AbstractTwo sensitive, selective and precise chromatographic methods have been established for concomitant quantification of ciprofloxacin HCl (CIP), fluocinolone acetonide (FLU) along with ciprofloxacin impurity A (CIP-imp A). The first method was thin-layer chromatography (TLC-densitometry) where separation was accomplished using TLC silica plates 60 G.F254 as a stationary phase and chloroform–methanol–33%ammonia

AbstractA reversed-phase high-performance liquid chromatography (RP-HPLC) method has been developed and validated for the identification and assay of Ivermectin, including the identification and estimation of its process-related impurities and degradation products in bulk drug substance of Ivermectin. Analytes were separated on a HALO C18 column (100 mm × 4.6 mm I.D., 2.7 μm particle size) maintained

AbstractA novel and reliable microextraction technique was used for the fast determination of benzene, toluene, ethylbenzene and xylenes (BTEX) from contaminated water without any extra steps for the preparation or extraction of the aqueous sample. Vacuum-assisted-total vaporization-solid-phase microextraction (SPME) eliminated one of the partitioning steps in conventional headspace SPME and caused

Fosamprenavir calcium is a protease inhibitor widely used in the treatment and prevention of human immunodeficiency virus and acquired immunodeficiency syndrome. This protease inhibitor serves as a prodrug of amprenavir, offering better oral bioavailability. Although this drug was approved by the FDA in 2003, there are few methods established for quantifying the stability for quality control analysis

Thirteen pairs of I3P enantiomers were screened using nine polysaccharide chiral stationary phases and three different mobile phases. The purification strategy for 13 pairs of I3P enantiomers were designed and optimized considering enantiomeric purity and enrichment of isomers. Out of 13 I3P derivatives which were screened using supercritical fluid chromatography, 10 derivatives displayed excellent

For the quantification of resveratrol (RV) in the Wistar rat skin, an ultra-performance liquid chromatography-mass spectrometric (UPLC-MS/MS) method was developed and validated on ACQUITY UPLC BEH C18 column (1.7 μm). The mobile phase ratio of methanol (A) and 2% formic acid (B) (ratio 10: 90% v/v, 80: 20 v/v) at isocratic elution with flow rate 0.3 mL/min, and run time 3 min was used for analysis

A simple high performance liquid chromatography (HPLC) method was developed and validated for the determination of coumarin-3-carboxylic acid analogues (C3AA) in rat plasma and a preliminary study on pharmacokinetics. Ferulic acid (FA) was used as the internal standard substance, and coumarin-3-carboxylic acid (C3A) was used as a substitute for quantitative C3AA. After protein precipitation with methanol

Saccharides are one of the most important biomoleculars in the world, which are responsible for various roles in living organisms. In this work, a combined use of mass spectrometry (MS) together with supercritical fluid chromatography (SFC) was applied for the separation of eight saccharides. A satisfactory separation was achieved within 15 min on a Unitary Diol column using 10 mM ammonium acetate

AbstractA novel stability-indicating isocratic reverse phase high-performance liquid chromatographic method was developed for the quantitative determination of perampanel in the presence of degradation products and its process-related impurities. Good resolution was achieved between the peaks corresponding to process-related impurities and degradation products from the analyte using Shim-pack GIST

The fixed-dose combination (FDC) of montelukast sodium (MLS) and bilastine (BIL) is used for monotherapy in the patient with seasonal allergic rhinoconjuctivitis and asthma. According to the upcoming ICH (International Council for Harmonization) Q14 guideline, the development of the analytical method by the implementation of the Analytical Quality by Design (AQbD) approach based on principles of Quality

A novel isocratic stability-indicating chromatographic method was developed, optimized and validated using Design-Expert® following ICH guidelines for the quantification of Timolol maleate (TM). The intrinsic stability of TM was assessed by force degradation studies, which concluded no extensive degradation except under alkaline and oxidative conditions. TM was quantified accurately in the surfactant-based

AbstractA simple, accurate, rapid and sensitive reversed-phase high-performance liquid chromatography (RP-HPLC) method was established for determination of a novel non-vitamin K antagonist oral anticoagulant drug, betrixaban, and its co-administered calcium-channel blocker drug, lercanidipine, in pharmaceutical formulations and biological fluids. The proposed HPLC method was the first chromatographic

