Journal of chromatographic science最新文献

Antidiabetic drugs, including metformin hydrochloride, are typically used to treat diabetes mellitus. Current methods for evaluating these drug combinations often involve the use of harmful solvents and specific conditions, leading to environmental risks and substantial toxic waste. White analytical chemistry proposes an innovative solution to this problem by developing environmentally friendly, cost-effective and user-friendly chromatographic methods. A synchronous chromatographic assay method for multiple combined pharmaceutical dosage forms of antidiabetic drugs was developed using a single set of chromatographic conditions and safe organic solvents. Method development was carefully carried out using a design of experiments approach to reduce organic solvent waste. The Plackett-Burman design was used in the screening phase to identify critical method variables and responses, facilitated by Minitab 18 software. The Box-Behnken design was then used to optimize these critical variables. A synchronous chromatographic assay of multiple combined pharmaceutical dosage forms was conducted under optimized chromatographic conditions. Finally, a thorough evaluation of the proposed and existing chromatographic methods was conducted using green and white analytical chemical metrics.

A simple, sensitive, and specific liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was successfully developed and validated to determine navitoclax and doxorubicin in rat plasma. Ketoconazole and daunorubicin were employed as internal standards to ensure accurate quantification and method consistency. The sample preparation involved a straightforward protein precipitation technique, which facilitated efficient extraction of the analytes from the plasma matrix. The resulting supernatant was subjected to drying using a vacuum concentrator and later reconstituted before being injected into the LC-MS system. Separation was carried out using a SHIMADZU Shim-pack GIST C-18 column with mobile phase, consisting of a carefully balanced mixture of acetonitrile and water with 0.1% formic acid, with a flow rate of 0.5 mL/min. This composition ensured efficient elution and minimized matrix effects, contributing to the method's robustness and reproducibility. The developed method was comprehensively validated according to regulatory guidelines, assessing various parameters including specificity, selectivity, sensitivity, calibration curve performance, precision, accuracy, stability and dilution integrity. This bioanalytical method has the potential to be extended to various clinical settings, enabling the monitoring drug metabolism, monitoring potential drug-drug interactions and understanding the pharmacokinetic profile and adverse effect potential of the combination therapy.

A novel and validated reverse-phase high-performance liquid chromatography (RP-HPLC) approach was established for the concurrent measurement of cyproconazole (CYP) isomers and tebuconazole (TBZ) in suspension concentrate (SC) agrochemical formulations. The approach employed a C18 column with a gradient elution of 0.1% formic acid in water and methanol, attaining baseline resolution of CYP isomer-1, isomer-2 and TBZ without requiring chiral columns or sample pretreatment. Linearity was confirmed within the range of 80-120% of the target concentration, with a R2 value of 0.999. Accuracy varied from 101.2% to 102.8%, with a %RSD of less than 0.8%. LC-MS analysis verified analyte identity through distinctive ion transitions (CYP: m/z 292, TBZ: m/z 308). This is the initial method for isomer-specific detection of CYP using RP-HPLC within a formulation matrix. The methodology is straightforward, resilient and appropriate for standard quality assurance and regulatory adherence in agrochemical manufacturing.

Polymer monoliths are stationary-phase materials for liquid chromatography and solid-phase extraction. Their porous structure, tuneability and simple synthesis enable tailoring to specific analysis requirements in analytical chemistry. Typically, polymer monoliths are used to separate larger biomolecules. Due to their lower binding capacity, the applications of polymer monoliths for the chromatographic separation of small molecules remain limited. However, recent literature has shown that polymer monoliths have the potential for the extraction of small molecules. In this research, butyl methacrylate-co-ethylene glycol dimethacrylate polymer monoliths were synthesized using localized UV polymerization in capillaries. The performance of reversed-phase polymer monoliths in automated in-line solid-phase extraction-mass spectrometry was demonstrated by the analysis of endocannabinoids from neat standard mixes and spiked cell culture media without prior sample preparation. The synthesized monoliths exhibited a binding capacity of 1896 pmol. Furthermore, we showed the repeatability of the monolith synthesis, with a variance in permeability of 19%. The system's stability is demonstrated through the analysis of multiple batches, comparing different monoliths and reusing the same monolith repeatedly, resulting in relative standard deviations (RSDs) below 20% for all extracted compounds. This automated method with hyphenated mass spectrometry improves throughput over previous manual monolithic extractions for small molecules.

Sodium N-lauroylsarcosinate (NLS) and sodium methyl cocoyl taurate (SMCT) are widely used in sulfate free personal care products. We present a straightforward and highly sensitive High-Performance Liquid Chromatographic (HPLC) method for simultaneous detection and estimation of these substances in commercial personal care products. The HPLC method has a detection limit for NLS of concentrations as low as 1.5 ppm, and that for SMCT of 4.0 ppm, all with a signal-to-noise (S/N) ratio exceeding 3.0. Additionally, the method enables quantification down to 4.5 ppm for NLS, and 12.0 ppm for SMCT, with an S/N ratio surpassing 10.0. This validated method serves as a versatile tool for the accurate quantification of NLS, and SMCT in sulfate free personal care products like shampoos, face washes, body washes, baby shampoos, and toothpastes.

