Tryptamines are hallucinogenic substances many of which have appeared recently as novel psychoactive substances (NPS). Herein, we describe the establishment of a rapid UHPLC-MS/MS quantitative method for the targeted screening of 16 tryptamines of abuse in hair. Twenty milligram pieces of hair were pulverized below 4 °C in 0.5 mL of deionized water containing 0.1% formic acid and an internal standard

We describe a simplified approach for purification and characterization of human ‘IgG-Fc’ fragment used widely as immunochemical tool and for therapeutic purposes. The ‘Fc’ fragment was purified from human IgG in a 3-stage column chromatography. The purified ‘Fc’ fragment appeared as a dimer glycoprotein with an apparent molecular mass of 52981 Dalton (Ultraflex MALDI TOF/TOF). The Size-exclusion HPLC

An affinity ligand was designed from 1-aminocyclohexane based on the crystal structure of Streptomyces albidoflavus phospholipase A1 (saPLA1) by using Discovery Studio software. The molecular docking results indicated that the designed ligand could interact with the active pocket of saPLA1. Epichlorohydrin, cyanuric chloride and 1-aminocyclohexane were used to synthesize the affinity ligand, which

Urinary catecholamines and their methylated metabolites are biochemical indicators of pheochromocytoma, paraganglioma and neuroblastoma. A rapid and precise analytical method based on solid-phase extraction (SPE) and liquid chromatography separation coupled to high-resolution mass spectrometry (LC-HRMS) was developed and validated to measure urinary catecholamines (epinephrine (E), norepinephrine (NorE)

In this work, α-glucosidase was immobilized on a type of nanoscaled magnetic materials Fe3O4@ZIF-67 to construct a biomicroreactor for rapid screening α-glucosidase inhibitors. The parameters that affected the immobilization efficiency were investigated. Under optimal conditions, the amount of α-glucosidase loaded was up to 79.07 μg·mg-1. Then, the enzyme biomicroreactor was immobilized by an external

Glaucoma is a heterogeneous group of multifactorial optic neuropathies and the leading cause of irreversible blindness and visual impairment. Epidemiological data has estimated that in 2020 there will be more than 80 million individuals affected by the disease worldwide. Nowadays, intraocular pressure (IOP) lowering is carried out mainly by pharmacotherapy, with different drugs. The study of ocular

In this paper, a calibration procedure for LC/MS-based bioanalysis methods, termed “A/B fortification”, is proposed. The concept relies on the post-extraction fortification (B-spike) of an aliquot of the injection-ready sample extract for the determination and compensation of specific signal suppression or enhancement effects compared to matrix-free extract prepared in buffer or mobile phase. Conventional

Extraction of polar acidic compounds is a challenging task in electromembrane extraction. In this study, gel-electromembrane extraction was employed for the extraction of phenolic acids as polar acidic compounds from fruit juices. For this aim, the extraction of phenolic acids from the juice samples (4 mL, pH = 6.0) was carried out across the agarose gel membrane (concentration of agarose; 3% (w/v)

The aim of this study was to develop and to validate a UPLC-MS/MS method for the quantification of morphine, morphine-3-glucuronide, and morphine-6-glucuronide in mouse plasma and tissue homogenates to support preclinical pharmacokinetic studies. The sample preparation consisted of protein precipitation with cold (2-8 °C) methanol:acetonitrile (1:1, v/v), evaporation of the supernatant to dryness,

A simple, rapid, cost-effective and sensitive high-performance liquid chromatography method with diode array detection was developed and validated for the quantification of letermovir, a compound approved for prophylaxis of cytomegalovirus infection and disease in adult recipients of an allogeneic hematopoietic stem cell transplant. Sorafenib was used as internal standard. Samples were pre-treated

Treatment of multidrug-resistant tuberculosis (MDR-TB) is challenging due to high treatment failure rate and adverse drug events. This study aimed to develop and validate a simple LC-MS/MS method for simultaneous measurement of five TB drugs in human plasma and to facilitate therapeutic drug monitoring (TDM) in MDR-TB treatment to increase efficacy and reduce toxicity. Moxifloxacin, levofloxacin, prothionamide

Pesticides are chemicals widely applied in agriculture and proven environmental contaminants; their hazards include harmful effects on human health, therefore the evaluation of exposure is relevant to risk assessment. Hair is a non-invasive specimen that incorporates pollutants allowing an extended exposure window to be surveyed. Aim of this work was to develop and validate an assay for measuring 41

