Abstract:
:Due to severe chelating effect caused by N-hydroxylpyridone group of ciclopirox, there is no published direct HPLC or LC/MS/MS method for the determination of ciclopirox in any in vitro or in vivo matrix. Instead, the time-consuming pre-column derivatization methods have been adapted for indirect analysis of ciclopirox. After overcoming the chelating problem by using K(2)EDTA coated tubes, a direct, sensitive and high-throughput LC/MS/MS method was successfully developed and validated to determine the amount of ciclopirox that penetrated across the nail plate during in vitro nail penetration studies. The method involved adding a chemical analog, chloridazon as internal standard (IS) in K(2)EDTA coated tubes, mixing IS with ciclopirox in a 96-well plate and then proceeding to LC/MS/MS analysis. The MS/MS was selected to monitor m/z 208.0-->135.8 and 221.8-->77.0 for ciclopirox and IS, respectively, using positive electrospray ionization. The method was validated over a concentration range of 8-256 ng/mL, yielding calibration curves with correlation coefficients greater than 0.9991 with a lower limit of quantitation (LLOQ) of 8 ng/mL. The assay precision and accuracy were evaluated using quality control (QC) samples at three concentration levels. Analyzed concentrations ranged from 101% to 113% of their respective nominal concentration levels with coefficients of variation (CV) below 10.6%. The average recovery of ciclopirox from nail matrix was 101%. The validated method was successfully used to analyze the ciclopirox formulation and in vitro nail penetration samples.
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
Bu W,Fan X,Sexton H,Heyman Idoi
10.1016/j.jpba.2009.08.019subject
Has Abstractpub_date
2010-01-05 00:00:00pages
230-5issue
1eissn
0731-7085issn
1873-264Xpii
S0731-7085(09)00523-8journal_volume
51pub_type
杂志文章abstract::A rapid and simple reversed-phase high performance liquid chromatography (HPLC) method for the quantitation of colistimethate sodium in pharmaceutical formulations has been developed. The chromatographic separation was performed using a Phenomenex Kinetex XB-C18 column with gradient elution using a mobile phase contai...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2017.04.021
更新日期:2017-08-05 00:00:00
abstract::A sensitive and specific method for the determination of bifendate in human plasma was developed, based on high-performance liquid chromatography (HPLC)-mass spectrometry (MS). The samples were extracted from plasma with diethyl ether, followed by separation and evaporation after addition of internal standard diazepam...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 临床试验,杂志文章
doi:10.1016/j.jpba.2005.08.007
更新日期:2006-03-03 00:00:00
abstract::Guggulipid is known to be useful for hypercholesterolemia, arthritis, acne, and obesity. These activities are attributed to its two principal isomeric active constituents, viz., E- and Z-guggulsterones. There are several side effects reported for guggulipid, which include widespread erythematous papules in a morbillif...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2020.113275
更新日期:2020-07-15 00:00:00
abstract::A sensitive reverse phase high performance liquid chromatography-electrospray ionization-mass spectrometry (RP-HPLC-ESI-MS) method has been developed and validated for the determination of hydromorphone in human plasma using naloxone as the internal standard (IS). After alkalization with saturated sodium bicarbonate, ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2011.11.012
更新日期:2012-03-05 00:00:00
abstract::DuP 747, a selective kappa agonist analgesic, was found to have at least two polymorphic forms, and this was confirmed by X-ray powder diffraction. DSC and thermomicroscopic studies indicated the polymorphic pair to be monotropic. Solubility studies suggested the relative stability of the two forms to be similar. The ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(94)e0002-i
更新日期:1994-06-01 00:00:00
abstract::A simple liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for simultaneous quantification of aripiprazole and its active metabolite, dehydro-aripiprazole, in human plasma. Stable isotopically labeled aripiprazole, aripiprazole-D8, has been used as the internal standard ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2017.12.049
更新日期:2018-03-20 00:00:00
abstract::Supercritical Fluid Chromatography (SFC) has known a strong regain of interest for the last 10 years, especially in the field of pharmaceutical analysis. Besides the development and validation of the SFC method in one individual laboratory, it is also important to demonstrate its applicability and transferability to v...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2018.08.042
更新日期:2018-11-30 00:00:00
