Abstract：
:Thermodegradation of labile compounds in the hot injection port of a gas chromatograph causes many problems and can lead to ambiguous, poorly reproducible results. Splitless injection used in trace analysis in order to achieve a lower detection limit may even enhance the difficulties due to the longer residence time of the volatized sample in the injection port. Different techniques were tested to avoid thermodegradation of an epoxide and its corresponding chlorohydrin in a drug substance: variation of the injector temperature, high inlet flow rate during injection by electronic pressure programming, and cool on-column injection. The results showed that on-column injection was superior to splitless injection. The chlorohydrin formed epoxide by release of HCl upon splitless injection. A more detailed investigation of the factors that affect epoxide formation indicates that active sites within the injector are responsible for the degradation and that the reaction is temperature dependent. However, results equivalent to those obtained by on-column injection were obtained for splitless injection when inert materials were used in the injector.
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
Klick Sdoi
10.1016/0731-7085(95)01307-7subject
Has Abstractpub_date
1995-04-01 00:00:00pages
563-6issue
4-5eissn
0731-7085issn
1873-264Xpii
0731-7085(95)01307-7journal_volume
13pub_type
杂志文章abstract：:Cobalt content (as vitamin B12 and inorganic cobalt) in two nutritional supplements, namely Spirulina platensis and Saccharomyces cerevisiae known as a "superfood", has been determined using inductively coupled plasma optical emission spectrometry (ICP-OES). Several sample pre-treatment protocols have been applied and...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2018.03.058
更新日期：2018-06-05 00:00:00
abstract：:In a previous work [J. Pharm. Biomed. Anal. 23 (2000) 447] a rapid high-performance liquid chromatography (HPLC) method, using a monolithic column in HPLC coupled with a diode-array detector, was developed for the quantitative determination of benzodiazepines in whole blood. The present method has been applied to the ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2004.01.023
更新日期：2004-05-28 00:00:00
abstract：:A sensitive and simple liquid chromatography-mass spectrometry (LC-MS) method has been developed and validated for the quantification of solamargine, a steroidal glycoalkaloid, in rat plasma. Vincristine was selected as the internal standard. Sample preparation involved simple liquid-liquid extraction by ethyl acetate...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2011.04.007
更新日期：2011-07-15 00:00:00
abstract：:Acyclovir and its major impurity guanine are determined rapidly by the incorporation of a monolithic column (100 mm x 4.6 mm i.d., Merck) to an automated HPLC system. A simple flow gradient protocol was adopted in order to accelerate the separation-detection cycle. Using 0.2% CH(3)COOH (pH 3.1) as the mobile phase and...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2006.11.002
更新日期：2007-03-12 00:00:00
abstract：:A reversed phase high-performance liquid chromatographic method with detection at 220 nm was developed and validated for the determination of piperacillin, I, and tazobactam, II, in Tazocin injectable powder. Acetaminophen was used as internal standard. A Hypersil BDS RP-C(18) column (250 x 4.6 mm), 5 microm particle ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(02)00129-2
更新日期：2002-07-31 00:00:00
abstract：:A short review of the principles of atomic absorption spectrometry (AAS) - sources, atomizers, background correction, instrumentation, sample preparation, sensitivity, limit of detection, etc. - is given. The technique can be applied for impurity tests for trace metals as well as for assay of various commonly occurrin...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(83)80065-x
更新日期：1983-01-01 00:00:00
abstract：:A quick and sensitive method has been developed and validated for the determination of tungsten in bulk drug substance and intermediates using either Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) or Inductively Coupled Plasma Mass Spectrometry (ICP-MS). Sample preparation is by direct dissolution w...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(98)00259-3
更新日期：1999-05-01 00:00:00
abstract：:Relationships among Fallopia multiflora (Thunb.) Haraldson., F. multiflora var. angulata (S. Y. Liu) H. J. Yan, Z. J. Fang & Shi Xiao Yu., and F. multiflora var. ciliinervis (Nakai) Yonekura & H. Ohashi. were determined based on macroscopic and microscopic morphology, molecular phylogeny, and chemical analysis. The ma...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2019.01.040