Vitamin D status is typically assessed by the measurement of 25-hydroxy vitamin D (25(OH)D). However, in selected patient groups the sole determination of 25(OH)D has been proven insufficient for this purpose. The simultaneous measurement of additional vitamin D metabolites may provide useful information for a better evaluation of the vitamin D status. Therefore, we developed and validated a liquid

The continuous bed bioreactor systems have been used for the production of protein therapeutics, such as IgG, using immobilized enzyme in biopharmaceutical applications. We developed macroporous poly(hydroxyethyl methacrylate-co-glycidyl methacrylate) cryogel-based bioreactor matrix using sodium dodecyl sulfate as surfactans in the presence of ethylene glycol dimethacrylate as cross linking agent by

Serotonin (5-hydroxytryptamine, 5-HT) is readily secreted in patients with carcinoid tumors, especially arising from the midgut. Although serotonin assay in human plasma or whole blood has been extensively studied, serotonin assay in human serum by liquid chromatography-tandem mass spectrometry (LC-MS/MS) has received much less attention. In this study, a simple and reliable LC-MS/MS method based on

This study presents the development and validation of a fast and simple bioanalytical ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS) method intended for quantifying the anti-inflammatory candidate 5'-methoxynobiletin (5'-MeONB) in rat plasma. Standard of 5’-MeONB was purified from A. conyzoides extract by using preparative HPLC. After a pretreatment of plasma samples with

A procedure for the quantification of steroid hormones of various classes in human urine (androgens, estrogens, progestins, corticosteroids) has been described consisting of sample preparation by means of dispersive liquid-liquid extraction after enzymatic hydrolysis with β-glucuronidase from E. Coli followed by ultra-high performance liquid chromatography–high resolution mass spectrometry (quadrupole

Residue chemists who analyze pesticides in vegetables or veterinary drugs in animal-based food are currently facing a situation where there is a requirement to detect more and more compounds at lower and lower concentrations. Conventional tandem quadrupole instruments provide sufficient sensitivity, but speed and selectivity appear as future limitations. This will become an even larger issue when there

A selective and sensitive procedure for quantitation of a new antithrombotic drug (GRS) in rat plasma was developed and validated using an HPLC-UV. The method was validated according to recommendations of the FDA, EMA in terms of selectivity, linearity, accuracy, precision, recovery, matrix effect, stability, and carry-over. The preparation of the biological sample included liquid-liquid extraction

In the present study, the adsorption of phenolic compounds, first of all, chlorogenic acid isomers (chlorogenic, neo-chlorogenic and crypto-chlorogenic acids) predominant in the artichoke (AE) or green coffee bean (GCBE) extracts on cross-linked cationic starch having quaternary ammonium groups (CCS) has been investigated. The equilibrium adsorption studies showed that adsorption closely followed the

The main challenges in the purification of αS2-casein are due to the low quantity in milk and high homology with other casein subunits, i.e., αS1-casein, β-casein, and κ-casein. To overcome these challenges, the aim of this study was to develop a two-step purification to isolate native αS2-casein in goat milk from five different breeds; British Alpine, Jamnapari, Saanen, Shami, and Toggenburg. The

3′, 5′ – Cyclic adenosine monophosphate (cAMP) is a ubiquitous second messenger that is involved in many cellular functions and biological processes. In several cell types, cholera toxin will increase the level of cAMP, which mediates toxic effects on cells. In this context, we have developed a fast and simple method based on extraction with 5% trichloroacetic acid (TCA) and quantitation with liquid

The successful application of monoclonal antibodies (mAb) in oncology and autoimmune diseases paved the way for the development of therapeutic antibodies with a wider range of structural and physico-chemical properties. A pH-gradient combining 2-(N-morpholino)ethanesulfonic (MES) and 4-(2-hydroxyethyl)-1-piperazineethanesulfonic acid (HEPES) buffers and mediated with potassium chloride was developed

Snake venoms are complex chemical mixtures of biologically active proteins and non-protein components. Toxins have a wide range of targets and effects to include ion channels and membrane receptors, and platelet aggregation and platelet plug formation. Toxins target these effectors and effects at high affinity and selectivity. From a pharmacological perspective, snake venom compounds are a valuable

