Abstract:
:LC-MS-MS method using automated on-line solid-phase extraction (SPE) has been developed and validated for the quantitation of brostallicin (I), a new distamycin derivative, in human plasma. I is a DNA minor groove binder currently under phase I-II clinical evaluation as an anticancer drug. Plasma (0.4 ml) was spiked with 0.2 ml stable label IS solution and placed in a 96-well plate maintained at +4 degrees C. Aliquots of 0.1 ml of prepared samples were loaded into the on-line SPE HySphere Resin SH cartridges (10 mm x 2 mm ID) and the analytes back eluted with the mobile phase into LC-MS-MS system. A Platinum Cyano column (100 mm x 4.6 mm, 3.6 microm) was used to perform the chromatographic analysis. The mobile phase was acetonitrile-ammonium formate buffer (pH 3.5; 20 mM) (70:30, v/v) at a flow rate of 1.0 ml/min. LC flow was split so that 300 microl/min was directed toward the mass spectrometer interface. Retention time of I was 2.6 min and the total cycle time was 8 min. MS detection used an Applied Biosystems/MDS SCIEX API 365 with a TurboIonSpray interface and MRM (m/Z: 725/257 for I and m/Z: 729/257 for IS) operated in positive ion mode. The method was validated over the calibration range 0.124-497 ng/ml. A negligible carry-over effect from the system was observed. In spite of the known instability of I in human plasma (about 20% decrease over 12 h), the ratio analyte/IS peak area showed good stability over the analysis time required for 96 samples. The automated on-line SPE method can be considered as a valid alternative to the off-line manual SPE procedure previously developed.
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
Calderoli S,Colombo E,Frigerio E,James CA,Sibum Mdoi
10.1016/s0731-7085(03)00167-5subject
Has Abstractpub_date
2003-08-08 00:00:00pages
601-7issue
4-5eissn
0731-7085issn
1873-264Xpii
S0731708503001675journal_volume
32pub_type
杂志文章abstract::A sensitive and specific ultra-performance liquid chromatography tandem mass spectrometry (LC-MS/MS) method has been developed for the determination of nicousamide in human plasma. This method has also been validated in terms of selectivity, linearity, lower limit of quantification (LLOQ), accuracy, precision, stabili...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2013.01.025
更新日期:2013-04-15 00:00:00
abstract::A simple, rapid and sensitive high-performance liquid chromatographic (HPLC) method has been developed to quantify Ivermectin (IVM) in plasma using an isocratic system with fluorescence detection. The method included a fast liquid phase extraction using cold methanol. HPLC separation was carried out by reversed phase ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(02)00720-3
更新日期:2003-03-26 00:00:00
abstract::A simple and rapid method was developed for measuring 10 organophosphorus pesticides (acephate, methidathion, dichlorvos, fenthion, EPN, diazinon, phenthoate, malathion, fenitrothion, and cyanophos) in the serum of acute poisoning patients by LC/MS. Following deproteinization by acetonitrile, an aliquot of the biologi...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2007.01.036
更新日期:2007-05-09 00:00:00
abstract::A micellar electrokinetic chromatographic (MEKC) method was developed for the quantification of lovastatin and simvastatin, cholesterol lowering agents in pharmaceutical dosage forms. Lovastatin and simvastatin were separated using an electrolyte system consisting of 12% acetonitrile (v/v) in 25 mM sodium borate buffe...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(02)00128-0
更新日期:2002-07-20 00:00:00
abstract::Extemporaneous oral preparations are routinely compounded in the pharmacy due to a lack of suitable formulations for special populations. Such small-scale pharmacy preparations also present an avenue for individualized pharmacotherapy. Orodispersible films (ODF) have increasingly been evaluated as a suitable dosage fo...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2017.11.068
更新日期:2018-02-20 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::Two impurities showing structures 5 and 6 were isolated and characterised by means of NMR analysis, during the optimisation of a synthetic procedure to tazarotene. Impurity 5, i.e. ethyl 6-((4,4-dimethyl-4H-thiochromen-6-yl)ethynyl)nicotinate, was a by-product of the reduction of the intermediate sulfoxide 7 with PCl(...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2007.11.004
更新日期:2008-02-13 00:00:00
abstract::A high-performance liquid chromatographic method for the simultaneous determination of 5-aminosalicylic acid (5-ASA), acetyl-5-aminosalicylic acid (Ac-5-ASA) and 2,5-dihydroxybenzoic acid (5-HSA) in human endoscopic intestinal biopsy with electrochemical detection has been developed and validated. A liquid-liquid extr...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(95)01608-2
更新日期:1995-12-01 00:00:00
abstract::DuP 937, an anthrapyrazole antitumour agent that is chemically unstable in aqueous solution, was shown, by absorption spectroscopy, to form an inclusion complex with heptakis(2,6-di-O-methyl)-beta-cyclodextrin (DM beta CD) in aqueous solution. Proton nuclear magnetic resonance spectroscopy was used to determine the st...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(94)00063-8
更新日期:1994-10-01 00:00:00
abstract::In an expanded newborn screening program for inborn errors of metabolism by LC-MS/MS in Tuscany, six newborns out of 169,000 showed decreased blood citrulline levels. In one of them, molecular analysis of the OTC gene identified the known p.Trp265Leu mutation, which is correlated with late-onset ornithine transcarbamy...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2009.03.001
更新日期:2009-07-12 00:00:00
abstract::Polarography was the first developed automated method of voltage-controlled electrolysis with dropping mercury electrode (DME). Then, hanging mercury drop and static mercury drop electrodes were added as an alternative indicator electrode. In this way, polarography turned formally into voltammetry with mercury electro...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章,评审
doi:10.1016/j.jpba.2016.05.006
更新日期:2016-10-25 00:00:00
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 handli...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章,评审
doi:10.1016/0731-7085(89)80002-0
更新日期:1989-01-01 00:00:00
abstract::A simple HPLC method with UV detection is proposed for the simultaneous determination of three lipophilic vitamins: all-trans-retinol, alpha-tocopherol and coenzyme Q(10) (ubiquinone) in human plasma. The following chromatographic conditions were used: RP-18 column, a mobile phase consisted of methanol -n-hexane 72:28...
