Abstract：
:As high-performance liquid chromatography (HPLC), the premier analytical technique in the pharmaceutical industry, becomes more ubiquitous, methods are more frequently being transferred from one laboratory to another. This review will discuss sources of failures to reproduce HPLC procedures, ranging from sample handling and preparation, through mobile phase, injector, column, detector and data manipulation problems. Also to be considered will be the precautions that should be taken, when initially developing a method, to obviate future problems. These precautions include using stable, well-defined analytical columns, buffered mobile phases, low wavelengths (or a mass-sensitive detector) and internal tests for accuracy; based on the author's experiences. Since the laboratory that originally developed the procedure has the moral obligation and, perhaps, the regulatory responsibility to "guarantee" that the method will perform successfully elsewhere, a series of increasingly comprehensive steps will be given, based on practice, to be followed by the laboratory that could not reproduce the procedure. Also to be discussed are approaches for treating methods that were initially successful but have slowly deteriorated and now fail, and several examples of procedures that were not reproducible in some other laboratories.
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
Kirschbaum JJdoi
10.1016/0731-7085(89)80002-0subject
Has Abstractpub_date
1989-01-01 00:00:00pages
813-33issue
7eissn
0731-7085issn
1873-264Xpii
0731-7085(89)80002-0journal_volume
7pub_type
杂志文章,评审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：:The stability of the new chemical synthetic enaminone derivative (E118) was investigated using a stability-indicating high-performance liquid chromatography (HPLC) procedure. The examined samples were analyzed using a chiral HSA column and a mobile phase (pH 7.5) containing n-octanoic acid (5 mM), isopropyl alcohol an...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(01)00532-5
更新日期：2002-01-01 00:00:00
abstract：:A method was validated and optimized to determine tobramycin (TOB) and its related substances. TOB is an aminoglycoside antibiotic which lacks a strong UV absorbing chromophore or fluorophore. Due to the physicochemical properties of TOB, capillary electrophoresis (CE) in combination with Capacitively Coupled Contactl...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2011.09.032
更新日期：2012-01-25 00:00:00
abstract：:A gas chromatographic method to measure urinary levels of the central nervous system stimulant fencamfamine and some of its metabolites is described. When 100 mg fencamfamine was given orally to four horses the parent drug could not be detected in the urine. After enzymatic hydrolysis of the urine the major human meta...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(92)80093-3
更新日期：1992-09-01 00:00:00
abstract：:Obesity is one of the independent risk factors for several health problems, leading to metabolic perturbations and for which analytical approaches i.e., "metabolomics" is needed to monitor the underlying metabolic changes. In this study, obesity associated changes were assessed via serum metabolites analysis of obese ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2017.05.001
更新日期：2017-08-05 00:00:00
abstract：:GR117289X, 3-(3-Bromo-2-[2-(1H-tetrazol-5-yl)-phenyl]-bezofuran-5-yl methyl)-2-butyl- 5-chloro-3H-imidazole-4-carboxylic acid, 1, is an angiotensin II receptor antagonist. A sensitive, accurate and precise assay for the determination of 1 in human plasma and validation data is described. The assay consists of a novel ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(94)e0032-v
更新日期：1994-09-01 00:00:00
abstract：:Bromadiolone (BRD), a substituted 4-hydroxycoumarin derivative, is known to possess anti-coagulant activity with acute toxicity. In this paper, we report a study on the interaction of bromadiolone with the plasma proteins bovine serum albumin (BSA) and human serum albumin (HSA), using the intrinsic fluorescence emissi...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2005.01.023
更新日期：2005-07-01 00:00:00