This study aimed to optimize a new sample preparation method using N-doped mesoporous carbon sorbent for simultaneous measurement of 1-naphthol and 2-naphthol, the biomarkers of exposure to naphthalene. The samples were analyzed using high-performance liquid chromatography supplied with ultraviolet detector (HPLC-UV). N-doped mesoporous carbon sorbent was obtained via the hard template procedure. The

Monosaccharide composition of biological samples can reflect an individual’s health status. Monitoring the concentration of individual monosaccharides in human serum requires a technique for the simultaneous analysis of multiple monosaccharide molecules. Furthermore, certified reference materials (CRMs) for overall monosaccharide composition of human serum are required in order to validate the performance

Dexmedetomidine, as a safe sedative, mainly exerts on the central nervous system particularly in the locus coeruleus producing arousable sedation with potential analgesic and anxiolytic effects. The quantification and pharmacokinetic investigation of dexmedetomidine in the central nervous system have been described rarely. In order to estimate the unbound dexmedetomidine concentrations in brain extracellular

A sensitive liquid chromatography-tandem mass spectrometry (LC-MS) method was developed for the screening of five β-blockers (BBs), including atenolol, metoprolol, bisoprolol, propranolol, and betaxolol, in rabbit plasma. An inhouse prepared hydrazonoyl chloride compound (UOSA54) and dansyl chloride (DNS) were successfully coupled with BBs via the amino functional group and analyzed by LC-MS/MS. The

As an anticoagulant, Edoxaban (EDX) is a high risk drug that may cause a life-threatening bleeding. Also, it is prescribed as a chronic therapy for atrial fibrillation and venous thromboembolism patients. They are special population that needs appropriate care and optimum dosing of EDX. Hence, its monitoring in the patient plasma is fundamental, especially in emergency and special circumstances. However

Exposure to repeated stress is associated with the occurrence and development of many prevalent diseases. Here, we evaluated the impact of a repeated restraint stress (RRS) paradigm on male Wistar rats and compared global plasma metabolites in stressed and unstressed rats using an ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC/Q-TOF-MS) approach and

A rapid, highly sensitive and simple high-performance liquid chromatographic–tandem mass spectrometric (LC–MS) assay is developed and validated for the quantification of leuprolide: a Gonadotropin Releasing Hormone analog (GnRH) in human plasma. Moreover, various parameters of the method stability are determined. After the addition of stable isotope (internal standard), the leuprolide was extracted

Solid phase micro extraction-Gas Chromatography/Mass Spectrometry (SPME-GC/MS) analysis was performed in exhaled breath samples of 48 healthy volunteers: 20 non-smokers, 10 smokers and 18 e-cigarette (EC, vape) users. Each volunteer provided 1 L of exhaled breath in a pre-cleaned Tedlar bag, in which an SPME fiber was exposed to absorb the emitted breath volatile organic compounds (VOCs). The acquired

Gas chromatography-mass spectrometry (GC–MS) is an ideal tool for analyzing the intermediates of tricarboxylic acid cycle and glycolysis, sugars, organic acids and amino acids, etc. High-throughput metabolomics methods are required by large-scale clinical researches, and time of flight mass spectrometry (TOF MS) having fast scanning rate is preferable for rapid GC. Quadrupole MS (qMS) instruments have

Urate anion exchanger 1 (URAT1) expressed in the proximal renal tubules is responsible for about 90% of the reabsorption of uric acid. URAT1 is identified as an important target of uricosuric drugs. Here we present an LC-MS/MS-based approach, combined with URAT1-transgenic MDCK cells, for the assessment of uric acid. Cell lysis was executed with 50 mM NaOH to release uric acid. 1,3-15N2 uric acid was

A simple, rapid, sensitive, and reproducible liquid chromatography-tandem mass spectrometry method was developed to determine sitagliptin in human plasma. Diphenhydramine HCl was used as internal standard (IS). The chromatographic separation was achieved using Agilent Poroshell 120 EC-C18 – Fast LC column (100 × 2.1mmID, 2.7) fitted with UHPLC Guard Poroshell 120 EC-C18 (5 × 2.1mmID, 2.7 µm). The mobile

N-ethylhexedrone (NEH) and buphedrone (BUPH) are synthetic drugs structurally related to natural cathinone. These synthetic cathinones (SC) are members of the heterogenous family of new psychoactive substances (NPS), which have caused major concern in scientific and forensic communities over the past years, due to their widespread consume. Thus, there is a constant need for monitoring the use of these

