This review presents a critical examination of the interface for coupling high performance liquid chromatography (HPLC) with Fourier transform infrared spectrometry (FTIR) since 2010. This coupling offers a robust ana...
详细信息
This review presents a critical examination of the interface for coupling high performance liquid chromatography (HPLC) with Fourier transform infrared spectrometry (FTIR) since 2010. This coupling offers a robust analytical approach characterized by exceptional chemical specificity and the capacity to analyze complex multi-component mixtures qualitatively and quantitatively with high sensitivity, particularly in low limit of detection ranges. This coupling enables the identification of individual components of a mixture by IR after their separation by HPLC, although challenges arise from the potential distortion of infrared spectra by mobile phase components. Addressing this issue necessitates the implementation of suitable interfaces, such as flow cells or off-line indirect measurement methods like hot inert gas streams or ultrasonic nebulizers. The key parameters influencing the coupling of HPLC-FTIR include the solvent elimination methods, mode of FTIR technique, and IR background for accurate analyte identification. Moreover, the composition of the mobile phase and the utilization of buffer solutions in the HPLC mobile phase profoundly impact analyte identification by FTIR.
Herein, for the first time, a vitamin-based metal organic framework is synthesized from vitamin B3 (as a bio linker) and cobalt ions (as a metallic center) and employed as an efficient sorbent in dispersive micro soli...
详细信息
Herein, for the first time, a vitamin-based metal organic framework is synthesized from vitamin B3 (as a bio linker) and cobalt ions (as a metallic center) and employed as an efficient sorbent in dispersive micro solid phase extraction of patulin and ochratoxin A from fruit juice samples. The extracted analytes are quantitatively analyzed using high performance liquid chromatography-tandem mass spectrometry. In this work, after synthesizing the sorbent, it was characterized using X-ray diffraction, Fourier transform infrared spectrophotometry, scanning electron microscopy, nitrogen adsorption/desorption, and energy-dispersive X-ray spectroscopy. In the following, it was used as an efficient sorbent in the offered microextraction method and numerous parameters that could affect extraction efficiency of the method were investigated and optimized using response surface methodology. Based on the method validation results, limits of detection and quantification were 39.6 and 131.7 ng L-1 for patulin, and 24.8 and 82.6 ng L-1 for ochratoxin A, respectively. The extraction recoveries for patulin and ochratoxin A were 75 and 87%, respectively. Repeatability of the suggested approach, expressed as relative standard deviations, were equal to or<5% (at a concentration of 250 ng L-1 of each analyte). Also, environmentally friendly synthesis of the metal organic framework (using vitamin B3 as a linker, water as the reaction solvent, and mild conditions) and usage low amount or volumes of the sorbent and organic solvents in the microextraction procedure were other advantages of the current work.
Development of an accurate analytical method for sulfur species in cyanide leaching units of gold ores where sulfur speciation occurs has important role to explain the metal recovery deviations. This study presents th...
详细信息
(E)-5-Methylhept-2-en-4-one is a key flavour compound in hazelnuts with practical applications in perfumery, flavour, and food industries due to its unique sensory properties. This study developed an effective and sus...
详细信息
(E)-5-Methylhept-2-en-4-one is a key flavour compound in hazelnuts with practical applications in perfumery, flavour, and food industries due to its unique sensory properties. This study developed an effective and sustainable achiral reverse-phase high-performanceliquidchromatography (HPLC) method with diode array detection (DAD) to determine (E)-5-methylhept-2-en-4-one and its reaction intermediates prepared via chiral-pool-based chemoenzymatic synthesis. Given that two reaction intermediates are thermally unstable at the high temperatures used in gas chromatography, HPLC separation at ambient temperatures (avg. 25 degrees C) was an appropriate approach. Optimised HPLC conditions consisting of C18 type stationary phase, mixture of acetonitrile: water (60:40, v/v) as mobile phase under isocratic conditions and flow rate 0.5 ***-1 were used. Chiral normal phase HPLC-DAD method with polysaccharide derivative stationary phase and n-hexane:propan-2-ol (90:10, v/v) as mobile phase was used for separation of enantiomers of (E)-5-methylhept-2-en-4-one. Both achiral and chiral methods were successfully used for monitoring the course of chemoenzymatic synthesis, conversion of reaction intermediates and purity of final product. The achiral HPLC-DAD method showed good linearity (R2 = 0.9997) in concentration range 0.5-100 mu ***-1. The limits of detection and quantitation were 0.1 and 0.3 mu ***-1, respectively. Using developed chiral HPLC-DAD method, sufficient enantioseparation was achieved with resolution of 4.73. Values of LOD and LOQ were 0.2 mu ***-1 and 0.5 mu ***-1, respectively. Besides synthesis monitoring and purity product determination, the developed chiral and achiral HPLC methods could find application in the analysis of (S)-(E)-5-methylhept-2-en-4-one in nut-flavoured foods (e.g., pastries, cookies, desserts, beverages) and personal care products, as well as differentiate pure olive oil from those adulterated with hazelnut oil.
