New ion interaction chromatographic (IIC) system with RP column and boric acid plus tetra-n-butylammonium hydroxide (TBAOH) mobile phase was investigated. In the system: CPhenylHexyl—10 mM H3BO3/4 mM TBAOH, a large group of anions viz. F−,IO3−, Cl−, ClO2−, BrO3−, NO2−, Br−, NO3−, ClO3−, I−, HPO42−, SO42−, CrO42−, S2O32−, benzoate−, SCN−, ClO4− and phthalate2−, could be isocratically resolved. A study

As a result of the excipient materials added to the drug substance to create a formulated pharmaceutical product, the preparation of drug product samples for chromatographic or other quantitative analysis can be manually intensive and time-consuming. It is therefore important that enough focus is placed on this aspect of method development to ensure accurate and reproducible results are obtainable

In the present work, the development and application of two HPLC methods enabling the semipreparative enantioresolution of 1-(biphenyl-3-yl)-2-(1H-imidazol-1-yl)ethanol (1) and 1-[4-[(4-bromobenzyl)oxy]phenyl]-2-(1H-imidazol-1-yl)ethanol (2), two among the most potent and selective heme oxygenase-1 (HO-1) inhibitors known, are described. During the optimization step, different chiral stationary phase

In this work, the synthesis, characterization and chromatographic performance of a silica material chemically bonded with a liquid crystal based on terminal citronellol for HPLC separation were investigated. This bonded liquid crystal stationary phase denoted as LC-LCC8 resulted from the grafting of a mesogenic carboxylic acid, 3′-((3,7-dimethyloct-6-en-1-y1)oxy)-[1,1′-biphenyl]-4-carboxylic acid (LCC8)

An ultrasound-assisted deep eutectic solvent-based liquid-phase microextraction (UA-DES-LPME) was established, for the first time, for the extraction of carbamazepine (CBZ) from human plasma samples. The extract was determined by HPLC-ultraviolet detection (HPLC–UV). A deep eutectic solvent (DES) was readily synthesized by mixing choline chloride and phenol (ChCl:Ph) in the mole ratio of 1:2 in ambient

In this study, Radix Paeoniae Alba with different appearance traits and from three geographical regions was analyzed using a combination of high-performance liquid chromatography fingerprints, chemometrics, and content determination. Hierarchically clustered heatmap was developed for sample visualization. Principal component analysis was used to classify 47 Radix Paeoniae Alba samples with different

In this study, the influence of the different mobile phase compositions on the sensitivity and chromatographic performance of prohibited small peptides (< 2 kDa), their metabolites, and non-peptide substances (anamorelin, ibutamoren) were demonstrated using LC–electrospray ionization coupled with triple quadrupole tandem mass spectrometry (LC–ESI–MS/MS). In the mobile phase, widely used mobile phase

A method involving pyrolysis pretreatment followed by ion chromatography was developed to determine the residual thionyl chloride in levetiracetam. Levetiracetam was combusted at high temperature. After the pyrolysis gas was absorbed, the sulfur in thionyl chloride was converted to sulfate, which were determined by ion chromatography with conductivity detector using potassium hydroxide as the mobile

In this study, the chemical profile of Ling-Gui-Zhu-Gan Decoction (LGZGD) which was prepared by the method recorded in Synopsis of Golden Chamber was analyzed by LC–QTOF MS. A total of 89 compounds were identified, including flavonoids, pentacyclic triterpenes, glycosides, organic acids and others. Among them, nine major active components with high response value in chromatogram were selected for quantification

In this research, three novel ultra-hydrophobic, low-viscosity, non-ionic, and heavier-than-water deep eutectic solvents (DES) based on salol and terpenes are proposed. The prepared DESs were effectively used as extraction solvents in the solidification of settled organic drop (SSOD) microextraction. Despite other hydrophobic DESs, these sustainable bio-compatible extraction mediums are compatible