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.2006.03.037
更新日期:2006-09-18 00:00:00
abstract::Values of the ionization constants at 37 °C, which are scarcely reported, are more meaningful for interpreting mechanisms of cellular transport by ionizable molecules and in mechanistic dissolution studies, which are often performed at the biorelevant temperature. An equation was developed where the pK(a) values of dr...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2011.05.007
更新日期:2011-09-10 00:00:00
abstract::Brain distribution pattern of "street" heroin metabolites (morphine and codeine) was investigated in two fatalities due to "acute narcotism". A suitable sample pretreatment prior to solid-phase-extraction was developed to achieve a good recovery of the analytes and to eliminate the interfering species. After derivatiz...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2012.04.001
更新日期:2013-01-25 00:00:00
abstract::A rapid clean-up procedure based on solid-phase extraction (SPE) and HPLC determination of lincomycin in premixes with UV detection is described. After extraction of lincomycin from premix with extraction solvent the extract is applied to OASIS HLB column treated with methanol and water. Lincomycin is eluted with meth...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2005.07.041
更新日期:2006-03-03 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::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::In this study, a new approach using 1H NMR spectroscopy combined with chemometrics method was developed for qualitative and quantitative analyses of extracts of Compound Danshen Dripping Pills (CDDP). For the qualitative analysis, some metabolites presented in Compound Danshen extract (CDE, extraction intermediate of ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2016.08.017
更新日期:2016-11-30 00:00:00
abstract::This paper describes a method for quantification of d-amphetamine and diphenhydramine in beagle dog plasma by organic solvent field-amplified sample stacking (FASS)-capillary zone electrophoresis (CZE), using amlodipine as the internal standard. The separation was carried out at 25 °C in a 40.2 cm × 75 μm fused-silica...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2018.04.040
更新日期:2018-07-15 00:00:00
abstract::A high-performance liquid chromatographic (HPLC) method is described for the assay of salmon calcitonin. The method uses a 5-microns octadecasilyl silica column (100 x 4.6 mm) at 50 degrees C and an initial mobile phase (flow rate 1 ml min-1) comprising 35% of B (1 M tetramethylammonium hydroxide-water-acetonitrile, 8...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(90)80118-9
更新日期:1990-01-01 00:00:00
abstract::Brucellosis is a serious zoonosis with a rapid increase in incidence across epidemic regions. Currently, there are numerous methods for diagnosing brucellosis. However, these studies often have a few defects, such as low sensitivity, poor specificity, time consuming, laborious, and even potential biological risk. To o...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2017.03.002
更新日期:2017-07-15 00:00:00
abstract::Pharmaceutical excipients containing volatile odor-active molecules can be used in pharmaceutical development to increase patients' compliance. However, capturing the molecular composition of these odor-active substances is challenging. Therefore, guidance for the analytical investigation of these excipients should be...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2015.01.033
更新日期:2015-06-10 00:00:00
abstract::Spectroscopic and chromatographic methods (HPLC, HPLC-MS, NMR) were used to observe, separate and identify products of radiolysis of thiamphenicol (TF), irradiated in the solid state at room temperature and atmospheric pressure with an electron beam from a linear accelerator to doses between 25 and 800 kGy. Nine produ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2010.03.026
更新日期:2010-12-01 00:00:00
abstract::In this paper, binding interaction of 5-(ethoxycarbonyl)-6-methyl-4-(4-methoxyphenyl)-3,4-dihydropyrimidin-2(1H)-one (EMMD) with human serum albumin (HSA) under physiological conditions was investigated by using spectroscopy, isothermal titration calorimetry (ITC) and molecular modeling techniques. The results of spec...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2011.03.006
更新日期:2011-07-15 00:00:00
abstract::Diclofenac (DCF) is the most widely prescribed non-steroidal anti-inflammatory drug in the world and it has been detected in drinking and surface waters. In this paper, the effect of chlorination process on DCF in aqueous solutions was investigated and the structures of 14 isolated degradation by-products (DPs), of wh...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2020.113762
更新日期:2021-02-05 00:00:00
abstract::The present manuscript deals with a simple and sensitive flow-injection method for the chemiluminescent determination of thiazides. The method is based on the on-line photodegradation and chemiluminescent determination of the resulting photo-fragments. The on-line photodegradation is performed in basic medium by using...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2004.08.020
更新日期:2004-11-19 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::A method for routine base composition determination of phosphorothioate oligonucleotides containing as many as 21 nucleobases has been developed and systematically evaluated in terms of factors contributing to assay precision and accuracy. Phosphorothioate internucleotide linkages were oxidized with a mixture of tetra...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(94)00099-9
更新日期:1994-11-01 00:00:00
abstract::Platycladi Cacumen (PC) is a traditional Chinese medicine used for the treatment of hemorrhages, cough, asthma and hair loss. To get a better understanding of the chemical constituents in PC, ultra-high performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight tandem mass spectro...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2018.03.005
更新日期:2018-05-30 00:00:00