The study presents a green and efficient approach for the determination of phthalates, such as diethyl phthalate (DEP) and dibutyl phthalate (DBP), in sewage water. The method combines dispersive liquid-liquid microex...
详细信息
The study presents a green and efficient approach for the determination of phthalates, such as diethyl phthalate (DEP) and dibutyl phthalate (DBP), in sewage water. The method combines dispersive liquid-liquid microextraction (DLLME) with high-performanceliquidchromatography (HPLC) detection, utilizing ionic liquids, specifically [C6MIM]PF6, as environmentally friendly extraction solvents, and methanol as the dispersant. Through optimization of parameters, including extractive solvent volume and kind, dispersive solvent selection, and salt influence, the method demonstrates exceptional sensitivity and selectivity. Validation studies confirm its analytical robustness, with low limits of detection, high precision, and successful avoidance of matrix interferences. Application to real industry sewage samples from one sewage outfall reveals elevated DEP and DBP detection levels, highlighting the method's efficacy in monitoring environmental pollution. Good linearity of DEP and DBP in the range of 0.200-180.00 mu g/mL (R-2: 0.9999) could be obtained. The spiked recoveries of DEP and DBP were in a range of 90.23%-95.11% and 91.18%-107.4% (RSD <= 5.34) with the detection limits of 0.0053 mu g/mL and 0.0094 mu g/mL respectively. The choice of ionic liquids aligns with green analytical chemistry principles, contributing to sustainable and eco-friendly analytical methodologies. In conclusion, the developed DLLME-HPLC method stands as a promising tool for rapid, efficient, and environmentally conscious determination of trace-level phthalates in complex environmental matrices.
A simple one-step synthesis method was proposed to prepare magnetic carbon material, which were subsequently employed for the magnetic solid phase extraction of carbamate pesticides prior to their determination by hig...
详细信息
A simple one-step synthesis method was proposed to prepare magnetic carbon material, which were subsequently employed for the magnetic solid phase extraction of carbamate pesticides prior to their determination by high performance liquid chromatography. The optimized condition resulted in the efficient extraction of a 30-mL sample solution using 50 mg of magnetic carbon as a sorbent, a 2-min vortex loading time and 1000 mu L of acetone as an elution solvent with a 3-min vortex elution. The linear range of the proposed method was 5-200 mu g L-1, with limits of detection and quantitation in the ranges of 3-40 and 5-60 mu g L-1, respectively. The relative standard deviations were <9.5%, which indicated a high level of precision. The results suggested that the proposed magnetic solid phase extraction method was an effective enrichment procedure and could be effectively implemented for the determination of carbamate pesticides in fruit samples. Satisfactory recoveries in the range of 70.2%-120.0% were obtained with the relative standard deviations of <11.6%. The method provided the benefit of a rapid extraction process, and the magnetic carbon functioned as an eco-friendly adsorbent that could be prepared in an easy manner.
A novel method has been developed for the simultaneous online determination of the isotopic compositions of different antimony (Sb) species in a single analytical run using high-performanceliquidchromatography (HPLC...
详细信息
A novel method has been developed for the simultaneous online determination of the isotopic compositions of different antimony (Sb) species in a single analytical run using high-performanceliquidchromatography (HPLC) coupled with multicollector inductively coupled plasma mass spectrometry (MC-ICPMS), with hydride generation (HG) serving as the interface. Various parameters affecting the precision of Sb isotope analysis including HG conditions, transient signal processing methods and peak integration windows, were optimized. The linear regression slope method and a 100% peak integration window provided the optimal precision. Under optimized conditions, our method achieved external 2SD precisions better than 0.05 parts per thousand for both Sb(III) and Sb(V), with minimal consumption of 0.5 ng for Sb(III) and 5 ng for Sb(V). Furthermore, flow injection (FI) coupled with HG-MC-ICPMS demonstrated precise Sb isotopic analysis with sample requirements as low as 0.25 ng. The proposed methods were validated by analyzing delta 123Sb in synthetic solutions and reference materials. Additionally, it was applied to investigate isotopic fractionation during the reduction of Sb(V) by KI, revealing preferential reduction of the light Sb isotope(121Sb). The isotopic compositions of Sb(V) varied from -0.04- 1.18 parts per thousand, fitting well with a Rayleigh fractionation model and yielding a fractionation factor (alpha Sb(III)-Sb(V)) of 0.99831. In summary, this approach enables high precision isotopic analysis of Sb(III) and Sb(V) simultaneously with reduced sample consumption, providing a powerful tool for investigating Sb isotopic fractionation in various environmental processes and advancing our understanding of the Sb biogeochemical cycle.