The purpose of this work was to develop and validate a single sensitive, selective and rapid bioanalytical method to determine ceftolozane and tazobactam concentrations in human plasma and urine and to use this method to analyze samples from a human clinical study. Human plasma and urine samples were prepared by protein precipitation using a solution of acetonitrile, water and formic acid. Following

The arachidonic acid derivatives N-arachidonoylethanolamine (anandamide; AEA), 2-arachidonoylglycerol (2-AG), N-arachidonoyldopamine (NADA), 2-arachidonoylglycerol ether (noladine ether; 2-AGE) and O-arachidonoylethanolamine (virodhamine; VA) were identified as physiological components of the endocannabinoid (EC) system. In order to gain further profound knowledge about the different EC-induced physiological

Vitamin D has a potential role in protecting against cardiovascular disease (CVD). Serum 25-hydroxyvitamin D (25D) is the most widely used indicator of vitamin D status in the human body. 25D is estimated as total of 25-hydroxyvitamin D2 (25D2) and 25-hydroxyvitamin D3 (25D3). However, the presence of 3-epi-25-hydroxyvitamin D3 (3epi25D3) can affect 25D measurement. In this research a novel validated

The protruding (P) domain of the major capsid protein VP1 of norovirus (NoV) is the crucial element for immune recognition and host receptor binding. The heterologous P protein expressed by Pichia pastoris self-assembles into P particles. However, tag-free NoV protein purification schemes have rarely been reported due to the low isoelectric point of NoV proteins, which leads to highly competitive binding

A comparison of high-performance liquid chromatography (HPLC) and solid-phase extraction (SPE) methods is carried out for the simultaneous analysis of indoxyl sulfate and sodium butyrate in plasma using Phenyl (250 x 4.6 mm; 5 µm) and SunShell (150 x 4.6 mm, 2.6 µm) columns with mobile phases ammonium acetate (20 mM)-ACN (95:5, v/v) and water-ACN (90:10), respectively. The values of the retention,

Glycoengineering and biosimilarity are the key factors for growing, promising and progressive approaches in monoclonal antibodies development. In this study, the physicochemical stability of anti-CD20 rituximab (RTX); originator and biosimilar was compared to its glycoengineered humanized version; obinutuzumab (OBZ). An orthogonal stability-indicating protocol using a set of validated bioanalytical

The determination of the concentrations of urinary biomarkers of oxidative damage to DNA and RNA is difficult due to the low content of targets and the complex matrix of urine. A method using polystyrene/polypyrrole (PS/PPY) electronspun nanofibers as the adsorbent was introduced to the routine urinary treatment and determination of 8-OHdG and 8-oxoG for the first time. And 2-aminoethyl diphenylborate

Jasminum is an important genus in the olive family (Oleaceae), comprising about 200 species distributed all over the world. In the current study, the methanolic extract of Jasminum grandiflorum subsp. floribundum aerial parts and its respective fractions; dichloromethane and n-butanol fractions were analyzed using ultra-performance liquid chromatography coupled to high resolution mass (UPLC-HRMS) for

A new type of immunomagnetic bead based on the metal–organic framework materials (MOFs) and the magnetic core (Fe3O4) was prepared for analysis of the mycotoxins in food samples. The MOF conjugated with the monoclonal antibodies (McAbs) was coated on the surface of Fe3O4 beads by reversed-phase microemulsion method, which could purify deoxynivalenol (DON), zearalenone (ZEN), T-2, and HT-2 mycotoxins

Alzheimer's disease (AD) is a chronic and progressive neurodegenerative disorder. Rhodiola crenulata extract (RCE) has shown its protective effects on AD, however, the underlying mechanism is still unclear. In this work, serum lipidomics was conducted to reveal the action mechanism of RCE on AD by HPLC coupled with Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS). The animal

A simple and reliable method was developed and validated to determine the endocannabinoids anandamide (AEA) and 2-arachidonoylglycerol (2-AG) in rat brain samples by micro salting-out assisted liquid-liquid extraction combined with ultra-high performance liquid chromatography tandem mass spectrometry (SALLLE/UHPLC-MS/MS). The SALLE parameters (brain homogenate volume, salting-out agent, salt concentration

