LC–MS method for the determination of albuterol enantiomers in human plasma using manual solid-phase extraction and a non-deuterated internal standard

Jacobson, GA; Chong, Fayun; Davies, Noel W.

doi:10.1016/s0731-7085(02)00734-3

Cited by 28 publications

(21 citation statements)

References 13 publications

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“…Finally, each pure enantiomer was eluted with 2 mL of a mixture of methanol/ammonia solution (95:5 v/v) and this solution was then evaporated by means of a Rotavapor. (2)-Salbutamol and (1)-salbutamol were separated by LC according to the procedure of Jacobson et al [27] using a mobile phase consisting of a mixture of methanol/acetic acid/ammonia solution (1000/5/1 v/v/v) at a flow rate of 1.3 mL/min on a teicoplanin-based ASTEC Chirobiotic T column (25064.6 mm ID) from Alltech Associates (Deerfield, IL, USA). Separation took place at 257C.…”

Section: Chromatographic Isolation Of Enantiomersmentioning

confidence: 99%

Enantiomeric separation of basic compounds using heptakis(2,3‐di‐O‐methyl‐6‐O‐sulfo)‐β‐cyclodextrin in combination with potassium camphorsulfonate in nonaqueous capillary electrophoresis: Optimization by means of an experimental design

et al. 2004

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The enantiomeric separation of a series of basic pharmaceuticals (beta-blockers, local anesthetics, sympathomimetics) has been investigated in nonaqueous capillary electrophoresis (NACE) systems using heptakis(2,3-di-O-methyl-6-O-sulfo)-beta-cyclodextrin (HDMS-beta-CD) in combination with potassium camphorsulfonate (camphorSO3-). For this purpose, a face-centered central composite design with 11 experimental points was applied. The effect of the concentrations of HDMS-beta-CD and camphorSO3- on enantioresolution was statistically evaluated and depended largely on the considered analyte. The presence of camphorSO3- was found to be particularly useful for the enantioseparation of compounds with high affinity for the anionic CD. CamphorSO3- seems to act as a competitor, reducing the affinity for the CD, probably by ion-pair formation with these analytes. For compounds with lower affinity for HDMS-beta-CD, the combination of camphorSO3- and the CD appeared to have a favorable effect on enantioresolution only if the optimal CD concentration could be reached. On the other hand, for compounds characterized by a very low affinity for the anionic CD, the association of camphorSO3- and HDMS-beta-CD is always unfavorable. Finally, experimental conditions were selected by means of the multivariate approach in order to obtain the highest resolution (Rs) value for each studied compound.

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Section: Chromatographic Isolation Of Enantiomersmentioning

confidence: 99%

Enantiomeric separation of basic compounds using heptakis(2,3‐di‐O‐methyl‐6‐O‐sulfo)‐β‐cyclodextrin in combination with potassium camphorsulfonate in nonaqueous capillary electrophoresis: Optimization by means of an experimental design

et al. 2004

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“…It is interesting to note that the elution order of enantiomers reversed when acetic acid and ammonium hydroxide in methanol were used. 22 …”

Section: Resultsmentioning

confidence: 99%

“…There have been several assays reported recently for the determination of albuterol enantiomers in plasma. These assays include capillary electrophoresis (CE), 18 chemical derivatization and gas chromatography/mass spectrometry (GC/MS), 19 high-performance liquid chromatography (HPLC) with fluorescence detection, 20 HPLC with electrochemical detection, 21 and solid-phase extraction with LC/ MS. 22 The goal of this research was to develop an automated on-line sample extraction/chiral LC/tandem mass spectrometric method to analyze albuterol enantiomers in dog plasma. This approach implemented turbulent flow chromatography for on-line sample cleanup, and employed a chiral HPLC method for separation using a polar organic mobile phase with MS-compatible additives.…”

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confidence: 99%

High‐throughput chiral analysis of albuterol enantiomers in dog plasma using on‐line sample extraction/polar organic mode chiral liquid chromatography with tandem mass spectrometric detection

