based sorbents. Pyriproxyfen and abamectin B1a were selected as the analytes, and orange-flavored carbonated soft drinks as the matrix. The proposed system could be successfully applied to the pyriproxyfen analysis in a concentration range between 0.5 to 25 µg/mL presenting a linearity of R2 = 0.9931 and an intra-day and inter-day accuracy of 82.2–111.4% (RSD < 13.3%) and 95.5–99.8% (RSD < 12.7%), respectively. Furthermore, the matrix composition affected the area observed for the pyriproxyfen: the higher the concentration of orange juice in the soft drink, the higher the pyriproxyfen the signal observed. Additionally, the SiGO extraction column presented a life use of 120 injections for this matrix. In contrast, the proposed system could not apply to the analysis of abamectin B1a, and the SiGO-C18ec analytical column presented significant tailing compared to a similar approach with a C18 analytical column.

Bisphenol A diglycidyl ether (BADGE) and its related derivatives (BADGEs for short) are reactive epoxides condensed from bisphenol A (BPA) and epichlorohydrin. Nowadays, they are heavily used as additives in the production process of food and beverage contacting materials. However, BADGEs are considered as emerging organic pollutants due to their high toxicity including cytotoxicity, mutagenicity, and genotoxicity. In this work, an online analytical method integrated column-switching technique with supercritical fluid chromatography (SFC) was proposed for the simultaneous determination of bisphenol A diglycidyl ether and its derivatives. In this process, a homemade column was utilized in the first dimension of the column-switching SFC system to preconcentrate the analytes as well as eliminate interferences online. Under the optimal conditions, the obtained calibration curves for BADGEs showed good linearity ranging from 0.02 μg/mL to 10.00 μg/mL, while the values of LOD and LOQ were in the range of 0.0024–0.0035 μg/mL and 0.0080–0.0116 μg/mL, respectively. The optimized method exhibited a good recovery ranging from 85.6% to 105.5% with relative standard deviations less than 11.8%. The developed method provides an eco-friendly and effective way for the rapid and automated analysis of BADGEs at trace levels in canned beverages and can be applied to the high-throughput analysis of other similar matrices.

Angiotensin II receptor blockers (ARBs), a critical class of second-generation antihypertensive drugs, require azide intermediates for constructing their biphenyl tetrazole pharmacophore. This synthetic reaction introduces hypertoxicity risks, as residual azides can induce fatal damage even at trace concentrations. The pharmacopoeias of most countries have highlighted the urgency for improved detection paradigms of the control of azides in ARBs. Current ion chromatography (IC) methods face analytical challenges due to matrix interference from organic solvents and incompatibility with hydrophobic ARB ingredients. Herein, an in situ matrix elimination ion chromatography methodology was established for the sensitive detection of trace azides in angiotensin II receptor blocker pharmaceuticals. The switching strategy used in the proposed methodology eliminates organic interference and avoids the incompatibility issue with ARB ingredients. Under the optimal conditions, the proposed method exhibited satisfactory linearity in the range of 2.0–200.0 ng/mL, with a correlation coefficient of 0.9996. Validation studies demonstrated a detection limit (LOD, S/N = 3) of 0.57 ng/mL and a quantification limit (LOQ, S/N = 10) of 1.89 ng/mL, surpassing the sensitivity requirements in pharmacopeias. Method robustness was confirmed, with recovery rates from 92.8 to 108.7% using spiked ARBs real samples, and the intra-day and inter-day RSDs were less than 9.7%. The proposed approach establishes a reliable, precise, and sensitive alternative for monitoring azide impurities in ARBs, and such a framework can overcome limitations such as solubility issues, contributing to a universal applicability to diverse hydrophobic drugs.

In this study, we developed a column-switching high-performance liquid chromatography (HPLC) method with fluorescence detection for the analysis of vitamin K. Column-switching is accomplished by changing the direction of flow using a switching valve with a set time program. Using this method, three vitamin K, phylloquinone (PK), menaquinone-4 (MK-4), and menaquinone-7 (MK-7), were separated and identified with high sensitivity, and impurities were eliminated. This method was used to determine the vitamin K content in meat, fish meat, snails, bivalves, sea urchins, seaweeds, vegetables, tea, soy products, milk products, and supplements. The results showed that chicken showed the highest content of MK-4 (15.35 ± 0.35 μg/100 g), matcha showed the highest content of PK (3069.66±80.10 μg/100 g), and dried natto showed the highest content of MK-7 (3997.57±79.42 μg/100 g). This method can also be used to analyze vitamin K in supplements and pharmaceuticals. The results of this study revealed that different manufacturers add different types of vitamin K to their commercial supplements and infant formulas. The developed method provides highly reproducible and quantitative results and allows for the rapid analysis of the three vitamin K types. Thus, the method developed in this study may aid the sequential analysis of vitamin K in different samples to assess food nutrients.

