Abstract:
:Recently direct plasma injection LC/MS/MS technique has been increasingly used in pharmaceutical research and development due to the demand for higher throughput of sample analyses. In this work, two on-line extraction methods including high flow LC/MS/MS and high flow column switching LC/MS/MS were investigated. The evaluations were conducted and focused on their performances with respect to peak responses, separation efficiency, and signal to-noise ratio in a multiple-component LC/MS/MS assay. Two HPLC pumps were used-with one for high flow delivery and one for gradient elution. A CTC autosampler was used to inject plasma samples. High flow LC was achieved by the use of 4 ml/min flow rate on a 1 x 50 mm Waters Oasis column. A 2 x 100 mm YMC column was coupled via a column-switching valve. The extracted analytes were analyzed in multiple-reaction-monitoring (MRM) mode using a triple quadrupole MS/MS. As a rapid and simple procedure, vortex-mixing plasma and internal standard directly in sample vials completed sample preparation. The high flow column switching method (two-column system) provided sharper peak shape than the conventional high flow method. This effect increased analyte signal-to-noise ratio and sensitivity. Narrower peak width resulted in much better separation efficiency, which was required for multiple compound (N-in-1) analysis. A 2 mm I.D. column resulted in better peak shape and resolution than using a smaller I.D. column. The selected method achieved acceptable recoveries for most of the compounds tested, and it was successfully applied to a 10-in-1 pharmacokinetic (PK) study. The results showed that the dynamic range, lower limit of quantitation, assay accuracy and precision were acceptable for all compounds. Rapid sample preparation eliminated labor intensive and time consuming processes and improved productivity. This high throughput on-line extraction high flow column switching method has been proven particularly useful for multiple component analysis in PK studies.
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
Zeng H,Wu JT,Unger SEdoi
10.1016/s0731-7085(01)00541-6subject
Has Abstractpub_date
2002-03-01 00:00:00pages
967-82issue
6eissn
0731-7085issn
1873-264Xpii
S0731708501005416journal_volume
27pub_type
杂志文章abstract::The crystallographic texture, i.e. the preferred orientation of crystallites of delta-mannitol samples, has been experimentally determined by pole figure analysis. The pole figures were measured with an X-ray diffraction texture goniometer. It was found that already the uncompressed delta-mannitol powder sample was sl...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2004.07.019
更新日期:2004-11-15 00:00:00
abstract::Charge variant profiling of therapeutic proteins is required by the International Council for Harmonisation guidelines and is traditionally performed by capillary electrophoresis or ion exchange chromatography. Recently, improvements in the hyphenation of capillary electrophoresis with mass spectrometry and the introd...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2020.113218
更新日期:2020-06-05 00:00:00
abstract::The pharmacokinetics and pharmacodynamics (PK/PD) of imidaprilat, an active metabolite of imidapril, a new angiotensin-converting enzyme (ACE) inhibitor, were investigated. Imidapril was infused subcutaneously for 4 weeks via an osmotic pump implanted under the skin in the back of male spontaneously hypertensive rats ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(96)02015-8
更新日期:1997-08-01 00:00:00
abstract::A new procedure for kinetic determination of paracetamol in pharmaceuticals is proposed. The method is based on potentiometric monitoring of the concentration perturbations of the matrix reaction system being in a stable non-equilibrium stationary state close to the bifurcation point. In the case considered as the mat...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2005.11.043
更新日期:2006-05-03 00:00:00
abstract::In the series of our previous reports, we showed that some cancer cell lines specifically express polylactosamine-type N-glycans and such glycans were often modified with fucose and sulfate residues. To confirm the proteins expressing these glycans, glycopeptide mixture obtained by digestion of whole protein fractions...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2012.06.035
更新日期:2012-11-01 00:00:00
abstract::A new methodology based on Nuclear Magnetic Resonance (NMR) was developed to determine plasma protein binding (PPB) of drug candidates in drug discovery programs. A strong correlation was found between the attenuation of NMR signals of diverse drugs in the presence of different plasma concentrations and their fraction...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2019.01.049
更新日期:2019-04-15 00:00:00