更新日期：2019-03-20 00:00:00
abstract：:Biotin labelled with a cymantrene moiety (cyclopentadienyl manganese tricarbonyl complex) is described for the first time. Because this metallo-biotin retains full recognition for the specific glycoprotein avidin (or streptavidin), the labelled streptavidin-biotin system is proposed for use in a solid-phase competitio...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(91)80031-4
更新日期：1991-01-01 00:00:00
abstract：:A simple and sensitive liquid chromatography/tandem mass spectrometry method was developed and validated for the quantification of rosuvastatin in human plasma. After being treated with acetic acid and tetrabutyl ammonium hydroxide, the analyte was extracted by simple one-step liquid-liquid extraction with the interna...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2006.12.022
更新日期：2007-06-28 00:00:00
abstract：:Three impurities were detected in the LC/MS analysis of fluconazole bulk drug substance. Two of the impurities were unknowns having not been reported previously. Structural assignment of these impurities was carried out by LC/MS/MS using electrospray ionization source and an ion trap mass analyzer. Structural elucidat...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2006.04.012
更新日期：2006-09-26 00:00:00
abstract：:The subject of the analysis of various elements, including metals and metalloids, in the pharmaceutical industry has seen increasing importance in the last 10-15 years, as modern analytical instrumentation has afforded analysts with the opportunity to provide element-specific, accurate and meaningful information relat...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章,评审
doi：10.1016/j.jpba.2010.11.030
更新日期：2011-06-25 00:00:00
abstract：:Species-specific acid-base and partition equilibrium constants were experimentally determined for the therapeutically important semisynthetic opioid receptor agonist hydromorphone, dihydromorphine, and mixed agonist-antagonist nalorphine and nalbuphine. The acid-base microequilibria were characterized by combining pH-...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2016.12.014
更新日期：2017-02-20 00:00:00
abstract：:Quantitative IR- and Raman spectroscopic determinations of four cephalosporin antibiotics in six solid binary mixtures have been conducted. This is a new approach for spectroscopic determination of these antibiotics, since the corresponding quantitative analysis in solution only has been reported so far. The correlati...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2008.04.026
更新日期：2008-09-10 00:00:00
abstract：:Nonsteroidal anti-inflammatory drugs (NSAIDs), which are globally prescribed, exhibit mainly anti-inflammatory and analgesic effects but also can cause adverse effects including gastrointestinal erosions, ulceration, bleeding, and perforation. The purpose of this study was to investigate surrogate biomarkers associate...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2016.07.045
更新日期：2016-09-10 00:00:00
abstract：:Fentanyl, a potent analgesic drug, has traditionally been used intravenously in surgical or diagnostic operations. Formulations with fentanyl in oral transmucosal delivery system and in transdermal depot-patch have also been developed against breakthrough pain in cancer patients. In this report, LC-MS/MS methods to de...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2004.09.024
更新日期：2005-04-29 00:00:00
abstract：:Cyclodextrins are cyclic oligosaccharides able to form inclusion complexes with a variety of hydrophobic guest molecules, positively modifying their physicochemical properties. A thorough analytical characterization of cyclodextrin complexes is of fundamental importance to provide an adequate support in selection of t...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章,评审
doi：10.1016/j.jpba.2015.01.058
更新日期：2015-09-10 00:00:00
abstract：:An extracellular thermostable antibacterial peptide designated as MFAP9 was purified from marine Aspergillus fumigatus BTMF9 by ammonium sulfate precipitation followed by ion exchange chromatography on a DEAE-sepharose column. The molecular weight of MFAP9 was found to be∼3 kDa in SDS-PAGE gel corresponding a single i...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2020.113808
更新日期：2021-02-05 00:00:00
abstract：:Measurement of the total target ligand can help to provide pharmacokinetic (PK) and pharmacodynamic (PD) informations. However, the presence of monocloncal antibody therapeutics (ThAs) interferes with ELISA determinations of the total target proteins. The interferences can cause over- or under-estimation of the target...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2009.11.021