abstract：:Free D-aspartate and D-serine occur at substantial levels in the mammalian brain. D-Serine is a physiological endogenous co-agonist for synaptic N-Methyl D-Aspartate (NMDA) receptors (NMDARs), and is involved in the pathophysiology of schizophrenia. Much less is known about the biological meaning of D-aspartate. D-Asp...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章,评审
doi：10.1016/j.jpba.2015.03.024
更新日期：2015-12-10 00:00:00
abstract：:The increasing complexity of novel biotherapeutics such as bispecific antibodies or fusion proteins raises new challenges for functional characterization. When compared to standard antibodies, two individual interactions and the inter-dependency of binding events need to be considered for bispecific antibodies. We hav...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2016.09.028
更新日期：2017-01-05 00:00:00
abstract：:A simple and efficient MEKC method was developed to simultaneously determine human insulin, its five analogues, the main degradation products and the excipients usually present in injection formulations. A very fast method with a total analysis time of 3 min was then successfully validated for the analysis of human in...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2014.12.038
更新日期：2015-01-01 00:00:00
abstract：:A new HPLC method for the determination of paeoniflorin in rat serum with solid-phase extraction (SPE) for preconcentration is introduced. Paeoniflorin and an internal standard (pentoxifylline) were extracted from serum by means of SPE using cartridges with octadecyl chemically bound phase. The HPLC separation was the...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(03)00294-2
更新日期：2003-10-15 00:00:00
abstract：:A method for the determination of 4-aminophenol as an impurity in paracetamol (N-(4-hydroxyphenyl)-acetamide) by proton nuclear magnetic resonance ((1)H-NMR) spectroscopy has been developed. The (13)C-satellite from the protons in the ortho position from the hydroxyl group in paracetamol was used as an internal standa...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(02)00086-9
更新日期：2002-07-01 00:00:00
abstract：:An electrochemical DNA nano-biosensor is prepared by immobilization of double stranded DNA (dsDNA) onto a mixed self-assembled monolayer (SAM) composed of azide- and hydroxyl-terminated thiols. The SAMs- and dsDNA-modified gold electrodes were characterized by cyclic voltammetry (CV) and electrochemical impedance spec...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2008.12.035
更新日期：2009-04-05 00:00:00
abstract：:A comprehensive review with 276 references for the analysis of members of an important class of drugs, cephalosporin antibiotics, is presented. The review covers most of the methods described for the analysis of these drugs in pure forms, in different pharmaceutical dosage forms and in biological fluids. ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章,评审
doi：10.1016/j.jpba.2007.06.002
更新日期：2007-09-21 00:00:00
abstract：:Extracts from the Carica papaya L. plant are widely reported to contain metabolites with antibacterial, antioxidant and anticancer activity. This study aims to analyze the metabolic profiles of papaya leaves and seeds in order to gain insights into their phytomedicinal constituents. We performed metabolite fingerprint...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2015.06.035
更新日期：2015-11-10 00:00:00
abstract：:A practical HPLC-MS method for the quantitative determination of salacinol (1) and kotalanol (2), potent alpha-glucosidase inhibitors from Salacia species (Hippocrateaceae) as a specific remedy for diabetes in Ayurvedic system, was developed. The optimum conditions of separation and detection of these two constituents...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2010.02.025
更新日期：2010-09-05 00:00:00
abstract：:Type 1 diabetes mellitus is a major endocrine disorder, affecting approximately 5% of the world's population. It not only leads to hyperglycaemia but also causes many complications, and numerous studies have demonstrated that oxidative stress contributes to these complications. As a new strategy to improve the oxidati...