The combination of metformin (MET), teneligliptin (TEN), and pioglitazone (PIO) is newest fixed-dose combination for the treatment type 2 diabetes launched in India. An accurate, rapid, and cost-effective reversed phase ultra-fast liquid chromatography method was developed, validated, and applied for the quantification of MET, TEN, and PIO in bulk and tablet with a very short runtime. Box-Behnken design was implemented to optimize the ultra-fast liquid chromatography conditions. A C18 column (150 × 4.6 mm, 5μ) was utilized with a mobile phase buffer (0.01 M phosphate buffer, pH = 6.2) and acetonitrile in a 51:49 ratio with flow rate of 1.5mL/min at column oven temperature 40°C. Detection was carried out at 255nm by 20 μL injection volume. Retention times were found to be 0.94, 1.36, and 2.07 min, whereas the limit of quantification were 0.209, 0.712, and 57.030 μg/mL for MET, TEN, and PIO, respectively. The linearity of anticipated development was studied in the range of 250-1250 μg/mL (MET, r2 = 0.99974), 10-50 μg/mL (TEN, r2 = 0.99997), and 7.5-37.5μg/mL (PIO, r2 = 0.99999). The relative standard deviation values for method and intermediate precision were <2%. The method was validated as per International Conference on Harmonization guideline for accuracy, precision, linearity, limit of detection, limit of quantification, specificity, robustness, and forced degradation. This is the only study that presents reversed phase ultra-fast liquid chromatography method for the new fixed-dose combination of MET, TEN, and PIO, with the shortest run time of 3.0 min. The proposed method is innovative, efficient, precise, quickest, and economical with high accuracy which makes the study novel.

A screening method was developed for the determination of per- and polyfluoroalkyl substances in textiles by combustion and ion chromatography. In this work, a new type of high-temperature combustion absorption device was designed, and the samples were burned, cracked and gasified by temperature programmed heating mode. The produced free fluorine and hydrogen fluoride gases were absorbed by water vapor and completely transformed into inorganic fluoride anion. After condensation and collection, it was separated and determined by ion chromatography. The pre-treatment conditions were optimized including the sample weight, the combustion method, the combustion gas and its flow rate, the water evaporation rate and the condensate collection method. Method validation was performed in negative samples of cotton, wool and polyester, at spiked levels of 5, 50 and 200 mg/kg, respectively. The average recoveries were between 85.7 and 95.0% with relative standard deviations <20% (n = 7) indicating satisfactory accuracy and repeatability. The calibration curve was performed with the correlation coefficients (R2) higher than 0.999 within a linearity range of 0.01-2.0 mg/L. The limit of quantification was 5.0 mg/kg. The developed method was successfully used to determine the total fluorine in market samples. It can meet the screening determination of PFAS in various textiles.

Plasticizers such as phthalate acid esters including di-(2-ethylhexyl) phthalate (DEHP) and its alternatives are commonly found in extractables and leachables (E&Ls) from plastic-based medical devices. Regulatory agencies require manufacturers to monitor, qualify and quantify the E&Ls from medical devices to ensure the safety. Analyzing E&Ls from medical devices is difficult due to the unpredictability and complexity of matrices. The advent of the novel Polyarc/Flame Ionization Detector (FID), which features compound-independent response, provides the opportunity of quantitation of unknowns-to-be-identified E&Ls without using pure substances for establishing calibration. The present work evaluated firstly the feasibility and efficacy of full scan GC-MS with parallel Polyarc/FID system through analysis of plasticizers in E&Ls. In the same injection, E&Ls were identified by full scan GC-MS, then quantified through Polyarc/FID response factor of internal standards. The results showed that quantitation via response factor from internal standards are more accurate so the need for standards of the identified E&Ls is eliminated. The method can combine screening process and target analysis into a one-step execution, which makes it desirable for E&L analysis. The method was applied to a polyvinyl chloride medical device, yielding 1.183 g/device of acetyl tri-n-butyl citrate, 370.2 mg/device of trioctyltrimellitate, and 3.068 mg/device of DEHP.

Analytical quality by design was used to develop and validate a sensitive, accurate and precise high performance thin layer chromatography method for the determination of glycopyrronium (GLY), formoterol fumarate (FFD) and budesonide (BUD) in pharmaceutical dosage form (Rota caps). Design of Experiment was carried out by Placket-Burman screening design and Box- Behnken response surface methodology using peak area and Rf value as critical method attributes. Method operable design region was navigated for optimization and development of the method. The developed method was validated as per ICH Q2 guidelines. Linearity was found to be 0.25-1.25 μg/band, 0.12-0.60 μg/band and 4-20 μg/band respectively for GLY, FFD and BUD. Accuracy of the method was determined by recovery studies where the percentage recoveries were found to be 98-101%. The precision of the method was determined by repeatability and intermediate precision studies. The % RSD values were found to be less than 2, proving method was precise. The method was found specific and precise for the estimation of drugs. The developed method was applied for the assay of rotacaps and results were found in good agreement with the label claim.

In this report, an ultrasonication and vacuum-assisted headspace solid-phase microextraction procedure followed by gas chromatography-flame ionization detection (UVA-HS-SPME-GC-FID) was proposed for direct extraction of solvent residuals, including benzene, toluene, ethyl benzene, m,p-xylene and o-xylene, in pharmaceutical matrices. A novel robust, reliable and durable nanocomposite solid-phase microextraction (SPME) fiber was prepared by layer-by-layer coating of 3-aminopropyltriethoxysilane-functionalized graphene on a stainless-steel wire. Then, the proposed fiber was used for headspace SPME and trapping of toluene as a residual solvent in solid penicillin, ampicillin and cefazolin vials followed by gas chromatography-flame ionization detection. UVA-HS-SPME-GC-FID achieves better validation parameters, including the limit of detection, limit of quantification, linearity, recovery and repeatability, in comparison with conventional HS-SPME-GC-FID. The UVA-HS-SPME-GC-FID strategy is very effective for quantitatively tracing volatile and semivolatile solvent residuals in various pharmaceutical drugs.