Abstract：
:Dried blood spot (DBS) sampling was investigated as a means of obtaining micro-volume blood samples for the quantitative analyses of ten commonly UK prescribed cardiovascular drugs as an indicator of medication adherence. An 8mm disc was punched out from each DBS from calibration, quality control and volunteer samples and extracted using methanol containing the internal standard. Each extract was evaporated to dryness, the residue reconstituted in methanol:water (40:60v/v) containing 0.1% formic acid and analysed by LC-HRMS. Chromatography was performed using gradient elution on a Zorbax Eclipse C18 HD 100mm×2.1mm, 1.8μm pore size column with the column oven temperature at 40°C. Flow rate of the mobile phase was 0.6ml/min with a run time of 2.5min. Electrospray positive ionization was used for MS detection. Drug recoveries from spiked blood spots were 68% for simvastatin and ≥87% for all other target drugs. Compound specificity was obtained operating the MS with a 5ppm mass window. The LC-HRMS method was validated, with results for accuracy and precision within acceptable limits; analytes were stable at room temperature for at least 10 weeks and different blood spot volumes and haematocrit values had no significant effect. The LC-HRMS assay was used to analyse DBS samples from volunteers, some of whom were prescribed one or more of the target drugs. In results from 37 volunteers the assay successfully identified volunteers who were known to be either adherent or nonadherent; confirmed the correct drug/drugs for multiple prescriptions; demonstrated no false positives from other cardiovascular drugs; revealed several examples of unsuspected non-adherence. These results indicated that the developed assay was suitable for trials with patients.
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
Bernieh D,Lawson G,Tanna Sdoi
10.1016/j.jpba.2017.04.045subject
Has Abstractpub_date
2017-08-05 00:00:00pages
232-243eissn
0731-7085issn
1873-264Xpii
S0731-7085(17)30120-6journal_volume
142pub_type
杂志文章abstract：:A second order derivative spectrophotometric method for the determination of bifonazole in the presence of methyl- and propyl p-hydroxybenzoate as preservatives has been developed. The determination was performed in a 0.1 M HCl solution at 241.5 nm, a wavelength corresponding to the intersection of the second order de...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(03)00228-0
更新日期：2003-09-15 00:00:00
abstract：:Retention factors were determined for a set of 26 drugs, for which brain/blood concentration data are available, using immobilised artificial membrane (IAM) chromatography. The compound set represented acidic, basic and neutral drugs from various structural classes. The relationship between IAM retention and lipophili...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章,评审
doi：10.1016/s0731-7085(96)01883-3
更新日期：1997-01-01 00:00:00
abstract：:This work deals with the preparation of single-labeled bioconjugates of the antibiotic Gentamicin (GT) with the sulforhodamine-derived fluorescence dye Texas Red(®)-X (TR), its purification by high-performance liquid chromatography (HPLC) and its characterization by high-resolution mass spectrometry. Aminoglycosides s...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2015.12.053
更新日期：2016-03-20 00:00:00
abstract：:Two simple sensitive and accurate methods have been developed for the determination of ritodrine hydrochloride in bulk and pharmaceutical preparations. The first method involves the direct measurement of the native fluorescence of the drug in the concentration range 4-9 microg ml(-1), the second method is based on the...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(98)00093-4
更新日期：1998-11-01 00:00:00
abstract：:A highly sensitive sensor for the determination of rutin by adsorptive stripping voltammetry was described. It consists of a lead film modified glassy carbon electrode (LF/GCE). In the proposed procedure rutin was accumulated by adsorption on the lead film electrode and then during the stripping step a lead film and t...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2008.11.022
更新日期：2009-02-20 00:00:00
abstract：:Four analytical methods have been developed for the quality control of tablets containing mirtazapine: spectrophotometry, spectrofluorimetry, high performance liquid chromatography (HPLC) and capillary zone electrophoresis (CZE). All the methods only require a simple extraction procedure of mirtazapine from the tablet...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(01)00625-2
更新日期：2002-04-15 00:00:00
abstract：:The N-terminal glutamic acid (Glu) can be cyclized to form pyroglutamate (pGlu). Recent studies have suggested that N-terminal pGlu formation is an important posttranslational or co-translational event and is greatly facilitated by the enzyme glutaminyl cyclase, although the impact of the N-terminal cyclization on the...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2006.05.008
更新日期：2006-10-11 00:00:00
abstract：:The electrochemical reduction of meloxicam has been studied at a mercury electrode using various electrochemical methods in aqueous solutions over a wide pH range. The reduction of the drug produced a single reduction step in acidic media, whereas in slightly acidic and neutral media two reduction steps were observed....
