Abstract：
:This paper proposes a method for the validation of chromatography systems in which many experiments to estimate SD or RSD are difficult or impossible to carry out because of time, cost, etc. HPLC systems with UV-Vis and fluorescence detectors and GC-MS system for bisphenol-A leached from hemodialyzers are taken as an example. Examined as validation characteristics are not only the ordinary quantities (precision, accuracy, range, limit of detection (LOD), limit of quantitation (LOQ), specificity and linearity) but also precision plots (measurement RSD vs. concentration), 95% confidence intervals of calibration lines and LOD signals over baselines. The precision plots, calibration confidence intervals and LOD signals are shown to be advantageous to validate and compare the analytical performance of the systems. The LOD, LOQ, precision plots and 95% confidence intervals of calibration lines are all derived from the SD of measurements and the reliability of these quantities and plots depends totally on the reliability of the SD estimates. This paper uses a probability theory, called the FUMI theory, to estimate as exact a measurement SD as possible without the replication. The precision of the HPLC and GC-MS systems is shown to coincide with the repeatability obtained by the repetition of measurements.
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
Hayashi Y,Matsuda R,Haishima Y,Yagami T,Nakamura Adoi
10.1016/s0731-7085(01)00698-7subject
Has Abstractpub_date
2002-05-15 00:00:00pages
421-9issue
3-4eissn
0731-7085issn
1873-264Xpii
S0731708501006987journal_volume
28pub_type
杂志文章abstract：:This study addresses the lack of data on the stability of carfilzomib, a newly approved proteasome-inhibiting anticancer drug. A new stability-indicating UHPLC-UV method for analysis of carfilzomib was developed and validated within the concentrations of 10-250 μg/mL. The aforementioned method was utilized to evaluate...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2016.03.015
更新日期：2016-05-30 00:00:00
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 ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(01)00541-6
更新日期：2002-03-01 00:00:00
abstract：:A rapid, sensitive and high throughput UHPLC-MS/MS method was established and validated to assay the concentration of 2-(2-hydroxypropanamido) benzoic acid (HPABA), a promising anti-inflammatory drug, in rat plasma. Plasma samples were processed by liquid-liquid extraction with ethyl acetate and separated on a Shim-pa...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2014.02.008
更新日期：2014-07-01 00:00:00
abstract：:In the cell extraction_LC-MS method, when cells are incubated with natural product extracts, bioactive compounds selectively bind to extracellular or intracellular targets. The extracts and major compounds (phenylpropanoids and iridoid glycosides) of Scrophularia buergeriana Miquel have been reported to show neuroprot...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2017.10.018
更新日期：2018-01-30 00:00:00
abstract：:Potency is an important parameter for evaluation of quality of heparin active pharmaceutical ingredient (API). In this paper the feasibility to determine potency of heparin API with near infrared reflectance spectroscopy (NIRS) coupled with partial least squares (PLS) algorithm is attempted. PLS factors, correlation c...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2009.11.022
更新日期：2010-04-06 00:00:00
abstract：:A near-infrared reflection spectroscopy (NIRS) method was developed to determine the total content of kavapyrones, kavain and water in dry extracts of Piper methysticum Forst. (kava kava, Piperaceae). Based on the recorded spectra and the reference data, performed by HPLC and Karl Fischer titration, a chemometrical an...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2004.06.030
更新日期：2004-11-19 00:00:00
abstract：:Capillary electrophoresis (CE) was applied to the study of several inhibitors of the angiotensin-converting enzyme. Separation of the compounds was performed by means of two phosphate buffers (each 100 mM) at pH 7.0 and 6.25, respectively [S. Hillaert, W. Van den Bossche, J. Chromatogr. A, 895 (2000) 33-42.]. Due to t...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(01)00366-1
更新日期：2001-07-01 00:00:00
abstract：:A liquid chromatography-tandem mass spectrometric (LC-MS/MS) method following chemical derivatization with 3-nitrophtalic anhydride was developed for the simultaneous determination of farnesol and geranylgeraniol in rat liver and testis. One analogue compound of the analytes, n-pentadecanol, was used as an internal st...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2008.01.032
更新日期：2008-07-15 00:00:00
abstract：:The role of selenium as an antioxidant and anticancer agent is very well documented in the literature. Selenium compound showing the highest activity as a free radicals scavenger and as an anticancer agent should contain selenium at +4 oxidation level. The synthesis of selenitetriglycerides (named selol) was carried o...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(03)00205-x
更新日期：2003-08-08 00:00:00
abstract：:Alkaloids, the principal constituents in the caulis of Sinomenium acutum, have gained an increasing interest over the past decades since they are widely employed as a clinical treatment for rheumatoid arthritis. In the present study, an integrated characterization strategy by combining mass defect filtering-based stru...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2019.06.011
更新日期：2019-09-10 00:00:00
abstract：:2-Phosphonomethyl pentanedioic acid (2-PMPA) is a potent and selective inhibitor of glutamate carboxypeptidase-II, an enzyme which catabolizes the abundant neuropeptide N-acetyl-aspartyl-glutamate (NAAG) to N-acetylaspartate (NAA) and glutamate. 2-PMPA demonstrates robust efficacy in numerous animal models of neurolog...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2013.08.028
更新日期：2014-01-01 00:00:00
abstract：:Abiraterone acetate is administered as a prodrug to patients with metastatic, castration-resistant prostate cancer (mCRPC) and is readily metabolized into the potent 17a-hydroxylase/17,20-lyase (CYP17) enzyme inhibitor and androgen receptor inhibitor abiraterone and Δ(4)-abiraterone (D4A), respectively. To investigate...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2018.03.012
更新日期：2018-05-30 00:00:00
abstract：:The present investigation was aimed at the evaluation of possible interactions between mirtazapine and selected solid lipids that are commonly used to develop solid lipid nanoparticles (SLNs) and nanostructured lipidic carriers (NLCs). The solids lipids explored were palmitic acid, stearic acid, glycerylmonostearate, ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2018.08.041
