Abstract:
:In terms of risk assessment especially for the impurities with different ultraviolet (UV) absorptions in 16-membered macrolides produced by fermentation, quantification without the availability of corresponding reference substances currently poses a challenge. In this study, a reliable method was established for the analysis of impurities in 16-membered macrolides for the first time by high performance liquid chromatography tandem with charged aerosol detector (HPLC-CAD). The chromatographic conditions and CAD parameters were optimized for a good separation and sensitivity. The impurities were identified by ion trap time-of-flight mass spectrometry (IT-TOF/MS), the developed method was validated, and the sources of degradation impurities in production were investigated. Based on the experimental results, the superiority of the developed method over UV detection was demonstrated that the method provided a universal response to impurities with differences chromophores. In the method validation, good linearity was obtained with coefficient of determination (R2) greater than 0.999 in the range of 2-100 μg·mL-1. The limit of detection (LOD) and limit of quantification (LOQ) were 5 and 15 ng for impurity Ⅲ, respectively. The average content of the impurity Ⅲ was found to be 0.4 % in leucomycin. The recoveries were 98.7 %-102.5 % at the spiked concentration levels of 0.40 %, 0.60 % and 0.80 % with relative standard deviations (RSDs, n=3) lower than 2.0 %. The impurities in 10 leucomycin samples were determined to be 3.2 %-5.2 %. Finally, the acidity of solution during the purification and the temperature of drying process were found to be the main factors that causing the increased amount of impurities. Overall, the developed HPLC-CAD quantification method was a suitable alternative for the analysis of impurities in the 16-membered macrolides discussed in this manuscript. Our study provided guidance for pharmaceutical companies to improve the manufacturing process and control the impurities.
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
Wang J,Liu G,Zhu B,Tang Ldoi
10.1016/j.jpba.2020.113170subject
Has Abstractpub_date
2020-05-30 00:00:00pages
113170eissn
0731-7085issn
1873-264Xpii
S0731-7085(19)33164-4journal_volume
184pub_type
杂志文章abstract::The cardiac troponin T (cTnT) is specific biomarker important for trials of acute myocardial infarctions (AMI). In this paper, a SPR sensor in real time to detect the biomarker was developed on a commercially available surface plasmon resonance AUTOLAB SPIRIT. The cTnT receptor molecule was covalently immobilized on a...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2006.12.013
更新日期:2007-04-11 00:00:00
abstract::The 60 MHz (1)H NMR spectra of racemic thiopental, 1, have been studied with the achiral shift reagent, tris(6,6,7,7,8,8,8-heptafluoro-2,2-dimethyl-3,5-octanedionato) europium(III), 2, and the chiral tris[3-(trifluoromethylhydroxymethylene)-d-camphorato] europium(III), 3, and tris[3-(heptafluoropropylhydroxymethylene)...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(87)80027-4
更新日期:1987-01-01 00:00:00
abstract::Sampatrilat is a dual inhibitor of angiotensin converting enzyme (ACE) and neutral endopeptidase (NEP) under development for the treatment of hypertension and congestive heart failure. In order to support the early clinical development (with oral administration and an expected low bioavailability), a sensitive and sel...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(97)00127-1
更新日期:1998-01-01 00:00:00
abstract::Recently it was found that normal adults excrete pipecolic acid primarily as the D-enantiomer even though it is present in the blood stream mainly as the L-enantiomer (i.e. > 98% L). This study of pipecolic acid stereochemistry was extended to subjects with peroxisomal deficiencies since they are known to have high le...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(93)80044-2
更新日期:1993-10-01 00:00:00
abstract::The 60-MHz 1H NMR spectra of racemic mephenytoin, I, have been studied with the achiral shift reagent, tris(6,6,7,7,8,8,8-heptafluoro-2,2-dimethyl-3,5-octane-dionato) europium (III), II, and the chiral reagent, tris[3-(trifluoromethylhydroxy-methylene)-d-camphorato] europium (III), III. Moderate values of the enantiom...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(84)80043-6
更新日期:1984-01-01 00:00:00
abstract::Ziv-aflibercept (ziv-AFL) is a complex fusion protein which is widely used in hospitals for the treatment of colorectal metastatic cancer. Charge variants are critical attributes for assessing post-transitional modifications (PMTs) that have to be controlled during the development and manufacture of these proteins and...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2020.113233
更新日期:2020-06-05 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::Phytochemical investigation of the methanolic extract of Byrsonima crassifolia's bark led to the isolation of 8 known phenolic compounds 5-O-galloylquinic acid, 3-O-galloylquinic acid, 3,4-di-O-galloylquinic acid, 3,5-di-O-galloylquinic acid, 3,4,5-tri-O-galloylquinic acid, (+)-epicatechin-3-gallate along with (+)-cat...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2011.03.032
更新日期:2011-08-25 00:00:00
abstract::An ultra-sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS) assay was developed and validated to facilitate the assessment of clinical pharmacokinetics of nucleotide analogs from lysed intracellular matrix. The method utilized a strong anion exchange isolation of mono-(MP), di-(DP), and tri-phosphates...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2011.05.039
更新日期:2011-09-10 00:00:00
abstract::A study was performed to compare the pharmacokinetics of major bioactive analytes in rhubarb plants to explore the pharmacological differences between raw pieces (RP) and steamed pieces (SP) of rhubarb. A rapid and efficient ultra-performance liquid chromatographic coupled with mass/mass spectrometry (UPLC-MS/MS) meth...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2019.04.002
更新日期:2019-07-15 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::Sub-micron sized domains of a carbon surface are derivatized with antibodies using biotin/avidin technology. These sites are spatially-segregated from, and directly adjacent to, electron transfer sites on the same electrode surface. The distance between these electron transfer sites and enzyme-loaded domains are kept ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(98)00292-1