Sofosbuvir and daclatasvir are co-formulated as directly acting antiviral agents used for treatment of hepatitis C virus. Two chromatographic methods were developed for their determination; the first one is an Reversed phase-high performance liquid chromatography (RP-HPLC) method, in which the separation was performed on C8 Zorbax® SB column (4.6 × 250 mm, 5 μm) using acetonitrile:water:0.05 M phosphate

The pomace of sea buckthorn berries is usually discarded when transforming into nonalcoholic or alcoholic beverages, jellies, jams, juices, candies and dairy products. Here, we established a promising approach for one step separation of five flavonoids from the waste pomace of sea buckthorn berries through counter-current chromatography. The crude extract of waste pomace of sea buckthorn berries after

A simple, sensitive and accurate reversed-phase high-performance liquid chromatography (RP-HPLC) method was established for the determination of piperidine and piperidine hydrochloride in artane, using pre-column derivatization with 4-toluenesulfonyl chloride. The RP-HPLC method was carried out on a Inertsil C18 column (250 × 4.6 mm I.D.) maintained at 30°C. The mobile phase consisted of water with

A rapid and sensitive LC-MS/MS method was developed and fully validated for the determination of obeticholic acid in human plasma. Glimepiride was used as internal standard. For this method, liquid–liquid extraction was performed to extract analyte from the plasma samples. Chromatographic separation was performed on a C18 (2.1 × 50 mm, 2.7 μm, Agilent) column with isocratic elution using water containing

Chromatography is one of the most popular methods for the separation of compounds in modern pharmaceutical industry and science. Despite the extensive use of the reversed phase chromatography in analytical and preparative applications, the normal phase adsorption chromatography has a special place in purifying post-reaction mixtures or the separation of natural extracts, especially in wet load mode

AbstractDeep eutectic solvents (DESs) are regarded as promising solvents to extract chemicals from plant materials. In this study, a DES-based microwave-assisted extraction (MAE) method was developed for the chromatographic analysis of four bioactive flavonoids in Spirodela polyrrhiza. Chromatographic separation was achieved on a Promosil C18-column. Prior to the HPLC analysis, the flavonoids were

A chemometrics-oriented green ultra-performance liquid chromatography-mass spectrometry/mass spectrometry method was developed and validated for the first-time simultaneous estimation of capecitabine (CAP) and lapatinib (LPB) along with imatinib (as internal standard (IS)) in rat plasma. Analytes were extracted using ethyl acetate as the liquid-liquid extraction media. In the pre-development phase

A green and simple method, dynamic microwave-assisted micelle extraction coupled with cloud point preconcentration, was developed for the determination of triazine herbicides in soil samples. The method has the advantages of those two extraction procedures, which could eliminate the interferences from complex soil samples greatly. Non-ionic surfactant Triton X-114 aqueous solution used as extraction

AbstractA validated RP-HPLC method was developed for the estimation of paracetamol, caffeine, metoclopramide and ergotamine simultaneously in bulk and pharmaceutical formulation. The method was extended for the determination of two paracetamol genotoxic and nephrotoxic impurities and degradation products namely p-aminophenol and 4-chloroacetanilide. Separation was done on octadecyl column (15 cm ×

Traditional Chinese medicines (TCMs) have been considered as important alternative therapeutics because of their significant medicinal benefits in specific diseases. Chinese herb formula is characterized by a vast molecule that differs in routine medicines. Due to TCMs chemical complexity, proper quality control has been a great challenge. Choosing the appropriate method to identify and qualify these

AbstractPolygoni Multiflori Radix Praeparata (PMRP) is used as Chinese herbal medicine with long history. However, reports about PMRP hepatotoxicity have increased recently, and producing area might be one reason. This article aims to figure out the relationship between producing area and hepatotoxic ingredients in PMRP. HPLC fingerprint for PMRP was established and the contents of gallic acid, trans-stilbene

To support a phase III randomized trial of the multi-targeted tyrosine kinase inhibitor cabozantinib in neuroendocrine tumors, we developed a high-performance liquid chromatography mass spectrometry method to quantitate cabozantinib in 50 μL of human plasma. After acetonitrile protein precipitation, chromatographic separation was achieved with a Phenomenex synergy polar reverse phase (4 μm, 2 × 50 mm)

AbstractNeratinib, a tyrosine kinase inhibitor, was very recently approved by USFDA in 2017 as an anticancer drug to treat of HER2 positive breast cancers. The present work provides an account on the development of a validated bioanalytical UPLC–MS/MS method for quantification of neratinib and internal standard (imatinib) in rat plasma and tissue homogenates. A UPLC having a 100 mm C18 column (1.7 μm

Sinomenii Caulis (QingFengTeng) and Ramulus Cinnamomi (GuiZhi) are traditional Chinese drugs that have been used for anti-inflammation. In this study, the team plans to find out the material basis of a Chinese herb combination composed of the two herbs with different ratios.

