Abstract：
:IIIM-290, an orally bioavailable preclinical candidate is effective in human xenograft models of leukemia, colon and pancreatic cancer. The promising preclinical data of this lead candidate has shown its potential for clinical development. As a part of its preclinical development, impurity profiling of pilot scale batches is one of the most important component of the CMC documentation. Herein, we report impurity profiling, its quantification in different scale-up batches and analytical method validation. Three impurities ranging from 0.09 to 1.25% in preclinical anticancer candidate, IIIM-290 were detected by validated HPLC method. The impurities (Imp-A, Imp-B and Imp-F) were isolated from the partially purified batch of IIIM-290 using semi-preparative HPLC. Isolated impurities were characterized by 1H, 13C NMR, FTIR and ESI-MS spectral data. Based on the characterization data, the sources of these impurities were identified as unreacted starting material (Imp-A), impurity from botanical raw material (Imp-B; impurity carried from starting material) and the chemically transformed product (Imp-F) of Imp-B, respectively.
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
Kumar V,Bhurta D,Sharma A,Kumar P,Bharate SB,Vishwakarma RA,Bharate SSdoi
10.1016/j.jpba.2018.12.027subject
Has Abstractpub_date
2019-03-20 00:00:00pages
1-5eissn
0731-7085issn
1873-264Xpii
S0731-7085(18)32195-2journal_volume
166pub_type
杂志文章abstract：:A fast and sensitive ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination and pharmacokinetic study of nimodipine in human plasma. With nitrendipine as the internal standard, sample pretreatment involved one-step extraction with diethyl ether of 0.5 m...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2007.10.035
更新日期：2008-02-13 00:00:00
abstract：:Zopiclone (ZO) is a chiral drug that undergoes extensive metabolism to N-desmethylzopiclone (N-Des-ZO) and zopiclone-N-oxide (N-Ox-ZO). Pharmacological studies have shown (S)-N-Des-ZO metabolite presents anxiolytic activity and a patent for this metabolite was requested for anxiety treatment and related disorders. In ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2015.02.039
更新日期：2015-05-10 00:00:00
abstract：:A novel drug-delivery system was developed by loading the anticancer drug, mitomycin C (MC) into an oil/water system with the aim of investigation by electrochemical sensing the interaction between the drug and DNA in microemulsion phase. The physical and physicochemical properties (droplet size, pH, viscosity, conduc...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2007.05.005
更新日期：2007-10-18 00:00:00
abstract：:Comparison is made between conventional liquid-liquid extraction and solid-phase extraction techniques using Extrelut-1, Extrelut-3 and C18-RP cartridges respectively for the screening of several beta-blockers in urine. Generally, using GC with nitrogen specific detection as the screening technique, liquid-liquid extr...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(88)80098-0
更新日期：1988-01-01 00:00:00
abstract：:A series of synthesised tocainide analogues were characterized for their human serum albumin (HSA) binding, using high-performance liquid affinity chromatography (HPLAC) and circular dichroism (CD). The synthesis and physico-chemical characterization of compounds 7a-7d is reported here. For the HPLAC investigation HSA...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2010.03.005
更新日期：2010-10-10 00:00:00
abstract：:Efonidipine hydrochloride is a new generation dihydropyridine Ca(2+) channel blocker designed to inhibit both T-type and L-type Ca(2+) channels. Efonidipine possesses a chiral carbon and is clinically administered as a racemate. In the present study, an enantioselective and sensitive LC-MS/MS method of determining efo...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2016.01.039
更新日期：2016-04-15 00:00:00
abstract：:A high-performance liquid chromatographic method for the simultaneous determination of magnesium ascorbyl phosphate (I), imidazolidinylurea (II), a mixture of methyl-(III), ethyl-(IV), propyl-(V), butyl-(VI) parabens dissolved in phenoxyethanol, and ascorbyl palmitate (VII), was studied by using a cyano-propyl column ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(98)00173-3
更新日期：1998-10-01 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：:Mass spectrometry based precision identification of natural products requires the validation of the reference compounds. This study attempted to develop a LC-QTOF MS combined with LC-TQ MS method to precisely characterize the chemicals of Si-Ni-San (SNS), a classic traditional Chinese medicine formula, which is compos...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2020.113816
更新日期：2021-02-05 00:00:00
abstract：:An improved high performance liquid chromatographic assay for plasma-unbound atenolol is described. The assay has a wide range (10-5000 ng ml-1) of linearity and a detection limit of 5 ng ml-1 (or 0.1 ng per injection) with acceptable intra- and inter-assay reproducibilities using small volumes of plasma (100 microlit...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(96)01760-8
更新日期：1996-06-01 00:00:00
abstract：:Valproic acid (VA) is a drug widely used to treat epilepsy and bipolar disorder, at recommended serum concentrations ranging form 50 to 100μg ml(-1). A novel option for therapeutic drug monitoring that has been emerging recently its testing using dried blood spots on paper (DBS), but there are no reports of its applic...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 临床试验,杂志文章
doi：10.1016/j.jpba.2014.03.044
更新日期：2014-08-05 00:00:00
abstract：:4-Nitrobenzaldehyde is the synthetic raw material and an important photodegradation product of chloramphenicol. With a structural "alert" of human genotoxic potential and reported mutagenicity, this compound should be controlled in drug substances as a potential genotoxic impurity. However, current analysis methods re...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2018.04.024
更新日期：2018-07-15 00:00:00