The aim of this study was to develop a new approach to sample preparation of biological material based on a combination of the Dried Blood Spot (DBS) method and capillary electrophoresis coupled with mass spectrometry (CE-MS) for the analysis of blood samples collected in vivo or post-mortem. The proposed approach allowed the identification of typical drugs from different groups, such as tricyclic

The field of affinity chromatography, which employs a biologically-related agent as the stationary phase, has seen significant growth since the modern era of this method began in 1968. This review examines the major developments and trends that have occurred in this technique over the past five decades. The basic principles and history of this area are first discussed. This is followed by an overview

A new HPLC method was developed for the enantio-separation and chiral recognition mechanism of quinolones (lomefloxacine, ofloxacine, primaquine and quinacrine) on Vancomycin CSP. The column used was Chirabiotic V column (150 × 4.6 mm, 5.0 μm) with two mobile phases i.e. (I) MeOH:ACN:H2O:TEA (50:30:20:0.1%) and (II) MeOH:ACN: H2O:TEA (70:10:20:0.1%) at 1.0 mL/minute flow rate with various UV detection

Catechol-O-methyltransferase (COMT) is a major drug metabolizing enzyme in humans. COMT expression is directedly associated with various mental diseases and cancers due to its essential role in catalyzing metabolic inactivation of endogenous catecholamines and catechol estrogens. However, a practical method to precisely measure COMT activities in biological samples is lacking. In the current study

Novel restricted access molecularly imprinted nanomaterials (RAMIPs) were successfully prepared on the surface of metal-organic frameworks (NH2-MIL-125) by surface-initiated atom transfer radical polymerization (SI-ATRP) technology. Then it was applied as a solid phase extraction (SPE) material in analysis of quinolones in bovine serum by HPLC detection. NH2[email protected] was empolyed as a sorbent

A quick and efficient method was optimized and validated to determine chlorpyrifos in biobeds using ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS). Chlorpyrifos was extracted from the matrix with 30 mL of a mixture of acetone, phosphoric acid and water 98:1:1 (v/v/v). After homogenization, centrifugation and filtration, 125 µL of the extract was evaporated

Hydrogen sulfide is a toxic gas involved in the regulation of some essential biological processes. A novel, precise, accurate and rapid method based on high-performance liquid chromatography with diode array detection for the determination of sulfide ions in human urine sample is proposed. The method involves the derivatization of sulfide with pyrylium salts – (2,4,6-triphenylpyrylium hydrogensulfate(VI)

Traditional Chinese medicine was widely used in China since its definite effects and therapy. The components of TCM were absorbed into the circle system as the format of prototypes or metabolites, which contributed to the therapy or side effects. Declaring the functional changes in this process was of great importance to the clinical applications. In this work, an integrated strategy based on metabolites’

Capsaicinoids, including capsaicin, dihydrocapsaicin and N-vanillylnonanamide have been identified as characteristic markers for gutter oil. In this study, the nanocomposite of graphene oxide–Fe3O4 (GO–Fe3O4) was synthesized by a co-precipitation method, and applied to magnetic solid phase extraction (MSPE) process. The capsaicin, dihydrocapsaicin and N-vanillylnonanamide extracted in gutter oil were

Long-term hyperglycemia associated with diabetes mellitus (DM) causes damage to various organs and tissues, including the eyes, kidneys, heart, blood vessels and nerves. Rubus Suavissimus S. Lee (RS), a shrub whose leaves are used in traditional Chinese medicine (TCM), has been shown to exert hypoglycemic effects in DM patients. However, the underlying mechanism is unclear. This was investigated in

Glyphosate is the highest volume herbicide used worldwide, and its main biodegradation product is aminomethylphosphonic acid (AMPA), both are listed as priority substances in the Human Biomonitoring for Europe initiative (HBM4EU) which aims at improving policy by filling knowledge gaps by targeted research. The objective of the current study was to advance the sensitivity of an existing gas-chromatography

A novel sulfonate-bonded covalent organic polymer (COPTPBA-BPDA@SA) with mixed-mode interactions of hydrophobic and cation-exchange was synthesized and exploited as sorbent for on-line solid-phase extraction (on-line SPE) of ß2-receptor agonists. The successful synthesis of COPTPBA-BPDA@SA was confirmed by the characterization of SEM, XPS and FT-IR. Due to the excellent mixed-mode extraction ability