Trace level determination of chloroacetyl chloride and degradation products by derivatization gas chromatography.

Abstract:

:A gas chromatographic procedure has been developed for the trace determination of chloroacetyl chloride (CAC) and two of its impurities: methyl chloroacetate (MCA) and chloroacetic acid (CAA). All three compounds are derivatized using piperidine in dichloroethane prior to their analysis via gas chromatography coupled with a flame ionization detection (GC-FID). Recoveries of each compound were assessed in two different pharmaceutical matrices (intermediate and final active pharmaceutical ingredient) and ranged from 75 to 125%. The limit of quantitation has been determined to be 0.10% wt/wt for CAA and 0.03% wt/wt for CAC and MCA. The linearity ranged from 0.03 to 5.00% wt/wt for CAC and MCA and from 0.10 to 5.00% wt/wt for CAA, with correlation coefficients from 0.9995 to 1.0000. Repeatability was evaluated at LOQ and at 5.00% wt/wt and was found to be between 1.4-3.0%.

journal_name

J Pharm Biomed Anal

authors

Morissette MF,Wigman L,Tso J

doi

10.1016/j.jpba.2017.09.026

subject

Has Abstract

pub_date

2018-01-30 00:00:00

pages

93-99

eissn

0731-7085

issn

1873-264X

pii

S0731-7085(17)30840-3

journal_volume

148

pub_type

杂志文章
  • Clara cell secretory protein: determination of serum levels by an enzyme immunoassay and its importance as an indicator of bronchial asthma in children.

    abstract::Clara cell secretory protein (CC16) is a 16kDa protein secreted by Clara cells in the lining fluid of bronchiolar and bronchial epithelium. CC16 presents several biologic properties, and has been shown to have immunomodulatory and anti-inflammatory activity. It may play a role in controlling inflammation in the airway...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/S0731-7085(03)00570-3

    authors: Gioldassi XM,Papadimitriou H,Mikraki V,Karamanos NK

    更新日期:2004-03-01 00:00:00

  • Use of artificial neural networks to predict quaternery phase systems from limited experimental data.

    abstract::The aim of the present work was to develop a method for predicting the phase behaviour of four component systems consisting of oil, water and two surfactants from a limited number of screening experiments. Investigations were conducted to asses the potential of artificial neural networks (ANNs) with back-propagation t...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/s0731-7085(98)00232-5

    authors: Alany RG,Agatonovic-Kustrin S,Rades T,Tucker IG

    更新日期:1999-03-01 00:00:00

  • Europium(III) ion probe spectrofluorometric determination of diclofenac sodium.

    abstract::A new method has been devised for the determination of diclofenac sodium in bulk and in pharmaceutical preparations using Eu3+ ions as the Fluorescent probe. The technique was built around the hypersensitive property of the transitions of the fluorescent probe ion, Eu3+, at 616 nm. This is normally a forbidden transit...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/0731-7085(95)01567-5

    authors: Carreira LA,Rizk M,el-Shabrawy Y,Zakhari NA,Toubar SS

    更新日期:1995-10-01 00:00:00

  • One-step fabrication of trimetallic alloy nanozyme catalyzer for luminol-H2O2 chemiluminescence and its application for miRNA-21 detection coupled with miRNA walking machine.

    abstract::PtCuCo trimetallic alloys (PtCuCo-TAs) are synthesized by one-step reduction. The chemiluminescence (CL) properties of PtCuCo-TAs are studied systemically. PtCuCo-TAs show good catalyzing for luminol-H2O2 system. A CL platform is developed for the detection of miRNA-21 using PtCuCo-TAs as nanozyme catalyzer. In the CL...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2020.113280

    authors: Mei S,Liu B,Xiong X,Hun X

    更新日期:2020-07-15 00:00:00

  • Validation of a simple HPLC-UV method for rifampicin determination in plasma: Application to the study of rifampicin arteriovenous concentration gradient.

    abstract::In clinical practice, rifampicin exposure is estimated from its concentration in venous blood samples. In this study, we hypothesized that differences in rifampicin concentration may exist between arterial and venous plasma. An HPLC-UV method for determining rifampicin concentration in plasma using rifapentine as an i...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2016.02.013

    authors: Goutal S,Auvity S,Legrand T,Hauquier F,Cisternino S,Chapy H,Saba W,Tournier N

    更新日期:2016-05-10 00:00:00

  • Comparison of reversed phase and reversed phase ion pair high performance liquid chromatography for analysis of TcO and TcN complexes of L,L-ethylene dicysteine di-ethylester and its acid analogues.

