Abstract:
:A method development process is commonly finalized by a method transfer from the developing to the routine laboratory. Statistical tests are performed in order to survey if a transfer succeeded or failed. However, using the classic two-sample t-test can lead to misjudgments and unsatisfying transfer results due to its test characteristics. Therefore the International Society of Pharmaceutical Engineering (ISPE) employed a fixed method transfer design using equivalence tests in their Guide for Technology Transfer. Although it was well received by analytical laboratories worldwide this fixed design can easily bring about high beta-errors (rejection of successful transfers) or high workload (many analysts employed during transfer) if sigma(AN) (error due to different analysts) exceeds 0.6%. Hence this work introduces an extended concept which will help to circumvent this disadvantage by providing guidance to select a personalized and more appropriate experimental design. First of all it demonstrates that former t-test related acceptance criteria can be scaled by a factor of 1.15, which allows for a broader tolerance without a loss of decision certainty. Furthermore a decision guidance to choose the proper number of analysts or series at given percentage acceptance limits (%AL) is presented.
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
Kaminski L,Schepers U,Wätzig Hdoi
10.1016/j.jpba.2010.04.034subject
Has Abstractpub_date
2010-12-15 00:00:00pages
1124-9issue
5eissn
0731-7085issn
1873-264Xpii
S0731-7085(10)00275-Xjournal_volume
53pub_type
杂志文章,评审abstract::Cevimeline is muscarinic receptor agonist which increases secretion of exocrine glands. Cevimeline base is a liquid (m.p. 20-25 °C) at ambient conditions, therefore its pharmaceutical formulation as a solid hydrochloride hemihydrate has been developed. The synthesis of cevimeline yields its cis- and trans-isomers and ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2015.11.006
更新日期:2016-01-25 00:00:00
abstract::A selective and sensitive liquid chromatography-mass spectrometry (LC-MS) method was developed for the simultaneous determination of Euphorbia factor L(1), Euphorbia factor L(2) and Euphorbia factor L(3) from Euphorbiae semen in rat plasma. Larotaxel was added to a 200 μL plasma sample as the internal standard (IS). T...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2012.09.005
更新日期:2013-01-01 00:00:00
abstract::Tocopherols and tocotrienols, widely described as vitamin E derivatives, have been proven to take part in a number of important biological functions. Among them, antioxidant properties had been investigated and documented in the literature. Since tocochromanols have revealed their plausible beneficial impact on severa...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章,评审
doi:10.1016/j.jpba.2016.02.051
更新日期:2016-08-05 00:00:00
abstract::TopCount, a microplate scintillation counter (MSC), has been recently employed as an off-line liquid radiochromatographic detector for radioactive metabolite profile analysis. The present study was undertaken to validate TopCount for metabolite profiling with respect to sensitivity, accuracy, precision and radioactivi...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2005.03.012
更新日期:2005-09-01 00:00:00
abstract::The application of local anesthetics, usually administered by subcutaneous injection, is common in the course of diagnostic, therapeutic, and cosmetic dermatology procedures. The effective dermal delivery of lidocaine could offer a solution to many adverse effects caused by needle insertion, such as pain, local reacti...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2018.02.056
更新日期:2018-05-30 00:00:00
abstract::Detection of higher-order aggregates (HOA) using size-exclusion chromatography (SEC) was found to be variable for a basic protein, using exposed-silanol or diol-silica-based SEC columns. Preparations of the tetrameric biopharmaceutical enzyme Erwinia chrysanthemil-asparaginase (ErA), which has an isoelectric point of ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2017.03.004
更新日期:2017-05-30 00:00:00
abstract::Standard-size (4 mm ID) and micro-HPLC columns (0.5 mm ID) packed with a quinine-based ion-exchange type chiral stationary phase are comparatively evaluated for the separation of peptide enantiomers with up to six amino acid residues. The results show that downscaling the separation system in order to gain the advanta...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(02)00521-6
更新日期:2003-01-15 00:00:00
abstract::A simple, rapid, reliable and highly sensitive on-line two-dimensional reversed-phase liquid chromatography-tandem mass spectrometric (2D-LC/MS/MS) method to determine antiretroviral drugs viz., abacavir (ABC), nevirapine (NVP) and indinavir (IDV) in rat serum and urine was developed and validated. The analytes were e...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2009.07.005
更新日期:2009-12-05 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
abstract::Different therapeutically active ingredients, from plants, animals, and mineral sources, are prescribed as traditional Chinese medicines (TCM). TCMs, from animal sources, are rich in proteins and peptides. Different advanced proteomics technologies, such as two-dimensional gel electrophoresis (2-DE), multi-dimensional...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章,评审
doi:10.1016/j.jpba.2020.113609
更新日期:2020-11-30 00:00:00
abstract::Ionic liquid-based salt-induced liquid-liquid extraction was developed for the first time and applied to the extraction of four active constituents, including polydatin, resveratrol, emodin, and physcion in Polygonum cuspidatum (P. cuspidatum). In this study, ionic liquid was used as extraction solvent. The dried P. c...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2018.09.050
更新日期:2019-01-30 00:00:00
abstract::The resolution of four racemic 3-hydroxy-1,4-benzodiazepin-2-ones, widely used in therapeutics, by means of a chiral stationary phase is described. The chiral selector used is (S)-N-(3,5-dinitrobenzoyl)phenylalanine. This chiral stationary phase showed both good enantioselectivity and efficiency for the compounds. Elu...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(91)80100-n
更新日期:1992-10-01 00:00:00
abstract::Free thiols, or unpaired cysteines, are important product quality attributes in the therapeutic proteins due to their potential impact on the protein structure, bioactivity and stability. While many free thiol quantitation methods were developed for specific therapeutic formats, an unmet need still exists for a multip...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2020.113434