A novel HPLC method was developed and validated to simultaneously determine curcuminoids and dasatinib in a new dosage form. Excellent separation was achieved for a curcuminoids mixture and dasatinib with a ZORBAX Eclipse Plus Phenyl–Hexyl column (4.6 × 250 mm, 5 µm) and a mobile phase consisting of aqueous solution (0.2% acetic acid and 0.1% trifluoroacetic acid with the pH adjusted to 3.5) and acetonitrile

To explore the pharmacokinetic characteristics of the three monoterpene glycosides (paeoniflorin, albiflorin and oxypaeoniflorin) extracted from the Radix Paeoniae Rubra (RPR), we determined the plasma concentrations of these components in the cerebral ischemia–reperfusion (CIR) rats and the normal rats by a self-developed and validated ultra-performance liquid chromatography-tandem mass spectrometry

A new, sensitive, robust RP-HPLC method was developed using quality by design (QbD) approach for the determination of perampanel in pharmaceutical tablets. Screening of five independent factors; concentration and pH of the phosphate buffer, temperature, flow rate and % of the aqueous part of mobile phase; was performed by a fractional factorial design (FFD). Optimization of the significant variables

To determine deferasirox in human breast milk a novel, sensitive high-performance liquid chromatographic method with fluorescence detection has been developed. Precolumn derivatization process is applied to achieve fluorescent analyte using 4-bromomethyl-7-methoxy coumarin (BrMmC) as a reagent and dibenzo-18-crown-6-ether as catalyst. The method depends on reverse phase chromatography. C18 column has

The solubility of curcumin in the pure water subcritical and water–ethanol solution (water + (5–10) % (v/v) ethanol) subcritical is investigated for the first time. The design approach taken from this study is the response surface methodology due to the Box Behnken. The experiments were performed in the temperature range of (90–150) °C, (0–10) volumetric percent of ethanol and the flow rate of (0.2–0

Synthetic cannabinoids (SCs) are the most rapidly growing class of recreational designer drugs. The rapid growth in popularity of SC use among teens and adults is of serious in our country as all of the world. These products are saturated in various plants crumb in order to make herbal appearence. They are not for human consumption and also their chemical structures are rapidly evolving. They are known

Abstract A quality by design-based stability indicating HPLC method has been developed for hydroxychloroquine sulfate impurities. The optimized HPLC method can detect and quantify the hydroxychloroquine sulfate and related organic impurities in pharmaceutical solid oral dosage forms. Nowadays, for the quantification of impurities in drug products demands more comprehensive way of analytical method

A simple, rapid and robust protocol for the characterisation of strong cation exchange columns for the analysis of small molecular weight bases is described. A range of ten different phases were characterised, and the resultant selectivity and retention factors analysed using Principal Component Analysis. The score plots for the first and second principal components described 83% of the variability

There is a growing need for chemical analyses to be performed in the field, at the point of need. Tools and techniques often found in analytical chemistry laboratories are necessary in performing these analyses, yet have, historically, been unable to do so owing to their size, cost and complexity. Technical advances in miniaturisation and liquid chromatography are enabling the translation of these

Graphene oxide (GO)-based dispersive solid phase extraction (D-SPE) method combined with multi-step preparation has been put forward for the evaluation of trace ochratoxin A (OTA) in chicken liver. The homogenized tissue sample was initially clean-up and extracted with petroleum ether, ethyl acetate and 0.1 mol/L sodium bicarbonate solution and then adsorbed using GO originally targeting for OTA. The

A composite material featuring a zirconium-based metal–organic framework and graphene oxide (Zr-MOF@GO) was synthesized by a hydrothermal method and bonded to a stainless steel wire with an inorganic binder as a solid-phase microextraction (SPME) fiber for the derivatization-free extraction and analysis of nonsteroidal anti-inflammatory drugs (NSAIDs) coupled with gas chromatography (GC). The force

In this article, we depicted the structure of the investigated fat-and water-soluble vitamins in Fig. 2.