Xing

Apedo

et al. 2004

Rapid Comm Mass Spectrometry

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An automated chiral chromatography/tandem mass spectrometry bioanalytical method for the determination of albuterol in dog plasma was developed. The method employed on-line sample extraction using turbulent flow chromatography coupled to a Chirobiotic T column for chiral separation using a polar organic mobile phase consisting of methanol, 0.02% formic acid, and 0.1% ammonium formate. The analytes were detected by a tandem mass spectrometer operated in positive ion mode. The (S)- and (R)-isomers were resolved chromatographically with retention times of 5.1 and 5.6 min, respectively. The analytical run time was 8 min. The enantiomers did not interconvert either in mobile phase or in dog plasma at room temperature over the course of at least 2 h. The assay has a linear dynamic range from 2.5-2500 nM for both enantiomers. The lower limit of quantitation (LLOQ) was 2.5 nM for both enantiomers using 50 microL of plasma. The accuracy and precision of intraday validation were determined at five concentration levels of six replicates. The accuracy of the method for the (R)-isomer ranged from 94-103% of nominal concentrations, and the precision (%CV) ranged from 3.6-12%. The accuracy of the method for the (S)-isomer ranged from 94.5-108% of nominal concentrations, and the precision ranged from 3.2-9.3%. Interday accuracy and precision were evaluated for three days at five concentrations for one replicate. The accuracy of the method for the (R)-isomer ranged from 98-110% of nominal concentrations, and the precision ranged from 1.5-10.6%. The accuracy of the method for the (S)-isomer ranged from 96-104% of nominal concentrations, and the precision ranged from 1.5-8.7%. The combination of turbulent flow on-line sample extraction with polar organic mode chiral chromatography provided a specific, rugged, and high-throughput method for the chiral analysis of albuterol in biological fluids.

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“…Initial results in our laboratory have shown that there is potential for stereoselective uptake into muscle. This current tissue assay has been developed from earlier work in this laboratory [7] and Joyce et al [8] with the objective of detecting albuterol enantiomers at low levels in skeletal and cardiac muscle, liver, and brain for research rather than regulatory purposes. This assay is being used for studies investigating enantioselective uptake pathways relevant to meat production, therapeutic uses in muscle wasting disease and sports doping, and cardiac toxicity in respiratory therapy.…”

Section: Introductionmentioning

confidence: 99%

Determination of Albuterol Enantiomers in Animal Tissue Matrices by LC–MS/MS: Application in Therapeutic Myoanabolic Studies

2011

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Albuterol (salbutamol) is a widely used medication in respiratory disease including asthma and chronic obstructive airways disease; however, like other beta2-agonists, it also exerts some extrapulmonary effects on muscle and fat. Surprisingly, there have been relatively few reports of albuterol tissue distribution, and the distribution of individual albuterol enantiomers into tissue has not been reported. The method presented here explores the use of an HPLC tandem mass spectrometry (LC-MS/MS) system (LTQ Orbitrap hybrid mass spectrometer) with deuterated standard and solid-phase extraction to determine low levels of albuterol enantiomers in tissue. The lower limit of quantification (LLOQ) was 0.156 ng g -1 , with a precision RSD \15% for both enantiomers. The assay was linear over the calibration range of LLOQ-10.0 ng g -1 in muscle tissue (r 2 [ 0.98). The assay was successfully applied to pharmacokinetic studies in rats and mice. By utilizing a deuterated internal standard and LC-MS/MS detection, this assay can be used to measure albuterol enantiomers in muscle tissue. This assay has also identified that albuterol uptake appears to be stereoselective, and enantioselective assays are clearly warranted for myoanabolic studies involving administration of racemic-albuterol.

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LC–MS method for the determination of albuterol enantiomers in human plasma using manual solid-phase extraction and a non-deuterated internal standard

Cited by 28 publications

References 13 publications

Enantiomeric separation of basic compounds using heptakis(2,3‐di‐O‐methyl‐6‐O‐sulfo)‐β‐cyclodextrin in combination with potassium camphorsulfonate in nonaqueous capillary electrophoresis: Optimization by means of an experimental design

Enantiomeric separation of basic compounds using heptakis(2,3‐di‐O‐methyl‐6‐O‐sulfo)‐β‐cyclodextrin in combination with potassium camphorsulfonate in nonaqueous capillary electrophoresis: Optimization by means of an experimental design

High‐throughput chiral analysis of albuterol enantiomers in dog plasma using on‐line sample extraction/polar organic mode chiral liquid chromatography with tandem mass spectrometric detection

Determination of Albuterol Enantiomers in Animal Tissue Matrices by LC–MS/MS: Application in Therapeutic Myoanabolic Studies

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