Background: Methodologies that preconcentrate high quality nucleic acids (NAs) for downstream assays are essential for their accurate and reproducible analysis by mass spectrometry (MS). Established methods rely on so...
详细信息
Background: Methodologies that preconcentrate high quality nucleic acids (NAs) for downstream assays are essential for their accurate and reproducible analysis by mass spectrometry (MS). Established methods rely on solid-phase extraction that involves numerous steps and user intervention or liquid-liquid extractions that are time-consuming and employ toxic organic solvents. A promising alternative methodology involves anion- exchange microextraction sorbents that selectively isolate NAs through electrostatic interactions with the negatively charged phosphodiester backbone. The microextraction devices recover and preconcentrate NAs using a salt-containing solution, which is generally incompatible with MS analysis. Results: Six anion-exchange microextraction sorbents featuring monomers derived from 2-aminoethyl methacrylate were synthesized and examined in this study to understand the interactions that take place between NAs and the ammonium cationic moiety. Sorbent affinities for bovine serum albumin, small single-stranded oligonucleotides, RNA, short double-stranded DNA), and 2000 bp dsDNA were determined. Recoveries of an oligonucleotide and 2000 bp dsDNA were measured and examined in salt solutions of varied concentration, anion species, and organic additives. high oligonucleotide preconcentration factors of 8.6 +/- 0.2 were obtained for the sorbent featuring two cationic ammonium moieties on each monomer using 500.0 mM ammonium perchlorate. A separate sorbent composed of dimethyl ethyl ammonium moieties produced a preconcentration factor of 4.6 +/- 0.2 using only 31.25 mM ammonium perchlorate. The sorbents were demonstrated in the complete workflow in which an analog antisense oligonucleotide was spiked into human plasma and purified, enabling successful molecular weight analysis. Significance: This study demonstrates the compatibility of microextraction recovery solutions comprised of ammonium perchlorate with reversed-phase and hydrophilic interaction chromatog
chromatography is a key purification process in the pharmaceutical industry. The process design is based on knowledge of the adsorption isotherm that describes the separation within the chromatographic column. Althoug...
详细信息
chromatography is a key purification process in the pharmaceutical industry. The process design is based on knowledge of the adsorption isotherm that describes the separation within the chromatographic column. Although obtaining the values of isotherm model parameters has traditionally been the work of experimentalists, recently design methods based on mathematical models have emerged, and for these, accurate isotherm models and model parameter values are crucial. Different methods exist for parameter estimation, all depending on experiment execution. Model-Based Design of Experiments (MBDoE) can be used to optimally design experiments that maximise the information obtained from each experiment. In this work, we propose an MBDoE-based methodology that aims to identify the most suitable isotherm model, to estimate its parameters, and to evaluate its predictive capability. The methodology is tested on an in-silico case study where the performance is compared to that of traditional factorial design of experiments.
high performance liquid chromatography coupled with post-column derivatization is used for increasing the sensitivity and selectivity of the desirable analytes after the chromatographic separation. The transformation ...
详细信息
high performance liquid chromatography coupled with post-column derivatization is used for increasing the sensitivity and selectivity of the desirable analytes after the chromatographic separation. The transformation of the analytes can be conducted through the addition of a suitable reagent in the eluted stream or the ultraviolet irradiation of the eluted analytes, forming detectable derivatives for ultraviolet or fluorescence detectors. This review focuses on the developed methods using high performance liquid chromatography coupled with postcolumn derivatization for the determination of substances in food samples during the last two decades. The significance of the determination of each analyte in foods and the existing guidelines in each case are discussed. Preparation of the samples and the analytical methods are commented. For each analyte, official methods and commercially available systems and reagents are mentioned, as well.
暂无评论