abstract：:A simple and sensitive high-performance liquid chromatographic method for the determination of piperacillin in plasma is described. A C8 reversed-phase column was used with a mobile phase consisting of methanol-water-triethylamine (550:450:4, v/v/v) adjusted to pH = 3 with orthophosphoric acid and UV detection at 270 ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(91)80142-v
更新日期：1991-01-01 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：:In this paper a novel electrochemical sensor based on nickel carbide (Ni3C) nanoparticles as a new modifier was constructed. Ni3C nanoparticle was synthesized and characterized by scanning electron microscopy, X-ray diffraction and first-principles study. Electrochemical impedance spectroscopy (EIS) and cyclic voltamm...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2017.02.032
更新日期：2017-05-30 00:00:00
abstract：:UPLC-UV and HPLC-TOF-MS methods have been developed for the analysis of major sesquiterpenes and pyrrolizidine alkaloids from rhizomes of Petasites hybridus (L.) G.M. et Sch. (Family, Asteracea) and dietary supplements claiming to contain P. hybridus. The best results were obtained with Acquity UPLC™ HSS T3 (100 mm × ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2012.05.021
更新日期：2012-11-01 00:00:00
abstract：:An accurate and specific gas chromatography-mass spectrometry (GC-MS) method was optimized to quantify specific polyunsaturated fatty acids (PUFAs) in plasma and in erythrocyte membranes for clinical purposes. The developed and fully-validated method showed optimal linearity in addition to adequate results in terms of...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2019.07.012
更新日期：2019-11-30 00:00:00
abstract：:A rapid and simple LC-MS/MS method was developed and validated for the simultaneous determination of coniferyl ferulate (CF) and its metabolite coniferyl alcohol (CA) using bavachromene as an internal standard (IS). A TSQ Quantum Access mass spectrometer was operated under selected-reaction monitoring mode using negat...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2017.08.033
更新日期：2017-11-30 00:00:00
abstract：:Human milk oligosaccharides (HMOs) are complex carbohydrates that exist naturally in mother's milk. Due to their myriad beneficial biological effects, HMOs are in the focus of current researches. Some of these complex carbohydrates are already commercially available utilizing their health-promoting benefits not just i...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2020.113184
更新日期：2020-05-30 00:00:00
abstract：:Omega-3 fatty acids are clinically useful and the two marine omega-3 fatty acids eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) are prevalent in fish and fish oils. Omega-3 fatty acid formulations should undergo a rigorous regulatory step in order to obtain United States Food and Drug Administration (USFDA...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2017.04.002
更新日期：2017-07-15 00:00:00
abstract：:Derivatization of the free cys3,4 in human albumin, which is reported to occur under physiological conditions, has been performed in vitro by reaction of the protein with ethacrynic acid. This modification has been investigated by mass spectrometry and circular dichroism. Ethacrynic acid has been proven to bind human ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(98)00163-0
更新日期：1998-10-01 00:00:00
abstract：:Docetaxel is a semi-synthetic taxane with cytotoxic anti-neoplastic activity and, currently used as anticancer agent in several types of cancer. Docetaxel is highly bound to plasma proteins, and this significantly determines its clearance and activity. Therefore, measurement of free docetaxel in plasma is pharmacologi...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2015.08.025
更新日期：2016-01-05 00:00:00
abstract：:The aim of this study was to evaluate the relationship between serum levels of beta-trace protein (BTP), a low molecular weight (MW) protein, and glomerular filtration rate (GFR). GFR and serum levels of BTP, and for comparison creatinine (Creat), cystatin C (Cys) and beta 2-microglobulin (beta 2M), were measured in 6...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(03)00215-2
更新日期：2003-08-08 00:00:00
abstract：:A sensitive and simple high-performance liquid chromatography (HPLC) method was developed and validated for the analysis of amoxicillin in mouse serum and broncho-alveolar lavage (BAL) fluid. One hundred microlitres of sample were needed for the assay. Sample processing was carried out with liquid-liquid extraction. C...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2005.04.021
更新日期：2005-09-15 00:00:00
abstract：:Sinoporphyrin sodium (DVDMS) is a new photosensitizer (PS) and it is used in photodynamic therapy (PDT) against tumor. In this paper, a simple, rapid and specific ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the quantitation of DVDMS in human plasma was developed. The analyt...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2020.113852
更新日期：2021-02-20 00:00:00
abstract：:In this work, dissociation constants values of seven beta lactam antibiotics in water and acetonitrile-water mixtures using spectrophotometric and reversed phase liquid chromatography methods were determined. The dissociation constant values of these compounds were calculated by NLREG and STAR programs. Aqueous pK(a) ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2012.06.023
更新日期：2012-12-01 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：:A sensitive and specific method for the determination of bifendate in human plasma was developed, based on high-performance liquid chromatography (HPLC)-mass spectrometry (MS). The samples were extracted from plasma with diethyl ether, followed by separation and evaporation after addition of internal standard diazepam...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 临床试验,杂志文章
doi：10.1016/j.jpba.2005.08.007
更新日期：2006-03-03 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：:Chlorogenic acids and derivatives like phenolic acids are potentially bioactive phenolics, which are commonly found in many foods. Once absorbed, chlorogenic and phenolic acids are highly metabolized by the intestine and the liver, producing glucuronidated and/or sulphated compounds. These metabolites were analyzed in...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2013.10.009
更新日期：2014-01-01 00:00:00