    abstract::99mTc(V)-oxo complexes of L,L-ethylene dicysteine (L,L-EC) and its di-ester derivative L,L-ethyl cysteinate dimer (L,L-ECD) are useful tracer agents for evaluation of renal function and cerebral blood flow respectively. Labelling of these molecules with a 99mTc(V)-nitrido core instead of the 99mTc(V)-oxo core alters t...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/s0731-7085(96)01736-0

    authors: Mang'era KO,Bellande E,Pasqualini R,Verbruggen A

    更新日期:1996-06-01 00:00:00

  • Mechanism driven structural elucidation of forced degradation products from hydrocortisone in solution.

    abstract::Hydrocortisone degradation products 1, 2, 3, and 4 along with hemiacetal derivatives 5, 6, 7, and 8 were observed through stressed hydrocortisone in solution. Their structures were identified based on HPLC-UV, HPLC-MS, and HPLC-HRMS (high resolution/high accuracy mass spectrometry) analyses as well as reaction mechani...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2016.06.004

    authors: Zhang F,Zhou J,Shi Y,Tavlarakis P,Karaisz K

    更新日期:2016-09-05 00:00:00

  • Analysis of nifedipine and its pyridine metabolite dehydronifedipine in blood and plasma: review and improved high-performance liquid chromatographic methodology.

    abstract::A reversed-phase HPLC method is described for the simultaneous determination of nifedipine and its primary pyridine metabolite dehydronifedipine in blood and plasma, that involves UV detection and neutral (blood) or alkaline (plasma) extraction. The limit of reliable determination is found to be 3 ng ml-1 with an inte...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章,评审

    doi:10.1016/0731-7085(91)80249-9

    authors: Soons PA,Schellens JH,Roosemalen MC,Breimer DD

    更新日期:1991-01-01 00:00:00

  • Development of chromatographic methods for the determination of genotoxic impurities in cloperastine fendizoate.

    abstract::The classification of an impurity of a drug substance as genotoxic means that the "threshold of toxicological concern" (TTC) value of 1.5 μg/day intake, considered to be associated with an acceptable risk, should be the admissible limit in the raw material and that leads to new analytical challenges. In this study, re...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2011.12.014

    authors: García A,Rupérez FJ,Ceppa F,Pellati F,Barbas C

    更新日期:2012-03-05 00:00:00

  • Stability-indicating UPLC method for determination of Imatinib Mesylate and their degradation products in active pharmaceutical ingredient and pharmaceutical dosage forms.

    abstract::A simple, precise, accurate stability-indicating gradient reverse phase ultra-performance liquid chromatographic (RP-UPLC) method was developed for quantitative determination of purity of Imatinib Mesylate (IMM) drug substance and drug products in the presence of its process related impurities, and degradation product...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2012.03.022

    authors: Nageswari A,Reddy KV,Mukkanti K

    更新日期:2012-07-01 00:00:00

  • Identification of reaction products between drug substances and excipients by HPLC-SPE-NMR: ester and amide formation between citric acid and 5-aminosalicylic acid.

    abstract::The reaction between the high-dose drug substance 5-aminosalicylic acid (5-ASA) and the excipient citric acid during storage of an experimental enema preparation has been studied and three isobaric reaction products, i.e., an ester and an amide with non-symmetrically substituted citric acid moieties and a symmetrical ...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2008.12.028

    authors: Larsen J,Staerk D,Cornett C,Hansen SH,Jaroszewski JW

    更新日期:2009-04-05 00:00:00

  • The characterisation of the major metabolite of salmeterol in the dog.

    abstract::Salmeterol xinafoate is the first of a new class of long acting, selective beta2-adrenoceptor agonists introduced for the treatment of asthma. The major metabolite of salmeterol in the dog has been identified as the 3-catechol sulphate of the benzoic acid derivative. This metabolite was isolated from dog bile and was ...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/s0731-7085(98)00114-9

    authors: Bowers GD,Bayliss MK,Donnelly MC,Fellows I,Ismail IM,Mookherjee CR

    更新日期:1998-11-01 00:00:00

  • Analysis of ACE-inhibitors by CE using alkylsulfonic additives.