AbstractRifaximin, an antimicrobial used for the treatment of various diseases, lacks analytical methods in official compendia for evaluation of the final product. This paper presents an eco-friendly protocol for rifaximin tablets by high performance liquid chromatography coupled with mass spectrometry (HPLC-MS). The method was completely validated according to the International Conference on Harmonization

A simple, precise, rapid and accurate UFLC method has been developed with due validation for the simultaneous estimation of Amlodipine besylate and Celecoxib in rat plasma. The separation has been taken place by C18 Eclipse plus column at 1ml/min flow rate. The mobile phase comprises of 20 mM sodium acetate buffer of pH 4.5 adjusted with glacial acetic acid and methanol (30:70% v/v). The effluents

The volatile compound 6-methyl-5-hepten-2-one (MHO) is an important chemical intermediate and flavor component derived from carotenoid during fruit metabolism, which is important factor impacting consumer-liking. Fruit has complex matrix and is difficult to be purified during MHO analysis. A rapid liquid–liquid extraction-gas chromatography–mass spectrometry (LLE-GC–MS) method was developed for effective

An efficient and rapid liquid chromatographic method was developed for the separation of carotenoids and their geometrical isomers in tomato products using a core C30 column of 2.6 μm particles with gradient elution of tert-butyl-methyl-ether in 2% water in methanol. Excellent separation of the major carotenoids such as lycopene, β-carotene and lutein as well as their geometrical isomers and oxygen-containing

The anticancer effects of rosmarinic acid (RA) are a hotspot of current research. In order to enhance its pharmacological activity, N-substituted RA was prepared, and it has been shown to exhibit notable antitumor effects. In order to elucidate the underlying mechanisms of action, pharmacokinetic analysis is necessary. In the present study, liquid chromatography-tandem mass spectrometric method, was

A selective, sensitive and robust chiral analytical method was developed for the quantification of Brivaracetam (BRV) and its three isomers. Systematic chiral chromatographic elution process was executed in different modes on chiral columns of polysaccharide based to attain the finest condition. The analytical method was developed by utilizing immobilized polysaccharide chiral column (CHIRALPAK IG-U)

A method for the determination of 15 + 1 European priority polycyclic aromatic hydrocarbons (EUPAHs) in smoked meat samples by saponification/solid-phase extraction and gas chromatography-mass spectrometry has been developed. Both saponification and solid-phase extraction conditions were optimized, which lead to shorter sample preparation time and excellent sensitivity and selectivity. The optimal

Pomegranate flowers (PFs) were reported to possess various biological activities such as antidiabetic, anti-inflammatory and hepatoprotective activities, and using to treat diabetes. Although chemical constituents and pharmacological activities of PFs have been studied, unfortunately, there was no report on the pharmacokinetic profile of PFs in vivo. In this study, a selective high-performance liquid

An automated sorbentless cryogenic needle trap device (ASCNTD) was developed for the extraction of organic volatile impurities (OVIs) from solid pharmaceuticals prior to their determination by gas chromatography (GC). In this method, a new set up was designed and used to extraction of several OVIs from ceftazidime, ceftriaxone sodium and amoxicillin. For this purpose, a proper amount of the sample

Liquid chromatography interfaced with mass spectroscopy (LC-MS) is a sensitive and effective analytical method that combines high-resolution separation as well as specific mass detection of impurities in formulated products and as well as in active pharmaceutical ingredient (API). In this study, LC-MS/MS was used to determine impurities formed during the stability period of Efinaconazole (EFZ, a triazole

3-(Methylene-bis(1',4'-phenylene) dicarbamate-2,3-bis(3,5-dimethylphenylcarbamate)-amylose)-2-hydroxylpropoxy-propylsilyl-appended silica particles (DMP-AM-HPS), a new type of 2, 3-regioselectively substituted amylose-immobilized chiral stationary phase (CSP) for high-performance liquid chromatography (HPLC), have been prepared by treatment of 3-(2,3-dihydroxyl-propoxy)-propylsilyl silica particles