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(01)00528-3
更新日期：2002-02-01 00:00:00
abstract：:Point-of-collection testing (POCT) devices for drugs of abuse are used to screen for the presence of psychoactive substances (PAS) in different types of settings and environments. However, these quick and advantageous tools also present disadvantages, including low-reliability measures in comparison to chromatographic...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章,meta分析,评审
doi：10.1016/j.jpba.2017.05.021
更新日期：2017-09-05 00:00:00
abstract：:A new method for the quantitative analysis by liquid chromatography-tandem mass spectrometry (LC-MS/MS) of five tyrosine kinase inhibitors (afatinib, crizotinib, osimertinib, erlotinib and nintedanib) used in the treatment of non-small cell lung cancer (NSCLC) was developed and validated in human plasma. Separation wa...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2018.05.052
更新日期：2018-09-05 00:00:00
abstract：:A simple, sensitive and rapid liquid chromatography/tandem mass spectrometry (LC-MS/MS) method was developed and validated for the quantification of gabapentin, a new antiepileptic drug, in human plasma using its structural analogue, 1,1-cyclohexane diacetic acid monoamide (CAM) as internal standard. The method involv...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2005.07.012
更新日期：2006-02-13 00:00:00
abstract：:1-Benzo[b]thien-2-ylethanone (2-acetylbenzothiophene, 2-ABT) and related impurities were determined using a reverse-phase high performance liquid chromatography system and UV detection at 254 nm. Separation was achieved isocratically on a 4.6 mm x 25 cm, 5 microns Zorbax Rx-C8 column using an eluent which is 0.2% perc...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(95)01650-3
更新日期：1996-02-01 00:00:00
abstract：:Results gained from in vivo metabolism could be more authentic to reflect the biotransformation of drugs than in vitro metabolism. This paper discusses the development and characterization of an analytical method for controlling tiamulin (TIA) and doxycycline (DOX) residues in pig plasma and urine, as well as their in...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2020.113428
更新日期：2020-10-25 00:00:00
abstract：:The current study dealt with the degradation behavior of lacosamide (LAC) under ICH prescribed stress conditions. LAC was found to be labile under acid and base hydrolytic stress conditions, while it was stable to neutral hydrolytic, oxidative, photolytic and thermal stress. In total, seven degradation products (DPs) ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2014.03.010
更新日期：2014-07-01 00:00:00
abstract：:Protein modification generally occurs by addition to the amino acid side-chains of protein at the post-translational stage, for example, by enzymatic or chemical reactions after polypeptide synthesis. Recently, the recombinant hirudin analog CX-397, a potent thrombin inhibitor, was found to contain methylated Ile resi...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章,评审
doi：10.1016/s0731-7085(02)00703-3
更新日期：2003-04-01 00:00:00
abstract：:Three different procedures for the labeling of hyaluronan (HA) with (111)In, (125)I and (14)C radionuclides were compared, and the kinetic stability of radiolabeled HA under different conditions (saline, artificial gastric juice and plasma) was established. Modification of HA structure with bifunctional chelating agen...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2010.02.005
更新日期：2010-08-01 00:00:00
abstract：:Astemizole (AST), a second-generation antihistamine, is metabolized to desmethyl astemizole (DEA), and although it has been removed from the market for inducing QT interval prolongation, it has reemerged as a potential anticancer and antimalarial agent. This report describes a novel high-performance liquid chromatogra...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2015.04.036
更新日期：2015-10-10 00:00:00
abstract：:A very sensitive and convenient nanobiosensor based on fluorescence resonance energy transfer (FRET) was developed for the detection of a 22-mer oligonucleotides sequence in Human Papillomavirus 18 virus (HPV18) gene. For this purpose, water-soluble CdTe quantum dots (QDs) were synthesized and, subsequently, amino-mod...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2017.01.002