    abstract::Capillary electrophoresis (CE) was applied to the determination of angiotensin-converting enzyme (ACE) inhibitors in pharmaceuticals (tablets). Since a free solution CE system failed to reach a complete separation of closely related compounds (lisinopril, ramipril, benazepril, quinapril), alkylsulfonic additives (sodi...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/s0731-7085(00)00240-5

    authors: Gotti R,Andrisano V,Cavrini V,Bertucci C,Furlanetto S

    更新日期:2000-04-01 00:00:00

  • Treatment of selected pharmaceuticals by ferrate(VI): performance, kinetic studies and identification of oxidation products.

    abstract::The performance of ferrate(VI) in treating sulfamethoxazole (SMX), diclofenac (DCF), carbamazepine (CBZ) and bezafibrate (BZF) in test solutions containing the four compounds was investigated. A series of jar-test experiments was performed on a bench-scale at pH 6-9 and at a ferrate(VI) dose of 1-5 mg Fe/L. The result...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2014.06.032

    authors: Zhou Z,Jiang JQ

    更新日期:2015-03-15 00:00:00

  • Microwave-assisted extraction followed by salting-out phase separation for hierarchical screening of illegal adulterants in aphrodisiac health products by multi-dimensional fingerprint profiling analysis.

    abstract::A novel method for hierarchical screening of illegal adulterants in Fur seal ginseng pills (FSGP) products was developed by microwave-assisted extraction (MAE) coupled to salting-out assisted liquid-liquid extraction (SALLE) with multi-dimensional fingerprint profiling analysis. Using a homogeneous system formed by di...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2020.113774

    authors: Wang K,Jin P,Pi J,Xie X,Zhang Y,Yue Z,Mai X,Fan H,Zhang W

    更新日期:2021-02-05 00:00:00

  • Determination of chromatographic and spectrophotometric dissociation constants of some beta lactam antibiotics.

    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

    authors: Demiralay EÇ,Koç D,Daldal YD,Cakır C

    更新日期:2012-12-01 00:00:00

  • Development and validation of a high-performance liquid chromatographic stability-indicating method for the analysis of Synercid in quality control, stability and compatibility studies.

    abstract::A gradient high-performance liquid chromatographic (HPLC) method was developed for the analysis of Synercid freeze-dried powder in routine quality control, stability and compatibility studies. This method is suited for a simultaneous assay of drug substances and impurities. The method was validated for precision, repr...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/s0731-7085(98)00242-8

    authors: Vasselle B,Gousset G,Bounine JP

    更新日期:1999-04-01 00:00:00

  • Improved high performance liquid chromatographic analysis of omeprazole in human plasma.

    abstract::A simple high-performance liquid chromatographic method was developed for the determination of omeprazole in human plasma. Omeprazole and the internal standard, chloramphenicol, were extracted from alkalinized plasma samples using dichloromethane. The mobile phase was 0.05 M Na2HPO4-ACN (65:35, v/v) adjusted to pH 6.5...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/s0731-7085(00)00473-8

    authors: Yuen KH,Choy WP,Tan HY,Wong JW,Yap SP

    更新日期:2001-02-01 00:00:00

  • Determination of XLR-11 and its metabolites in hair by liquid chromatography-tandem mass spectrometry.

    abstract::Analysis of drugs in hair is often used as a routine method to obtain detailed information about drug ingestion. However, few studies have been conducted on disposition of synthetic cannabinoids including cyclopropylindoles (UR-144 and XLR-11) and their metabolites in hair. XLR-11 has been widely abused in South Korea...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2015.05.022

    authors: Park M,Yeon S,Lee J,In S

    更新日期:2015-10-10 00:00:00

  • Evaluation of mobile phase gradient supercritical fluid chromatography for impurity profiling of pharmaceutical compounds.

    abstract::The use of gradient supercritical fluid chromatography (SFC) for the impurity profiling of pharmaceutical products is not widely practiced. Historically, the limited advancement in SFC instrumentation and the lag in column development have resulted in marginal sensitivity, selectivity and reproducibility when compared...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2012.05.025

    authors: Alexander AJ,Hooker TF,Tomasella FP

    更新日期:2012-11-01 00:00:00

  • Comparison of free solution capillary electrophoresis and size exclusion chromatography for quantitating non-covalent aggregation of an acylated peptide.

    abstract::There are few methods available for the rapid and precise quantitation of non-covalent aggregation. The very methods used to measure the aggregation can easily disrupt the weak forces holding an aggregate together. This paper describes the novel application of free solution capillary electrophoresis (CE) for the quant...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/s0731-7085(98)00302-1

    authors: Clodfelter DK,Nussbaum MA,Reilly J

    更新日期:1999-04-01 00:00:00

  • Carbohydrates--purity assessment.