The conversion of azathioprine (AZA) to active 6-thioguanine nucleotides (6-TGN) is essential for its clinical efficacy; however, another metabolite formed, 6-methylmercaptopurine (6-MMP), is related to hepatotoxicity. Blood samples were collected from 37 patients under AZA's treatment, and a new HPLC-UV method was validated and applied for simultaneous quantification of 6-TGN and 6-MMP in erythrocytes

A simple, rapid and novel method has been developed and validated for determination of 16 phthalates in marine sediment samples by gas chromatography coupled to mass spectrometry. Freeze dried samples were first ultrasonic extraction by n-hexane:methylene chloride (1:1, v/v) and n-hexane:ethyl acetate (1:1, v/v) and followed by dispersive solid-phase extraction cleanup. The linearity of this method

Electrospun polyacrylonitrile/clinoptilolite (PAN/CP) nanofibers were used to extract polycyclic aromatic hydrocarbons (PAHs) (acenaphthene, acenaphthylene, naphthalene, and phenanthrene) from water samples by solid-phase microextraction (SPME). The target PAHs was detected and quantified by gas chromatography equipped with a flame ionization detector. The PAN/CP fibrous coating with uniform morphology

Ethyl acetate potentially contains formaldehyde and acetaldehyde as impurities. Ephedrines (ephedrine and pseudoephedrine) react with these aldehydes to give oxazolidines. The purpose of this study is to elucidate the effects of aldehydes in ethyl acetate on the analysis of ephedrines by gas chromatography/mass spectrometry (GC/MS). Ephedrines dissolved in a basic solution were extracted with five

An efficient method for simultaneous extraction, purification and determination of six lignans in Schisandra chinensis Baill was developed by employing matrix solid-phase dispersion (MSPD) extraction followed by HPLC-UV determination analysis. Several sorbent and desorption solvent that affected the extraction yield of lignans were investigated; neutral alumina and absolute ethanol were selected as

Ceftriaxone sodium is a widely used antimicrobial, which is only available as a lyophilized powder. The presence of methods for evaluating the quality of this product is very important and helps to ensure its effectiveness, in addition to contributing to the fight against bacterial resistance. Therefore, a clean and sustainable high-performance liquid chromatography (HPLC) method has been developed

A high-performance thin-layer chromatographic (HPTLC) method has developed for the selective detection of a diuretic drug, triamterene (TRIAM), in pure form, tablets and human plasma. The method was based on chromatographic separation of TRIAM using HPTLC plates, precoated with silica gel, and a mobile phase consisted of ethyl acetate: dimethylformamide: ammonia (7.0: 2.7: 0.3, by volume). The native

Telmisartan is an antihypertensive drug and several FDC products of telmisartan are available in the market for the treatment of hypertension. The multipurpose reverse-phase high-performance liquid chromatography (RP-HPLC) method has been developed and validated as economical and eco-friendly alternative to numerous published chromatography methods for synchronous estimation of FDC of telmisartan to

Non-depolarizing neuromuscular blocking agent Rocuronium bromide was quantified in drug substance and drug product using reversed-phase liquid chromatographic method. Forced degradation studies were conducted for Rocuronium bromide in drug substance under acidic (2MHCl), basic (2MNaOH), oxidative (3% H2O2), thermal (135°C) and photolytic (254 nm) stress conditions. An Agilent H12 C18 column was used

This research presents a green synthetic pathway for the preparation of a new biosorbent and eco-friendly extraction process of three phthalate esters: dimethyl phthalate, di-butyl phthalate and benzyl butyl phthalate, from cosmetics and baby care products. Dispersive solid-phase extraction was used based on a new core-shell biomass/sorbent; chitosan-loaded lawsone. The proposed method provides fortunate

A simple, fast and extremely sensitive for estimating Pimavanserin in human (K2EDTA) plasma using ultra high-performance liquid chromatography combined with tandem mass spectrometry (UHPLC–MS/MS) was newly developed and validated. Sample extraction was accomplished using a partition liquid extraction (LLE—liquid–liquid extraction) procedure utilizing extraction solvent, methyl tertiary butyl ether