更新日期:2020-09-10 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::This study aims to identify and quantify the six major bioactive flavones of the traditional Chinese medicine Scutellariae Radix (RS), including baicalein, baicalin, wogonin, wogonoside, oroxylin A and oroxyloside in rat after oral administration of a standardized RS extract. A novel, sensitive and selective method fo...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2014.03.033
更新日期:2014-08-01 00:00:00
abstract::Management of the therapy of life-threatening bacterial infection is extremely based on an optimal antibiotic treatment. Achieving the correct vancomycin dosage in blood and target tissues can be complicated in special situations, e.g., where large fluid sequestration and/or acute renal failure occur. A UHPLC-MS/MS me...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2017.04.029
更新日期:2017-08-05 00:00:00
abstract::Recombinant DNA technology has made possible the large-scale production of proteins for pharmaceutical applications. As a result, there has been a renaissance in methodology which can provide information on the structural stability and character of these materials. Circular dichroism (CD) spectroscopy, with its sensit...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章,评审
doi:10.1016/0731-7085(89)80049-4
更新日期:1989-01-01 00:00:00
abstract::The interactions between gemcitabine hydrochloride (GEM) and bovine serum albumin (BSA) or human serum albumin (HSA) have been studied by spectroscopic techniques. By the analysis of fluorescence spectrum and fluorescence intensity, it was observed that the GEM has a strong ability to quench the intrinsic fluorescence...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2005.11.037
更新日期:2006-05-03 00:00:00
abstract::Astragali Radix (AR) has been used in the traditional Chinese medicine (TCM) in the treatment of various renal diseases for many years. In this study, a NMR based metabolomic approach coupled with biochemical assay and histopathological inspection had been employed to study the protective effect of total flavonoids (T...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2018.05.045
更新日期:2018-09-05 00:00:00
abstract::Thiazolidinediones are known for their activity against Type 2 diabetes and are currently being repurposed for their potent anti-cancer activity. In the present study, we have assessed in vitro metabolic properties and in vivo pharmacokinetic parameters of a novel thiazolidinedione derivative, BIT-15-67, a potential a...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2019.113000
更新日期:2020-02-05 00:00:00
abstract::The binding of carbamazepine (CBZ) to human serum albumin (HSA) was investigated under simulative physiological conditions. In this study, intrinsic fluorescence of tryptophan-214 in HSA was monitored upon the addition of CBZ. Binding constant of CBZ-HSA was calculated by the remarkable static quenching effect of CBZ ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2010.05.025
更新日期:2010-11-02 00:00:00
abstract::A simple and reliable high-performance liquid chromatography coupled with electrospray ionization time-of-flight tandem mass spectrometry method was developed and validated for the determination of the major diterpenoids and flavonoids in the aerial parts of Herba Siegesbeckiae, including Kirenol, hythiemoside B, ent-...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2011.02.023
更新日期:2011-06-01 00:00:00
abstract::Triterpene saponins are important bioactive constituents widely distributed in many plants. Saponins present in Caulophyllum (Berberidaceae) have not been fully characterized. In this study, we studied triterpene saponins from Caulophyllum robustum using liquid chromatography combined with electrospray ionization quad...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2014.07.024
更新日期:2014-11-01 00:00:00
abstract::The extraction and determination of phthalic acid esters (PAEs) residue in Chinese herbal preparations (CHP) by C18-functionalized magnetic nanoparticles (C18-FS-MNP) has been firstly performed. It was synthesized through coating Fe3O4 nanoparticles with sodium silicate, followed by freeze-drying technique and then mo...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2014.08.027
更新日期:2014-11-01 00:00:00
abstract::A validated stability indicating RP-HPLC assay of doxofylline was developed by separating its related substances and degradants on LichrocartC18 (250 mm × 4.6 mm; 5 μm) column using 10 mM ammonium acetate and acetonitrile as a mobile phase in a gradient mode of elution at a flow rate of 1.0 mL/min at 30 °C. The column...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2013.02.004
更新日期:2013-05-05 00:00:00
abstract::Structured nanoparticles (NPs) with controlled size distribution and novel physicochemical features present fundamental advantages as drug delivery systems with respect to bulk drugs. NPs can transport and release drugs to target sites with high efficiency and limited side effects. Regulatory institutions such as the ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章,评审
doi:10.1016/j.jpba.2013.08.018
更新日期:2014-01-01 00:00:00
abstract::The reversed-phase high-performance liquid chromatography of a Peptide Nucleic Acid (PNA) trimer has been studied after its preseparation fluorogenic derivatization with naphthalene-2,3-dicarboxaldehyde in the presence of cyanide (NDA/CN). Trace levels of the PNA trimer were determined in cell homogenate samples conta...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(96)01927-9
更新日期:1997-04-01 00:00:00
abstract::A simple, rapid and sensitive method for the determination of nicotine, cotinine, nornicotine, anabasine, and anatabine in human urine and saliva was developed. These compounds were analyzed by on-line in-tube solid-phase microextraction (SPME) coupled with liquid chromatography-mass spectrometry (LC-MS). Nicotine, co...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2008.09.044
更新日期:2009-01-15 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::The permeation of essential oils through SkinEthic reconstructed human epidermis, (RHE), was studied in vitro to establish a convenient tool to monitor the kinetics of release of active principles from cosmetic formulations. Twelve days old human epidermis held on polycarbonate disks was revitalized by addition of gro...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2009.05.018
更新日期:2009-10-15 00:00:00