    abstract::In this brief review a superficial introduction is given to the important area of biologically active carbohydrates. The complexity of carbohydrate chemistry is considered and the possible uses of carbohydrates as drugs and diagnostic agents are outlined. The analytical tools and methods that are especially useful for...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/0731-7085(86)80007-3

    authors: Bergström K

    更新日期:1986-01-01 00:00:00

  • Investigation of pathogenesis and therapeutic targets of acute myeloid leukemia based on untargeted plasma metabolomics and network pharmacology approach.

    abstract::Acute myeloid leukemia (AML) is a malignant disease originating from bone marrow hematopoietic stem cells, characterized by anemia, hemorrhage, fever, and infection, with low survival rate. However, the pathogenesis of AML is not fully understood at present. In this work, an integrated approach based untargeted metabo...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2020.113824

    authors: Yuan Y,Wu Q,Zhao J,Feng Z,Dong J,An M,Wu G,Qin F,Zhao L

    更新日期:2021-02-20 00:00:00

  • Lipidomics in autoimmune diseases with main focus on systemic lupus erythematosus.

    abstract::Autoimmune diseases (AID) are a heterogeneous group of disorders that have in common a chronic inflammation and dysregulation of the immune system. Systemic lupus erythematosus (SLE) is one of the most frequent systemic autoimmune diseases characterized by autoimmune phenomena in multiple organs. The tests used for ev...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章,评审

    doi:10.1016/j.jpba.2019.06.005

    authors: Ferreira HB,Pereira AM,Melo T,Paiva A,Domingues MR

    更新日期:2019-09-10 00:00:00

  • High-performance liquid chromatography method for the determination of hydrogen peroxide present or released in teeth bleaching kits and hair cosmetic products.

    abstract::This manuscript presents an HPLC/UV method for the determination of hydrogen peroxide present or released in teeth bleaching products and hair products. The method is based on an oxidation of triphenylphosphine into triphenylphosphine oxide by hydrogen peroxide. Triphenylphosphine oxide formed is quantified by HPLC/UV...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2015.01.018

    authors: Gimeno P,Bousquet C,Lassu N,Maggio AF,Civade C,Brenier C,Lempereur L

    更新日期:2015-03-25 00:00:00

  • Determination of S 12024 enantiomers in human plasma by liquid chromatography after chiral pre-column derivatization.

    abstract::S 12024-2 is a new drug in phase II development that possesses cognitive enhancing properties. As its molecular structure has a chiral centre, a stereoselective method for the analysis of both enantiomers in human plasma has been developed. The method involves pre-column derivatization of the amine moiety with a homoc...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/0731-7085(93)80099-m

    authors: Boursier-Neyret C,Baune A,Klippert P,Castagne I,Sauveur C

    更新日期:1993-11-01 00:00:00

  • 750 MHz 1H NMR spectroscopy characterisation of the complex metabolic pattern of urine from patients with inborn errors of metabolism: 2-hydroxyglutaric aciduria and maple syrup urine disease.

    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

    authors: Holmes E,Foxall PJ,Spraul M,Farrant RD,Nicholson JK,Lindon JC

    更新日期:1997-07-01 00:00:00

  • Fluorimetric and spectrophotometric determination of ritodrine hydrochloride in bulk and pharmaceutical formulations.

    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

    authors: Razak OA

    更新日期:1998-11-01 00:00:00

  • Analysis of cationic liposomes by reversed-phase HPLC with evaporative light-scattering detection.

    abstract::Cationic lipid-mediated drug delivery of small pharmaceutical molecules and biological molecules, such as proteins and DNA, has gained increasing popularity for many in vitro and in vivo applications. For this purpose, 1,2-dioleoyl-3-trimethylammonium propane (DOTAP) is one of the most widely used and efficient cation...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2009.10.001

    authors: Zhong Z,Ji Q,Zhang JA

    更新日期:2010-03-11 00:00:00

  • Determination of tramadol in various dosage forms by capillary isotachophoresis.

    abstract::Cationic capillary isotachophoresis (ITP) with conductometric detection has been used for separating and determining milligram amounts of tramadol [2-dimethylaminomethyl-1-(3-methoxyphenyl)-cyclohexanol hydrochloride] (I) in seven commercial mass-produced pharmaceutical preparations. The optimised ITP electrolyte syst...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/s0731-7085(98)00270-2

    authors: Pospísilová M,Polásek M,Jokl V

    更新日期:1998-12-01 00:00:00