更新日期：2010-04-06 00:00:00
abstract：:A high-performance size exclusion chromatographic procedure using a Nucleosil Diol column and fluorescence detection has been developed for the determination of dextran-naproxen ester pro-drugs with varying molecular weights and degrees of substitution in aqueous buffer solutions and biological media in the presence o...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(89)80053-6
更新日期：1989-01-01 00:00:00
abstract：:To maximize the benefits of a LIMS, the system must be integrated with the analytical instrumentation in the laboratory. This provides on-line data capture or transfer of results for matching with the corresponding sample records held within the database, which reduces transcription error checking and ensures data int...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(88)80068-2
更新日期：1988-01-01 00:00:00
abstract：:Solid phase extraction (SPE) has been utilized extensively in the pharmaceutical industry for the isolation of pharmaceuticals from interfering biological matrices and the purification and concentration of impurities and degradation products present in analytical samples. The work described herein involves the novel u...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2007.04.029
更新日期：2007-09-03 00:00:00
abstract：:The extraction properties of Hisep, a novel bonded phase for solid phase extraction, have been investigated using a number of acidic and basic analytes and compared with those of a conventional ODS bonded material. Marked differences in extraction properties for the test analytes propranolol, anisic acid and ICI 12843...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(95)01647-3
更新日期：1996-02-01 00:00:00
abstract：:The development of high performance liquid chromatography method on amylose-based stationary phases (Chiralpak AD) has permitted to achieve the preparative enantioseparation of one benzimidazole derivative, potent-AMP-kinase (AMPK) activator with satisfactory yields. Analytical enantioseparation method was optimized a...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2008.01.048
更新日期：2008-04-14 00:00:00
abstract：:Ginseng saponins isolated from ginseng, have been regarded as the principal constituents responsible for the biological activities. The aim of this study was to set up a liquid chromatography-mass spectrometry (LC-MS) method for simultaneously determine the concentration of Ginsenoside Rg1 and its secondary glycoside ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2004.12.007
更新日期：2005-06-01 00:00:00
abstract：:Biosensors containing cytochrome P450cam in a didodecyldimethylammonium bromide vesicular system were prepared by cross-linking onto a glassy carbon electrode (GCE) with glutaraldehyde in the presence of bovine serum albumin. Cyclic voltammetric responses of the sensor in air-free buffer solution showed that the senso...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(98)00076-4
更新日期：1998-09-01 00:00:00
abstract：:Studies on molecular interactions between cellular receptors of herpes simplex virus (HSV) and the viral glycoproteins showing receptor-binding activity are of great relevance for understanding the molecular basis of virus entry. Information on such interactions further provides the basis for a rational design of anti...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(03)00177-8
更新日期：2003-08-08 00:00:00
abstract：:A liquid chromatographic tandem mass spectrometric method for the quantitative determination of sumatriptan base in human plasma and urine has been developed and validated over the concentration range 0.2-20 ng base ml-1. Sumatriptan is a 5-HT1 receptor agonist which has found widespread use in the treatment of migrai...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(97)00220-3
更新日期：1998-07-01 00:00:00
abstract：:A simple and rapid quantitative analytical method for the simultaneous detection of celecoxib and its two main metabolites, hydroxycelecoxib (celecoxib-OH) and celecoxib carboxylic acid (celecoxib-COOH), in rat plasma using liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed. The plasma sample was ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2014.12.004
更新日期：2015-03-25 00:00:00
abstract：:A simple, selective and sensitive method has been developed to determine debrisoquine and 4-hydroxydebrisoquine in human urine. Separation of the analytes was obtained using a mobile phase of 0.1 M sodium dihydrogen phosphate-acetonitrile (87:13, v/v) and a muBondapak C18 column. The column effluent was monitored with...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(93)80184-3
更新日期：1993-08-01 00:00:00