abstract::CE coupled with UV detection was assessed as a possible platform for the chemical identity and purity analysis of positron emission tomography (PET) tracers using [(18)F]FAC and [(18)F]FLT as examples. Representative samples containing mixtures of the tracers plus well-known impurities, as well as real radioactive sam...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2014.01.023
更新日期:2014-06-01 00:00:00
abstract::Two analogs of sildenafil (compounds 1 and 2) were detected in three powder products acquired from online drug markets during an LC-UV-MS analysis of psychotropic drugs. Their structures were established by high-resolution mass spectrometry and NMR spectroscopy. Compound 1 was identified as 5-(5-(3,5-dimethylpiperazin...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2017.09.025
更新日期:2018-01-30 00:00:00
abstract::The aim of this study was to evaluate the relationship between serum levels of beta-trace protein (BTP), a low molecular weight (MW) protein, and glomerular filtration rate (GFR). GFR and serum levels of BTP, and for comparison creatinine (Creat), cystatin C (Cys) and beta 2-microglobulin (beta 2M), were measured in 6...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(03)00215-2
更新日期:2003-08-08 00:00:00
abstract::A sensitive and stereospecific high-performance liquid chromatography (HPLC) method for the quantitation of ketoprofen enantiomers in human serum was developed. The assay involves the use of an octadecylsilane solid-phase extraction for serum sample clean-up prior to HPLC analysis. Chromatographic resolution of the ke...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(97)00161-1
更新日期:1998-05-01 00:00:00
abstract::A sensitive and specific ultra-performance liquid chromatography tandem mass spectrometry (LC-MS/MS) method has been developed for the determination of nicousamide in human plasma. This method has also been validated in terms of selectivity, linearity, lower limit of quantification (LLOQ), accuracy, precision, stabili...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2013.01.025
更新日期:2013-04-15 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::Diclofenac (DCF) is the most widely prescribed non-steroidal anti-inflammatory drug in the world and it has been detected in drinking and surface waters. In this paper, the effect of chlorination process on DCF in aqueous solutions was investigated and the structures of 14 isolated degradation by-products (DPs), of wh...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2020.113762
更新日期:2021-02-05 00:00:00
abstract::A differential pulse polarographic method is described for detection and trace determination of benzophenone (the main impurity) in phenytoin powder. The method depends upon the polarographic activity of benzophenone in Britton-Robinson buffer pH 5.6. The limit of detection was found to be 2.5 x 10(-6) microg ml(-1). ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(01)00669-0
更新日期:2002-05-15 00:00:00
abstract::The measurement uncertainty (MU) related to analytical results can lead to false decisions in conformity assessment, such as accepting or rejecting incorrectly a medicine lot (consumer's and producer's risks, respectively). These risks can be global or specific. It is important to understand the different types of con...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2020.113203
更新日期:2020-05-30 00:00:00
abstract::An unknown degradation product (DP-1) increased in olmesartan medoxomil (OLM) tablets stored at 40 degrees C/75% r.h., reaching 0.72% after 6 months. The molecular weight and fragment information obtained by LC-MS suggested that DP-1 was a dehydrated dimer of olmesartan (OL) and the presence of ester carbonyl group wa...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2008.02.021
更新日期:2008-07-15 00:00:00
abstract::A new method was developed for the simultaneous determination of nine major constituents in Dracocephalum rupestre, including 5,7-dihydroxychromone (1), eriodictyol-7-O-beta-d-glucoside (2), luteolin-7-O-beta-d-glucoside (3), naringenin-7-O-beta-d-glucoside (4), apigenin-7-O-beta-d-glucoside (5), eriodictyol (6), lute...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2008.09.013
更新日期:2008-12-15 00:00:00
abstract::This manuscript presents an HPLC/UV method for the determination of hydrogen peroxide present or released in teeth bleaching products and hair products. The method is based on an oxidation of triphenylphosphine into triphenylphosphine oxide by hydrogen peroxide. Triphenylphosphine oxide formed is quantified by HPLC/UV...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2015.01.018
更新日期:2015-03-25 00:00:00