abstract::With high morbidity and mortality, urinary bladder cancer (BC) ranks fifth among common cancers globally. The inherent limitations of urine cytology and cystoscopy, and marginal enhancements in the rate of survival promt us to develop surrogate serum based metabolic biomarkers of screening, identification, and follow-...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2020.113134
更新日期:2020-05-10 00:00:00
abstract::Besides several known impurities in cimetidine, two additional compounds at levels below 0.1% were detected by ion-pair reversed-phase high-performance liquid chromatography (HPLC). The impurities were isolated from crude cimetidine using normal-phase preparative HPLC. 1H and 13C NMR and mass spectrometric investigati...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(96)01815-8
更新日期:1996-10-01 00:00:00
abstract::This paper describes a method for quantification of d-amphetamine and diphenhydramine in beagle dog plasma by organic solvent field-amplified sample stacking (FASS)-capillary zone electrophoresis (CZE), using amlodipine as the internal standard. The separation was carried out at 25 °C in a 40.2 cm × 75 μm fused-silica...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2018.04.040
更新日期:2018-07-15 00:00:00
abstract::The objective of this study was to investigate the use of transmission hard X-ray nano-computed-tomography (nano-CT) for characterization of the pore structure and drug distribution in poly (lactic-co-glycolic acid) (PLGA) microspheres encapsulating bovine serum albumin and to study the correlation between drug distri...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2015.04.017
更新日期:2015-08-10 00:00:00
abstract::The public concern and increasing awareness of herbal medicines calls for methods available to assure quality and authenticity. In the present study, a novel strategy combing 1H nuclear magnetic resonance (1H NMR) spectral analyses coupled with chemometrics was developed and validated to allow comprehensive analysis a...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2018.08.003
更新日期:2018-10-25 00:00:00
abstract::Azurin p28 (NSC745104) is a 28 amino acid peptide fragment that inhibits proliferation of human solid and hematological malignancies in vitro and in vivo by reducing proteasomal degradation of oncogene p53. The present study aimed at developing a novel and fast liquid chromatography/tandem mass spectrometry (LC/MS/MS)...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2010.06.006
更新日期:2010-12-01 00:00:00
abstract::Meldonium is a drug exhibiting cardioprotective and anti-ischemic effects. Due to its potential performance-enhancing benefit in sports, meldonium was added to the World Anti-Doping Agency list of prohibited substances in 2016. Since then, a high number of adverse analytical findings reported on meldonium has question...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2018.08.053
更新日期:2018-11-30 00:00:00
abstract::Novel approaches to the development of analytical procedures for monitoring incoming starting material in support of chemical/pharmaceutical processes are described. High technology solutions were utilized for timely process development and preparation of high quality clinical supplies. A single robust HPLC method was...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(00)00333-2
更新日期:2000-08-15 00:00:00
abstract::A novel sensor based on a modification of glassy carbon electrode (GCE) with NH2-functionalized multi-walled carbon nano-tubes (NH2fMWCNTs) is reported and its applicability to the electrochemical sensing of Propafenone (PPF) demonstrated. The electrochemical catalytic activity was also utilized as a sensitive detecti...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2019.06.026
更新日期:2019-09-10 00:00:00
abstract::In this work, dissociation constants values of seven beta lactam antibiotics in water and acetonitrile-water mixtures using spectrophotometric and reversed phase liquid chromatography methods were determined. The dissociation constant values of these compounds were calculated by NLREG and STAR programs. Aqueous pK(a) ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2012.06.023
更新日期:2012-12-01 00:00:00
abstract::Docetaxel is a semi-synthetic taxane with cytotoxic anti-neoplastic activity and, currently used as anticancer agent in several types of cancer. Docetaxel is highly bound to plasma proteins, and this significantly determines its clearance and activity. Therefore, measurement of free docetaxel in plasma is pharmacologi...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2015.08.025
更新日期:2016-01-05 00:00:00
abstract::A fast and simple method for the quantitative analysis of monoclinic (form I) and orthorhombic (form II) paracetamol was developed, based on FT-Raman spectroscopy and PLS regression. Three different preprocessing algorithms, namely orthogonal signal correction (OSC), standard normal variate transformation (SNV) and mu...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2006.07.032