Previously developed three-phase retention model has been extensively used to understand the partition behaviors of solutes in micellar liquid chromatography (MLC). The model has been used to explain the linear plots of the reciprocal of the solute retention factor versus the micelle concentration in the mobile phase. Because a phase equilibrium model of micellization is assumed, the retention model

Dapagliflozin (DAP) is therapeutic agent for diabetes mellitus type II patients with insufficient glycemic control by exercise and diet. Stability-indicating LC–MS method was developed and validated on C8 column and method was able to separate DAP and three major hydrolytic degradation products. Structure elucidation of three major identified hydrolytic degradation products (DPs) and establishment

The combined implementation of quality by design principles and green analytical chemistry leads to development of green micellar HPLC method for analysis of atorvastatin calcium and amlodipine besylate in binary mixtures and in their tablet dosage forms within 8 min. A two-level fractional factorial design was implemented for screening of different method parameters affecting chromatographic responses

We developed a novel, rapid, sensitive, and stability-indicating UHPLC method for quantification of Perindopril (PER), Amlodipine (AML), and their impurities in pharmaceutical formulations. The optimum chromatographic separation was achieved in gradient elution mode using Agilent SB C18 (50 × 3.0 mm, 1.8 μm) column. A buffer containing 0.1% perchloric acid and acetonitrile was used as a mobile phase

Human–elephant conflicts continue to escalate as African elephants (Loxodonta africana) attempt to forage on cultivated crops. Chili pepper fencing is used as a deterrent but has varying success rates. These fences are constructed with crushed chili peppers, typically mixed in motor oil, placed on cloths, and strung around crop fields. This mixture is made using different formulas involving oil and

A simple, inexpensive, rapid and novel stability-indicating reversed-phase high-performance liquid chromatographic method employing Zorbax-CN column has been developed and validated for the determination of both, assay and related substances of Solifenacin Succinate (SOL) drug substance and in its drug product. Forced degradation study of SOL was performed at acid, base, oxidative, photolytic and thermal

A method for preparing a metal–organic framework (MOF)–polymeric monolith was established by in situ radical polymerization with derivatized UiO-66-2COOH and N-isopropylacrylamide (NIPAAm) as co-monomers. It was worth noting that the obtained monolith possessed characteristics of relatively uniform porous structure and a high surface area (84.16 m2 g−1). The adsorption capacity of the monolith increased

Lateral flow assays (LAFs) especially integrated with a microfluidic chip, provides a simple, rapid, user-friendly, potable robust, and cost-effective technology for broad assays. However, this technology suffers from low sensitivity. In this paper, one kind of automatic roller of tap, which can be precisely controlled to replace sample tap was integrated into the microfluidic LAFs platform. And then

A mass spectrometer compatible, reverse-phase high-performance liquid chromatography method capable to resolve twenty-six impurities and degradation products (DPs) in Ertapenem (ERT) has been developed. Eight dimer impurities (m/z 951) and two dehydrated dimers (m/z 933) were baseline resolved. Out of eight dimers, four dimers are reported the first time. The impurities and DPs were identified using

The choice between capillary electrophoresis (CE) and high-performance liquid chromatography (HPLC) is not easy and depends on many factors. An attempt to facilitate this choice is this work, in which both techniques have been confronted on the basis of the RGB model, offering a transparent and pictorial way to compare individual parameters as well as the overall analytical potential of each tool.