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.2010.07.034
更新日期：2010-12-15 00:00:00
abstract：:The aim of this work was to evaluate the compatibility of (+)-catechin (CA) and excipients commonly used to prepare micro and nanoemulsions using thermal analysis along with complementary assays. Lipid compounds labrasol, plurol and ethyl oleate were combined with CA according to a simplex centroid mixture design and ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2017.11.069
更新日期：2018-02-05 00:00:00
abstract：:Understanding the origin and fate of organic impurities within the manufacturing process along with a good control strategy is an integral part of the quality control of drug substance. Following the underlying principles of quality by design (QbD), a systematic approach to analytical control of process impurities by ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2010.01.043
更新日期：2010-08-01 00:00:00
abstract：:Combined infrared--mass spectra (IR--MS) have been used to examine a small data set of synthetic substances in order to elucidate whether a combination of spectral descriptors yield better classification and similarity predictions than their corresponding individual spectral descriptors. To eliminate differences in va...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(01)00427-7
更新日期：2001-09-01 00:00:00
abstract：:A high-performance chromatographic method is described for simultaneous determination of ambroxol in the presence of different preservatives in syrups. The method separates ambroxol from methyl- ethyl-, propyl- and butyl paraben and from other multi-component mixtures. The retention behaviour of ambroxol and parabens ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(00)00318-6
更新日期：2000-08-15 00:00:00
abstract：:Morroniside is an important constituent of traditional Chinese medicines Fructus Corni with several bioactivities. An HPLC method for determination of morroniside in rat plasma and tissues was developed and the pharmacokinetic and tissue distribution characteristics of morroniside after intravenous and oral administra...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2007.05.013
更新日期：2007-10-18 00:00:00
abstract：:A limited number of studies with application of the Arrhenius equation have been reported to drugs and biopharmaceuticals in biological fluids at frozen temperatures. This paper describes stability studies of ampicillin and cephalexin in aqueous solution and human plasma applying the Arrhenius law for determination of...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2012.04.010
更新日期：2013-01-25 00:00:00
abstract：:Co-crystallization brings new opportunities for improving the solubility and dissolution rate of drugs with the chance of finely tuning some relevant chemical-physical properties of mixtures containing bioactive compounds. As co-crystallization process involves several molecular species, which are generally solid at r...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2013.01.042
更新日期：2013-05-05 00:00:00
abstract：:A bioanalytical method using automated sample transferring, automated solid phase extraction (SPE) and liquid chromatography-tandem mass spectrometry (LC-MS-MS) was developed for morphine (MOR), and its metabolites morphine-3-glucuronide (M3G) and morphine-6-glucuronide (M6G) in human plasma. Samples of 0.25 ml were t...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(01)00497-6
更新日期：2002-01-01 00:00:00
abstract：:A molecular imprinted polymer (MIP) was prepared to 7-hydroxycoumarin (7-OHC). A number of preparation parameters were examined by ultraviolet (UV) spectroscopy, including the amount of solvent used for reaction, equilibration time, selectivity and capacity of material. The polymer which showed the most selectivity fo...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(97)00043-5
更新日期：1997-10-01 00:00:00
abstract：:Phytosterols are bioactive compounds, one of their most studied and outstanding properties being their cholesterol-lowering activity. This explains the growing interest in the phytosterol contents of foods as either intrinsic or added components. The different steps (extraction, saponification, clean up, chromatograph...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章,评审
doi：10.1016/j.jpba.2006.02.052
更新日期：2006-08-28 00:00:00
abstract：:Protandim is an over-the-counter herbal dietary supplement. The key components of Protandim, i.e., epigallocatechin-3-gallate (EGCG), silibinin (SIL), and curcumin (CUR) were simultaneously analyzed through a liquid chromatography-tandem mass spectrometric (LC-MS/MS) method in plasma and different tissues after admini...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2019.03.024
更新日期：2019-06-05 00:00:00
abstract：:A simple high-performance liquid chromatographic assay with using UV detection (266 nm) was developed to determine a novel gastroprokinetic agent, Z-338 in dog plasma. The extraction procedure using solid-phase extraction with a Isolute SCX column produces extremely clean eluates and a high recovery. Intra- and inter-...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(00)00593-8
更新日期：2001-06-01 00:00:00
abstract：:Alkyl quinolone molecules 2-heptyl-4-quinolone (HHQ) and 2-heptyl-3-hydroxy-4(1H)-quinolone (PQS) are important quorum sensing signals, which play a mediatory role in the pathogenesis of acute and chronic Pseudomonas aeruginosa infection. A targeted approach inhibiting the bacterial 'multiple virulence factor regulon'...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2017.02.034
更新日期：2017-05-30 00:00:00