更新日期:1999-02-01 00:00:00
abstract::The topical administration of timolol as an ion-pair with octanoate was achieved by use of an oil-in-water microemulsion containing lecithin as a surfactant. The microemulsion, a solution of the ion-pair and a solution of timolol alone were instilled in the conjunctival sac of rabbits. A rapid method for the separatio...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(89)80030-5
更新日期:1989-01-01 00:00:00
abstract::This study demonstrates the use of hydrophilic interaction liquid chromatography with a nano quantity analyte detector for the retention, separation and detection of magnesium from magnesium stearate in tablet formulations for a drug product formulation blend containing a hydrochloride salt of a weakly basic compound ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2013.02.003
更新日期:2013-05-05 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::The Xiao-Xu-Ming decoction (XXMD) is a traditional Chinese medicine prescription that is clinically used for the treatment of stroke. The active fraction of XXMD (AF-XXMD) exhibits pharmacological effects that are similar to those of XXMD. In this study, 21 primary compounds of AF-XXMD with potential anti-ischemic-str...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2016.01.052
更新日期:2016-04-15 00:00:00
abstract::The purpose of this research was to combine microdialysis sampling techniques with a highly sensitive radioimmunoassay (RIA) to study the in vivo kinetic response of pharmacologically important substances. This technique allowed for a dense sampling regimen from an awake, free-roaming experimental animal with no loss ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(91)80021-z
更新日期:1991-01-01 00:00:00
abstract::An analytical methodology using square wave voltammetry (SWV) at a hanging mercury drop electrode (HMDE) was developed for the quantitative determination of dipyridamole (DIP), a drug used for the treatment of several cardiovascular diseases, in pharmaceutical tablets and injections of Persantin in phosphate buffer (p...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2004.09.011
更新日期:2005-01-04 00:00:00
abstract::Spectrophotometric procedures for the determination of two irriversible proton pump inhibitors, omeprazole (OMZ) and pantoprazole (PNZ) sodium have been developed, the procedures are based on the formation of 2:1 chelates of both drugs with different metal ions. Pantoprazole sodium is quantified by a stability-indicat...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(03)00233-4
更新日期:2003-10-15 00:00:00
abstract::A HPLC-MS/MS Electrospray (ESI) method was developed and validated to quantify a peptide conjugate prodrug of doxorubicin (Dox-Con) and its active metabolites leucine-doxorubicin (Leu-Dox) and doxorubicin (Dox) in dog and rat plasma. The analytes were extracted from plasma by solid-phase extraction on a Bond Elut C8 c...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(03)00434-5
更新日期:2003-12-04 00:00:00
abstract::Trans-3,5,4'-trihydroxystilbene (trans-resveratrol, RES) exhibits very low bioavailability due to extensive conjugative metabolism. Whether RES metabolites exhibit pharmacologic activity is of great interest. The present study aimed at synthesis of monoconjugates of RES - the 3- and 4' monosulfates (R3S and R4'S), and...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2011.12.006
更新日期:2012-04-07 00:00:00
abstract::A new extraction technique based on the off-line combination of pressurized-liquid with solid-phase extraction (PLE-SPE) is described. The method was used for the extraction of bioactive phenolic acids (protocatechuic, p-hydroxybenzoic, 2,3-dihydroxybenzoic, chlorogenic, vanillic, caffeic, p-coumaric, salicylic acid),...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2009.03.027
更新日期:2010-01-20 00:00:00
abstract::An automated electronic tongue consisting of an array of potentiometric sensors and an artificial neural network (ANN) has been developed to resolve mixtures of anionic surfactants. The sensor array was formed by five different flow-through sensors for anionic surfactants, based on poly(vinyl chloride) membranes havin...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2007.09.013
更新日期:2008-01-22 00:00:00
abstract::A validated, highly sensitive and selective high-pressure liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the quantitative determination of quetiapine (QUE) in human Na2EDTA plasma with mass spectrometry (MS) detection. Clozapine (CLO) was employed as an internal standard. Samples we...
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.2007.03.034
更新日期:2007-06-28 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::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::Covalent binding of reactive metabolites (RMs) to proteins is thought to play an important role in the processes leading to adverse drug reactions. Therefore, there is great interest in methodologies that enable the characterization of covalent binding of drugs to proteins. To facilitate the study of drug-protein addu...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2012.04.035
更新日期:2012-08-01 00:00:00
abstract::A sensitive and specific liquid chromatography coupled with tandem mass spectrometry (LC/MS/MS) method was developed and validated for the determination of PAC-1 in rat plasma. After extraction with ethyl acetate, the chromatographic separation was carried out on an ACQUITY UPLC™ BEH C(18) column, with acetonitrile an...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2010.07.042
更新日期:2011-01-05 00:00:00
abstract::Two UV spectrophotometric methods have been validated for the analysis of hydrolyzed tinidazole solutions. The pH of the samples must be 5.00-7.00 for both methods. The multiwavelength method may be used for samples degraded at pH 6-12 if the amount of conserved 5-nitroimidazole species is at least 93 mol.% of the ori...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(02)00667-2
更新日期:2003-03-10 00:00:00
abstract::A selective and highly sensitive analytical methodology for determination of Bisphenol A in human plasma was developed and validated. The method was based on selective liquid/solid extraction, combined with liquid chromatography-electrospray ionization tandem mass spectrometry in the multiple reaction monitoring mode ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2017.02.058
更新日期:2017-06-05 00:00:00