AbstractScrophulariae Radix is one of the widely used traditional Chinese medicines. In this study, a high-performance liquid chromatography coupled with triple quadrupole-linear ion trap mass spectrometry method was established for the simultaneous determination of multiple bioactive constituents including four iridoid glycosides, two phenylpropanoid glycosides, six organic acids, 11 nucleosides and

A new methodology was proposed to determine the dispersive component of the surface energy |${\gamma}_s^d$| of a solid taking into account the effect of the temperature on the surface area of n-alkanes, methylene group (⁠|${a}_{- CH2-}$|⁠) and polar molecules, thus defeating the method used by Dorris–Gray Schultz et al. We determined the correct |${\gamma}_s^d$| of the surface energy, the specific

AbstractMultiresponse optimization approach to develop a simple isocratic, highly sensitive and accurate HPLC method for the simultaneous determination of Efavirenz, Atazanavir, Lopinavir and Ritonavir in human blood plasma along with carvedilol as an internal standard. Optimized the factors (ACN, buffer concentration and flow rate) effecting and interacting with the responses (k1, Rs2,1, Rs3,2 and

We investigated the dual retention mechanism in thin-layer chromatography taking place on three stationary phases of different polarity (C-18, plain silica gel and DIOL) and using binary mobile phases composed of acetonitrile as the main component and water, or methanol as a modifier. As the test analytes, we selected a set of 12 compounds of pharmaceutical importance and considerably different chemical

AbstractBorage oil that is extracted from (Borago officinalis Linn.) is a well-known medicinal plant having various medicinal benefits. In this work, an affordable, simple, reliable, rapid and easily accessible high-performance thin-layer chromatography (HPTLC) method was developed for the estimation of gamma-linolenic acid (GLA) in borage oil. HPTLC method employs thin-layer chromatography (TLC) aluminum

AbstractRavuconazole (RAV) is a triazole antifungal with broad spectrum and a novel alternative in the treatment of systemic fungal infections. A stability-indicating method by high-performance liquid chromatography–diode array detection was developed and fully validated to assay ravuconazole in the presence of its degradation products. Separation was achieved with a Sunfire C18 column (250 mm × 4

  Qilong capsule (QLC) is a well-known Traditional Chinese Medicine, and it has a long history for the treatment of ischemic stroke. Its major ingredients are saponins, such as paeoniflorin, amygdalin and calycosin-7-glucoside, contributing to vasodilation function. In this study, a simple, rapid and sensitive high-performance liquid chromatography-tandem mass spectrometry method was developed to determine

A sensitive and selective gas chromatography-tandem mass spectrometry method was developed for the identification and quantification of five potential genotoxic impurities (PGIs), i.e., chloromethane, 2-chloropropane, 2-bromopropane, 4-chloro-1-butanol and diethyl sulfate, in abiraterone acetate. The method was validated according to the International Council for Harmonisation (ICH) guidelines. The

AbstractFor the quantification of flurbiprofen in rat plasma, a simple UPLC-MS/MS method with high sensitivity and short retention time for flurbiprofen was developed and validated using specific parameters. Etodolac was used as internal standard. The transitions (precursor to the product) of flurbiprofen and internal standard were obtained using the electrospray ionization in the negative ion multiple

A high-performance thin-layer chromatographic method was developed and validated for the concurrent determination of simeprevir (SMV) and sofosbuvir (SOF). The chromatographic separation was attained on silica gel 60 F254 as stationary phase and ethyl acetate–hexane–methanol (5.0:4.0:1.0, v/v/v) as developing solvent with UV detection at 273 nm. The RF values were 0.67±0.02 and 0.43±0.02 for SMV and

AbstractFirst analytical methods were herein developed for determination of pregabalin (PGB) and amitriptyline (AMT) as an active binary mixture used for management of neuropathic pain whether in pure forms or in human biological fluids (plasma/urine). First method is green high-performance liquid chromatography-diode array detector (HPLC–DAD) after derivatization of PGB with ninhydrin (NIN) on a reversed-phase

A rapid, simple and sensitive liquid chromatography tandem mass spectrometry method for the determination of methohexital in human whole blood was developed and validated. Ethyl acetate/n-hexane (9:1) was used as extraction solvent while aprobarbital was used as internal standard. Methohexital was recovered by liquid–liquid extraction from 100 μL of human whole blood. The mobile phase was water-acetonitrile