更新日期：2018-11-30 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：:Aurantio-obtusin, an anthraquinone isolated from cassiae semen, possesses diverse pharmacological activities, including hypotensive, hypolipidemic and anti-inflammatory effects. However, our previous studies demonstrated that exposure to aurantio-obtusin induced hepatotoxicity, but the mechanisms of the toxic effects ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2021.113896
更新日期：2021-01-13 00:00:00
abstract：:Liquid chromatography (LC) and capillary electrophoresis (CE) methods were developed to perform the determination of residual sodium in mother liquors and successive washes of an active pharmaceutical ingredient (API). The addition of sodium chloride to the product solution results in rapid and complete crystallizatio...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2006.07.020
更新日期：2007-07-27 00:00:00
abstract：:While capillary electrophoresis has been established as a major enantioseparation technique within the last decade, the potential of capillary electrochromatography is still studied extensively. This review summarizes recent applications of electromigration techniques with regard to the enantioseparation of chiral dru...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章,评审
doi：10.1016/s0731-7085(01)00653-7
更新日期：2002-01-15 00:00:00
abstract：:An LC procedure was developed to separate diatrizoate sodium from three known impurities. These impurities are 2,4- and 2,6-diiodo-3,5-diacetamidobenzoic acid (DDZA), and the free amine (5-acetamido-3-amino-2,4,6-triiodobenzoic acid). The separation was achieved using a Hamilton, PRP-X100, anion exchange column. The r...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(97)00007-1
更新日期：1997-09-01 00:00:00
abstract：:The water content of six different substances was determined by means of five different methods. The methods used were loss on drying, thermogravimetry (coupled with DSC), a new phosphorous-pentoxide method, direct Karl-Fischer titration and the Karl-Fischer oven. A combination of direct Karl-Fischer titration and the...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2006.08.002
更新日期：2007-01-17 00:00:00
abstract：:Nitrofurnation is an antibacterial drug. It is used in the treatment of initial or recurrent urinary tract infections caused by susceptible organisms. The cyclic voltammogram of the drug in Britton-Robinson buffers (pH 2-11) exhibited a single well-defined cathodic peak at the hanging mercury drop electrode, that due ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(02)00344-8
更新日期：2002-10-15 00:00:00
abstract：:An automated system has been developed and validated for the analysis of liquid formulations (solution and suspension). The system comprises a multi-place magnetic stirrer, a diluter and a diode array UV spectrophotometer. The system can handle a wide range of drug formulation concentrations (> 200 mg ml-1) and gives ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(96)01882-1
更新日期：1997-02-01 00:00:00
abstract：:A solid phase fluorescence spectroscopic batch procedure for (acetyl) salicylic acid in drug formulations have been developed. The procedure is based on the sorption of salicylic acid (SA) on Sephadex DEAE A-25 anion exchanger gel (100 mg) by equilibration from an aqueous solution (10 or 25 ml) for 5 min; the equilibr...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(02)00719-7
更新日期：2003-03-10 00:00:00
abstract：:The fully humanized Lewis-Y carbohydrate specific monoclonal antibody (mAb) IGN311 is currently tested in a passive immunotherapy approach in a clinical phase I trail and therefore regulatory requirements demand qualified assays for product analysis. To demonstrate the functionality of its Fc-region, the capacity of I...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2009.01.029
更新日期：2009-05-01 00:00:00
abstract：:CGS 26214 is a racemic compound having cholesterol-lowering activity in rats, dogs, and monkeys. This compound has two equipotent chiral components CGS 28934(-) and CGS 28935(+). An analytical challenge was to develop a sensitive liquid chromatography/tandem mass spectrometry (LC/MS/MS) method for the analysis of the ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(00)00364-2
更新日期：2000-09-01 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：:Quantification of virus-like RNA sequences in biological fluids, like serum and cerebrospinal fluid, requires an RNA extraction method that is both reproducible and fast. Three RNA extraction methods were tested on enteroviruses: (1) the acid guanidine thiocyanate-phenol/chloroform (AGPC) method; (2) a method based on...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(03)00312-1
更新日期：2003-11-24 00:00:00
abstract：:Levo-tetrahydropalmatine (l-THP) is a tetrahydroprotoberberine isoquinoline alkaloid and has been used as an analgesic agent in China for over 50 years. Recent studies revealed that l-THP was effective in the treatment of drug addiction. However, the plasma metabolic profile, mass balance and clearance pathways of l-T...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2016.06.015
更新日期：2016-09-05 00:00:00
abstract：:Sunitinib is approved for advanced renal cell cancer, imatinib-resistant or -intolerant gastrointestinal stromal tumors and pancreatic neuroendocrine cancers. It is prescribed at a fixed dose but its plasma exposure shows large inter-individual variations. Taking into account the narrow therapeutic window and the posi...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2019.112949
更新日期：2020-02-05 00:00:00
abstract：:Nucleobases, nucleosides and ginsenosides, which have a significant impact on the physiological activity of organisms, are reported to be the active components of ginseng, while they are less present in ginseng extracts. Few analytical methods have been developed so far to simultaneously analyze these three classes of...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2017.03.059
更新日期：2017-09-10 00:00:00
abstract：:A sensitive high performance liquid chromatographic (HPLC) assay has been developed and validated for the quantitation of the novel anticancer agent topotecan and topotecan as its lactone plus carboxylate forms in rat and dog plasma. Linear responses in analyte standard peak areas were observed over the concentration ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(96)01838-9
更新日期：1996-11-01 00:00:00