abstract::A method has been developed for the quantitative determination of low concentrations of sufentanil citrate (1.0 microg/ml), in the presence of bupivacaine hydrochloride (0.125%), in the quality control of pharmaceutical preparations. The main problem in analysis of this combination is the low concentration of sufentan...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(99)00219-8
更新日期:1999-12-01 00:00:00
abstract::Chrome azurol S (CAS) was tested as a spectrophotometric reagent for the determination of imipramine (IMP). It reacts in aqueous media with IMP forming pink-red, sparingly soluble in water ion association compound. This compound was quantitatively extracted with chloroform and the absorbance of organic phase was measu...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(02)00314-x
更新日期:2002-10-15 00:00:00
abstract::Non-covalent interaction of hemicyanine dyes, derivatives of 2,3,3-trimethyl-3H-indolium with bovine serum albumin has been studied by spectral method. For this purpose, three hemicyanine dyes containing N-(2-carboxyethyl)-2,3,3-trimethyl-3H-indolium moiety were synthesized and their UV/Vis and fluorescence spectra, a...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2015.06.023
更新日期:2015-10-10 00:00:00
abstract::Analysis of drugs in hair is often used as a routine method to obtain detailed information about drug ingestion. However, few studies have been conducted on disposition of synthetic cannabinoids including cyclopropylindoles (UR-144 and XLR-11) and their metabolites in hair. XLR-11 has been widely abused in South Korea...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2015.05.022
更新日期:2015-10-10 00:00:00
abstract::Stable isotope analogues of phenytoin are useful for pulse dose pharmacokinetic studies in epilepsy patients. A simultaneous assay was developed to quantitate phenytoin (5,5-diphenylhydantoin) and its stable isotope analogue [13C3]-phenytoin (5,5-diphenyl-2,4,5-13C3-hydantoin) from plasma. Quantitation was achieved by...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(98)00018-1
更新日期:1998-09-01 00:00:00
abstract::Serum metabolic profiling can identify the metabolites responsible for discrimination between doxycycline treated and untreated chronic obstructive pulmonary disease (COPD) and explain the possible effect of doxycycline in improving the disease conditions. 1H nuclear magnetic resonance (NMR)-based metabolomics was use...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章,随机对照试验
doi:10.1016/j.jpba.2016.09.034
更新日期:2017-01-05 00:00:00
abstract::Quantitative assessment of disease activity is important for effective care of patients with Takayasu arteritis (TA). Activated glutaminolysis and reduced glycolytic flux is the hallmark of active inflammation. Based on this, we hypothesize that the circulatory Glutamine/Glucose ratio (QGR) can serve as an indicant of...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2019.113080
更新日期:2020-02-20 00:00:00
abstract::The stability of ketorolac tromethamine was investigated in acid (0.5M HCl) and alkaline conditions (0.5M NaOH), using the same procedure reported by Devarajan et al. [2]. The acid and base degradation products were identified by liquid chromatography-mass spectrometry (LC-MS). ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2010.01.031
更新日期:2010-06-05 00:00:00
abstract::A high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) method, using hydrophilic interaction liquid chromatography (HILIC) chromatography for the analysis of fosfomycin in human plasma and urine, has been developed and validated. The plasma method uses a simple protein precipitation using a low v...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2014.11.042
更新日期:2015-02-01 00:00:00
abstract::Nerolidol is a naturally occurring sesquiterpene found in the essential oils of many types of flowers and plants. It is frequently used in cosmetics, as a food flavoring agent, and in cleaning products. In addition, nerolidol is used as a skin penetration enhancer for transdermal delivery of therapeutic drugs. However...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2015.03.030
更新日期:2015-01-01 00:00:00
abstract::Regulatory guidance requires the quantification of encapsulated and free doxorubicin for a liposomal doxorubicin injection bioequivalence study. Due to the instability of liposome formulations in plasma samples, the release of free drug from the liposomal encapsulated doxorubicin during sample handling would result in...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2020.113388
更新日期:2020-09-10 00:00:00
abstract::A highly sensitive and selective liquid chromatography-tandem mass spectrometry method for the determination of tetrahydrocannabinol (THC), cannabidiol, and rimonabant in rat plasma was developed. Analytes and the internal standard were extracted from plasma using a combination of protein precipitation followed by liq...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2018.07.004
更新日期:2018-10-25 00:00:00