更新日期：2017-03-20 00:00:00
abstract：:750 MHz 1H NMR spectroscopy has been used to characterise in detail the abnormal low molecular weight metabolites of urine from two patients with inborn errors of metabolism. One case of the rare condition 2-hydroxyglutaric aciduria has been examined. There is at present no rapid routine method to detect this genetic ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(97)00066-6
更新日期：1997-07-01 00:00:00
abstract：:An electrochemical method for quantifying beta-lactam antibiotics (cephalexin and ampicillin) and their hydrolysis products is described. Cyclic voltammetry at the water/nitrobenzene interface in a four-electrode system was used. The zwitterionic compounds were ionized to the necessary electrochemical form by pH adjus...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(98)00147-2
更新日期：1999-02-01 00:00:00
abstract：:A sensitive method for the analysis of unconjugated morphine, codeine, normorphine and total morphine after hydrolysis of glucuronide conjugates is described. The method was applicable to 50-microliters volumes of plasma. The analytes were converted to heptafluorobutyryl (HFB) derivatives before analysis by gas chroma...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(94)00121-h
更新日期：1995-01-01 00:00:00
abstract：:Hereditary angioedema (HAE) is a rare genetic disease caused by deficiency or dysfunction of C1 esterase inhibitor (C1-INH). Plasma C1-INH activity and concentrations of C1-INH and complement components 1q and 4 (C1q, C4) are critical to the HAE diagnosis. We describe a novel multiplexed assay to simultaneously measur...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2020.113844
更新日期：2021-02-20 00:00:00
abstract：:A rapid and sensitive method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed for the simultaneous determination of telmisartan and hydrochlorothiazide in human plasma. Sample preparation involved liquid-liquid extraction with diethyl ether-dichloromethane (60:40, v/v). The analytes a...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2008.08.021
更新日期：2008-12-01 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：:A selective and sensitive isocratic high-performance liquid chromatographic (HPLC) method was developed for the quantitative analysis of low concentrations of fluoxetine (FLX) in human plasma, with ultra-violet detection at 226 nm. A reversed-phase column, LiChrospher 60 RP-Select B (125 x 3 mm i.d., 5 microm) (Merck)...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(00)00367-8
更新日期：2000-11-01 00:00:00
abstract：:Two methods are described for the simultaneous determination of tizanidine and rofecoxib in binary mixture. The first method was based on HPTLC separation of the two drugs followed by densitometric measurements of their spots at 311 nm. The separation was carried out on Merck HPTLC aluminium sheets of silica gel 60 F2...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2004.09.036
更新日期：2005-02-07 00:00:00
abstract：:A reliable, convenient, and sensitive on-line sweeping-MEKC sample concentration technique has been applied for the simultaneous separation of six steroids including two pairs of epimer with 10mM phosphate buffer (pH 7.0) that contains 80mM sodium dodecyl sulfate (SDS), 14mM β-cyclodextrin (β-CD), and 4% (v/v) methano...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2011.07.024
更新日期：2011-12-05 00:00:00
abstract：:A sensitive and stereospecific high-performance liquid chromatography (HPLC) method for determination of sertraline in bulk drug, tablets and capsules was developed. Chromatography resolution of the sertraline enantiomeric forms and trans diastereoisomers was performed on Alltima C18 (250 mm x 4.6mm i.d., 5 microm) co...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.japna.2003.08.013
更新日期：2004-01-27 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：:A first-derivative spectrophotometric method for the determination of irbesartan (IRB) alone and in the presence of hydrochlorothiazide (HCT) is described. Measurements are made at the zero-crossing wavelength at 263.0 nm for IRB. The calibration graph was linear over the range 1.0-12.0 mg l(-1) of IRB, detection limi...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(02)00073-0
更新日期：2002-06-20 00:00:00