The organic extracts recovered from 14 potsherds of Dressel 20 oil amphorae collected from Pax Julia civitas (Lusitania) were analysed by GC–MS. Biomarkers of plant oils (saturated and unsaturated fatty acids, alcohols and alkanes arising from plant waxes) were identified in ten samples, and Pinaceae spp. pitch biomarkers were also identified in eight samples. The biomarkers identified in the studied

AbstractAn aqueous normal-phase high-performance liquid chromatography method was developed to separate cis/trans isomers of 4,5-dihydroxy­imidazolidine-2-thione and 4,5-dimethoxy­imidazolidine-2-thione on a Luna HILIC 200 Å column containing silica surface covered with cross-linked diol with an eluent acetonitrile/water in the ratio of 95:5 v/v. Changing of the analysis parameters leads to selectivity

The quality by design strategy was applied for the simultaneous chromatographic quantification of a binary mixture of bromhexine HCl and its pharmacologically active metabolite ambroxol HCl in dosage forms as well as in human plasma. In this study, five independent parameters were screened by fractional factorial design to specify the critical ones. The optimal conditions were determined by a response

Perfluoroalkyl substances (PFASs) are used in a variety of industrial and household applications. Unfortunately, they are released to the environment including aquatic ecosystems and undergo accumulation processes (e.g., in sediment). Due to these aspects but also toxicity, PFASs can pose a threat to the environment and humans, so their determination (mainly with liquid chromatography) in environmental

In this research, new DABCO-based ionic liquid-modified Fe3O4 nanoparticles (NPs) were synthesized by the quaternization reaction. Modified magnetic NPs were characterized by different techniques. The functionalized magnetic NPs were utilized as a novel sorbent for magnetic SPE of imatinib mesylate (IMA) from human plasma samples followed with UPLC–MS–MS. Effective parameters on the extraction of IMA

Analytical prospects of ionic liquids as the components of the microemulsion for polyphenols separation by microemulsion electrokinetic chromatography are explored. Imidazolium-based hydrophilic ionic liquid 1-hexadecyl-3-methylimidazolium chloride was used as a surfactant and hydrophobic ionic liquids 1-hexyl-3-methylimidazolium tetrafluoroborate and 1-hexyl-3-methylimidazolium bis(trifluormethylsulfonyl)imide

The day-by-day increase in the novel drug delivery system market produces the utmost need to develop a reliable, robust, and accurate method. Moreover, the recent ICH (ICH Q8-Q11) guidelines recommend the use of modern systemic approaches such as quality by design (QbD) adopted for the development of robust analytical methods. Thus, the aim of the present study is to develop and validate a novel HPLC

A new type of partially substituted cyclodextrin-bonded silica particles, phenylcarbamate-(3-(2-O-β-cyclodextrin)-2-hydroxypropoxy)-propylsilyl-appended silica (P-CD-HPS), has been successfully prepared and used as chiral stationary phase (CSP) in high-performance liquid chromatography (HPLC) under normal-phase, reversed-phase, and polar organic mobile-phase conditions. The P-CD-HPS was characterized

Dasatinib is a protein kinase inhibitor used for the treatment of chronic myelogenous leukemia and acute lymphoblastic leukemia. Dasatinib along with its six known organic impurities were separated using the reversed-phase high performance liquid chromatography with C18 column and mobile phases consisting of gradient mixture of 20 mM potassium phosphate buffer at pH 6.0 with 1-octanesulphonic acid

A micellar electrokinetic capillary chromatography (MEKC) method has been developed and validated for simultaneous analysis of febuxostat and its related substances in active pharmaceutical ingredients and pharmaceutical formulations. Analysis was performed in an uncoated fused silica capillary (34 cm effective length, 50 µm diameter). Method sensitivity was enhanced using an extended light path capillary

In this study, two carotenoid antioxidants lutein and neoxanthin were investigated for their ability to prevent oxidatively induced DNA damage. A Chlamydomonas reinhardtii alga was used as the natural source of lutein and neoxanthin. Analysis using HPLC with Diode Array Detector (DAD) showed that lutein and neoxanthin were the most abundant carotenoids in the extract of C. reinhardtii. An analysis

A poly (N-isopropyl acrylamide) (polyNIPA)-based hybrid column for capillary liquid chromatography (cLC) was prepared with N-isopropyl acrylamide (NIPA) and alkoxysilanes through a sol–gel “one-pot” method. In this process, the hydrolyzed tetramethoxysilane (TMOS) and vinyltrimethoxysilane (VTMS) were the precursors for the synthesis of a silica-based monolith and subsequently reacted with organic