更新日期:2007-01-17 00:00:00
abstract::A study was conducted to investigate the quality of reference substances which were produced long before the introduction of advanced analysis and purification techniques. The quality and antimicrobial activity of WHO and EP oxytetracycline, doxycycline, colistin and spiramycin reference standards were assessed. The o...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2009.09.031
更新日期:2010-02-05 00:00:00
abstract::A simple, rapid and efficient microextraction method for the extraction and determination of some 2-pyrazoline derivative compounds in aqueous samples was developed. Microliter volumes of 1-undecanol were delivered to the surface of the aqueous sample and the sample was agitated for a desire time. The sample vial was ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2008.07.029
更新日期:2008-12-01 00:00:00
abstract::In this paper, a simple, rapid and high-throughput fluorescence polarization immunoassay (FPIA) based on polyclonal antibodies (PAb) is described for the determination of glycocholic acid (GCA) in human urine. Three fluorescein-labeled GCA (tracers) with different structures and spacer bridges were synthesized and pur...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2018.06.023
更新日期:2018-09-05 00:00:00
abstract::A micro-bore liquid chromatographic method was developed for the simultaneous determination of benazepril hydrochloride and hydrochlorothiazide in pharmaceutical dosage forms. The use of a BDS C-18 micro-bore analytical column, results in substantial reduction in solvent consumption and increased sensitivity. The mobi...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(99)00195-8
更新日期:1999-12-01 00:00:00
abstract::In the present work, oregano leaves (Origanum vulgare L.) are explored as natural source of nutraceuticals with antioxidant activity. To do this, subcritical water extraction (SWE), a new environmentally friendly technique, is employed as extraction procedure and HPLC coupled to DAD is used for the chemical characteri...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2006.01.018
更新日期:2006-08-28 00:00:00
abstract::Hernandezine, a novel anticancer AMPK activator, is a major active constituent of Thalictrum Ranunculaceae. A simple, specific and sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS) method has been developed and validated for the quantification of hernandezine in rat plasma and tissues after intraveno...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2017.03.038
更新日期:2017-07-15 00:00:00
abstract::This report describes the development of a potency ELISA using a peptide derived from the motavizumab binding epitope of respiratory syncytial virus (RSV) F-protein. Motavizumab is an antibody therapeutic studied for the prevention of RSV disease. It binds to the RSV glycoprotein F (F-protein), blocking the ability of...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2010.09.008
更新日期:2011-02-20 00:00:00
abstract::A simple HPLC-UV method was established for the determination of orientin in plasma and different tissues of rat (heart, liver, spleen, lung, kidney, brain, stomach and small intestine). The separation was achieved by HPLC on a C(18) column with a mobile phase composed of acetonitrile-0.1% acetic acid (20:80, v/v), UV...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2008.01.035
更新日期:2008-06-09 00:00:00
abstract::In order to study 2'-deoxycytidine (2'-dCyd) as a possible prognostic marker in cancer chemotherapy, an enzyme immunoassay (EIA) was developed. 2'-dCyd as a hapten was succinylated and two omicron-monosuccinyl-2'-dCyd's were purified by high performance liquid chromatography and identified by mass spectrometry and 1H-...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(96)01982-6
更新日期:1997-06-01 00:00:00
abstract::Ten free fatty acids namely lauric acid, myristic acid, pentadecanoic acid, palmitoleic acid, palmitic acid, linoleic acid, oleic acid, stearic acid, docosanoic acid and lignoceric acid and four free sterols including ergosterol, cholesterol, campesterol and beta-sitosterol in natural (wild) Cordyceps sinensis, Cordyc...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2009.02.025
更新日期:2009-07-12 00:00:00
abstract::A simple and rapid method for the determination of partition constants in the n-octanol/water system is presented. The substance under study is dissolved in n-octanol or water, and injected into a stream of the corresponding phase. Liquid-liquid segmented flow is utilized for equilibration of the two phases and after ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(94)00107-3
更新日期:1994-12-01 00:00:00