This study reports a fast, sensitive, and selective column switching ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method to determine the endocannabinoids (eCBs), anandamide (AEA), and 2-arachidonoylglycerol (2-AG) in plasma samples. This bidimensional system used a restricted access media column (RP-8 ADS, 25 mm × 4 mm × 25 μM) in the first dimension and a core-shell Kinetex C18 (100 mm × 2, 1.7 mm × 1 μM) column in the second dimension, followed by detection in a mass spectrometer triple quadrupole (multiple reactions monitoring mode) operating in the positive mode. RP-8 ADS was used for trace enrichment of eCBs (reverse phase partitioning) and macromolecular matrix size exclusion; the core-shell column was used for the chromatographic separation. The column switching UHPLC-MS/MS method presented a linear range spanning from 0.1 ng mL −1 (LOQ) to 6 ng mL −1 for AEA and from 0.04 ng mL −1 (LOQ) to 10 ng mL −1 for 2-AG. Excluding the LLOQ values, the precision assays provided coefficients of variation lower than 8% and accuracy with relative standard error values lower than 14%. Neither carryover nor matrix effects were detected. This high-throughput column switching method compared to conventional methods is time saving as it involves fewer steps, consumes less solvent, and presents lower LLOQ. The column switching UHPLC-MS/MS method was successfully applied to determine AEA and 2-AG in plasma samples obtained from Alzheimer’s disease patients. Graphical abstract A column switching ultra high-performance liquid chromatography-tandem mass spectrometry method using RP-8 ADS column and core shell column to determine endocannabinoids in plasma samples

The simultaneous determination of monosaccharides present in the activated sludge would be crucial to understand the water treatment mechanism. Herein, an ion chromatography–mass spectrometry (IC-MS) with online pretreatment of column switching technique was proposed to analyze monosaccharides hydrolyzed from extracellular polysaccharides in the activated sludge. When the matrix was eliminated in the first dimension, monosaccharides were immediately identified by IC-MS. The improved ionization efficiency was achieved with the addition of T-joint prior to MS. During the performance test, our established method showed excellent detection limits ranging from 0.34 to 2.15 μg/L for all sugar targets. Great linearity (R ≥ 0.9955) was also achieved using this method in the range from 0.01 to 5 mg/L. Furthermore, the average recoveries were obtained between 84.82 and 113.46%. RSDs for peak areas and retention times were determined as 3.76% and 0.27%, respectively. Finally, this approach provided a rapid, convenient, and practical determination of monosaccharides in the activated sludge, which would be helpful for the analysis of monosaccharides derived from other biological samples.

Polycaprolactone composite nanofibers coated with a polydopamine layer are introduced as a new type of absorption material for on-line solid phase extraction (SPE) in chromatographic system. A hybrid technology combining the electrospinning and melt blowing was used for the preparation of 3D-structured microfiber/nanofibrous polycaprolactone composite. The dopamine coating was then applied to functionalize the micro/nanofibers. Polydopamine-coated polycaprolactone fibers were tested as an extraction phase in on-line SPE prior to HPLC separation and UV detection. Four groups of biologically active substances including bisphenols (Bisphenol S, Bisphenol AF, Bisphenol A, Bisphenol C, Bisphenol AP, Bisphenol Z, Bisphenol BP, and Bisphenol M), betablockers (Timolol, Metoprolol, Labetalol, and Propranolol), nonsteroidal antiphlogistic drugs (Salicylic acid, Ketoprofen, Naproxen, Indomethacin, Diclofenac, Ibuprophen, and Meclofenamic acid), and phenolic acids (Chlorogenic acid, Caffeic acid, Sinapic acid, m-Coumaric acid, Benzoic acid, and Cinnamic acid) were used as the model analytes. Neat and coated fibers were compared and applied as sorbents for the on-line extraction set-up. Both materials produced good extraction potential for the determination of bisphenols and nonsteroidal drugs in model biological and environmental samples including river water, human urine, and blood serum. However, the polydopamine layer significantly increased the extraction efficiency of polar drugs. Typical repeatability of on-line extraction procedure on polydopamine coated fibers was in the range 0.12–4.11% for bisphenols, 0.55–1.41% for antiphlogistic drugs, 0.59–2.52% for phenolic acids, and 1.01–1.65% for betablockers. Graphical abstract Schematic representation of polycaprolactone composite nanofibers coated with a polydopamine layer as an advanced absorption material for on-line solid phase extraction in chromatography.

According to the EU legislation, ochratoxin A contamination is controlled in wines. Tokaj wine is a special type of sweet wine produced from botrytized grapes infected by “noble rot” Botrytis cinerea. Although a high contamination was reported in sweet wines and noble rot grapes could be susceptible to coinfection with other fungi, including ochratoxigenic species, no screening of Tokaj wines for mycotoxin contamination has been carried out so far. Therefore, we developed an analytical method for the determination of ochratoxin A (OTA) and ochratoxin B (OTB) involving online SPE coupled to HPLC-FD using column switching to achieve the fast and sensitive control of mycotoxin contamination. The method was validated with recoveries ranging from 91.6% to 99.1% with an RSD less than 2%. The limits of quantification were 0.1 and 0.2 µg L−1 for OTA and OTB, respectively. The total analysis time of the online SPE-HPLC-FD method was a mere 6 min. This high throughput enables routine analysis. Finally, we carried out an extensive investigation of the ochratoxin contamination in 59 Slovak Tokaj wines of 1959–2017 vintage. Only a few positives were detected. The OTA content in most of the checked wines did not exceed the EU maximum tolerable limit of 2 µg L−1, indicating a good quality of winegrowing and storing.