The use of high performance thin-layer chromatography (HPTLC) in combination with high resolution time of flight mass spectrometry (MS) for the detection, identification and imaging (HPTLC/MSI) of ecdysteroids (insect moulting hormones) present in a number of plant extracts obtained from members of the Silene family is demonstrated. DESI is shown to be a convenient method for the recovery of these

AbstractMulti and comprehensive two-dimensional gas chromatography application have been increasingly mentioned in different countries. This technique increases the efficiency of peak separation in chromatographic analysis, minimizing problems due to the presence of interfering compounds in the analysis, especially in complex matrices. In Latin America, it has been applied to different areas of study

Reliable simulation of retention factor (k) is crucial in high-performance liquid chromatography (HPLC) method development. In this research, three different Artificial intelligence (AI) based models, namely the multi-layer perceptron (MLP), Support vector machine (SVM) and Hammerstein–Weiner (HW) models, were employed as well as three ensemble techniques, i.e., neural network ensemble (NNE), weighted

The effects of furoic acid and furfuryl alcohol on the detection of furfural in transformer oil were studied using the traditional liquid–liquid extraction combined with high-performance liquid chromatography (LLE-HPLC) technology, in which, the methanol used as extraction agent and the C18 column and ultraviolet−visible detector were used as the separation and detection units for the determination

Solriamfetol is a novel FDA approved enantiopure drug used for the treatment of excessive sleepiness associated with narcolepsy or obstructive sleep apnea. Only the active R-enantiomer is marketed, therefore, a method to determine the chiral purity is essential. Chiral separation of solriamfetol was performed by HPLC using polysaccharide-type chiral stationary phases in polar organic mode and described

Drugs of abuse can be investigated in dried blood spot (DBS) samples to evaluate the intake of psychoactive drugs. We have developed the validated liquid chromatography–tandem mass spectrometry method to determine drug of abuse in whole blood with DBS. The mass spectrometer was performed using multiple reaction monitoring via positive electro-spray ionization. The analysis procedure was applied to

Histamine level determination in fish and fish products is important for human safety, fish quality and food industry. For this reason, a rapid, robust, and precise method is needed. To achieve this objective, an HPLC method with fluorescence detection was developed and validated. Histamine in fish samples was efficiently extracted with perchloric acid, and purified with ion-exchange solid-phase extraction

AbstractXiebai San (XBS) is a classical herbal prescription which has been used for the treatment of infantile cough and asthma for several hundred years. In this study, 39 compounds in XBS standard decoction were identified by HPLC–ESI–TOF system. Network pharmacology strategy was adopted to explore the relationship of chemicals, target genes and pathways, mulberroside A, kukoamine B and glycyrrhizic

In this study, a triazine-based polymeric network-modified magnetic nanoparticles (TPN/MNPs) was synthesized and applied as adsorbent for extraction of 1-naphthylacetic acid (NAA) from the fruit and vegetable samples followed by HPLC determination. The synthesized TPN/MNPs were characterized by the vibrating sample magnetometry (VSM), Fourier-transform infrared spectroscopy (FT-IR), field emission-scanning

A rapid reversed-phase gradient method employing a 50 mm × 1 mm i.d., C18 microbore column, combined with ion mobility and high-resolution mass spectrometry, was applied to the metabolic phenotyping of urine samples obtained from rats receiving different diets. This method was directly compared to a “conventional” method employing a 150 × 2.1 mm i.d. column packed with the same C18 bonded phase using

A high-performance liquid chromatographic method was developed for the separation and determination of 13 vitamin B compounds, including thiamin, riboflavin, riboflavin 5′-monophosphate, pyridoxine, hydroxocobalamin, cyanocobalamin, adenosylcobalamin, methylcobalamin, niacin, niacinamide, pantothenic acid, folic acid, and biotin. The method consisted of an ODS column, a gradient elution using pH 3