Detection of flunixin in equine urine using high-performance liquid chromatography with particle beam and atmospheric pressure ionization mass spectrometry after solid-phase extraction

Stanley, Shawn M.R.; Owens, Nicholas A.; Rodgers, J.P.

doi:10.1016/0378-4347(94)00603-3

Cited by 23 publications

(8 citation statements)

References 16 publications

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“…In the literature, fragments of piroxicam have been reported using ESI‐MS in the positive ion mode22 and for negative chemical ionisation by PB‐MS 23. While fragmentation of the molecular cation of piroxicam is completely different,22 m/z 267 and 211 have been reported as the two most intense fragment ions of m/z 331 upon negative chemical ionisation,23 corresponding to losses of SO 2 and the side chain, respectively. This is consistent with the collision induced dissociation (CID) fragmentation behaviour observed here for the molecular anion m/z 330.…”

Section: Resultsmentioning

confidence: 99%

Sensitive determination of acidic drugs and triclosan in surface and wastewater by ion‐pair reverse‐phase liquid chromatography/tandem mass spectrometry

Quintana

Reemtsma

2004

Rapid Comm Mass Spectrometry

149

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A new method is presented for the determination of 12 acidic pharmaceuticals (non-steroidal anti-inflammatory drugs and bezafibrate), including two metabolites from aqueous samples, together with triclosan as a personal care product. Ion-pair liquid chromatography (IP-LC) with electrospray ionisation tandem mass spectrometry (ESI-MS) in the negative ion mode was employed. The ion-pairing agent (tri-n-butylamine) increased the signal intensity for all acidic analytes and detection limits of 6-200 ng/L were obtained by multiple reaction monitoring. This allows analysis of wastewater samples by direct injection into the LC/MS system without the need for a preceding enrichment step. When combined with a solid-phase extraction (SPE) step, limits of quantification between 0.15 and 11 ng/L were obtained from 100-mL sample volumes, which is adequate for most applications. The occurrence of matrix effects was studied and standard addition was required for reliable quantification after SPE from wastewater. The method was finally applied to surface and wastewaters, with analyte concentrations ranging from below the detection limit up to 5.5 microg/L.

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Section: Resultsmentioning

confidence: 99%

Sensitive determination of acidic drugs and triclosan in surface and wastewater by ion‐pair reverse‐phase liquid chromatography/tandem mass spectrometry

Quintana

Reemtsma

2004

Rapid Comm Mass Spectrometry

149

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“…Sheng et al [25] developed and validated a liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS-MS) method for simultaneous analysis of nine acidic pharmaceutical drugs (bezafibrate, clofibric acid, diclofenac, fenoprofen, gemfibrozil, ibuprofen, indomethacin, ketoprofen and naproxen) in sewage treatment plant (STP) effluents. A normal-phase HPLC method combined with particle-beam mass spectrometry (PB-MS) was developed for the analysis of NSAIDs by Stanley et al [26]. The forty one NSAIDs analysed responded in one or more (electron impact, positive and negative chemical ionisation) modes and highly characteristic spectra were produced.…”

Section: Liquid Chromatography Coupled To Mass Spectrometry (Lc-ms)mentioning

confidence: 99%

Sample Pretreatment and Determination of Non Steroidal Anti-Inflammatory Drugs (NSAIDs) in Pharmaceutical Formulations and Biological Samples (Blood, Plasma, Erythrocytes) by HPLC-UV-MS and μ-HPLC

Sultan¹,

Stecher²,

Stöggl³

et al. 2005

Current Medicinal Chemistry

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The article discusses the qualitative and quantitative determination of non-steroidal antiinflammatory drugs like salicin, salicylic acid, tenoxicam, ketorolac, piroxicam, tolmetin, naproxen, flurbiprofen, diclofenac and ibuprofen by reversed phase high performance liquid chromatography (RP-HPLC) and micro-HPLC (µ-HPLC) hyphenated with UV-absorbance and mass spectrometric detection. Both detection methods delivered calibration plots with good linearity (r 2 > 0.9800), limits of detection in the low nanogram range and recovery rates between 94 and 104 %. For the analysis of biological samples such as blood, plasma and erythrocytes liquid-liquid extraction (LLE) and solid phase extraction (SPE) on the basis of new synthesized glycidylmethacrylate/divinylbenzene copolymer (GMA/DVB) particles and commercially available material on the basis of poly(divinylbenzene-co-N-vinylpyrrolidone) copolymer were investigated. Finally the use of a µ-HPLC system with separation columns in the range of 8 cm × 200 µm I.D. for the determination of non-steroidal anti-inflammatory drugs (NSAIDs) is presented, emphasizing on the type of column and sample amount needed.

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“…Literature data for analysis of NSAIDs indicate extraction and cleanup procedures for the determination of one or two compounds,3, 7–20 with mass spectrometry as the main detection technique. No literature data were found on multi‐residue methods in bovine muscle for structurally different compounds.…”

Section: Maximum Residue Limits (Mrls) Set For Nsaids In Bovine Musclementioning

confidence: 99%

Multi‐residue liquid chromatography/tandem mass spectrometry method for the detection of non‐steroidal anti‐inflammatory drugs in bovine muscle: optimisation of ion trap parameters

Hoof

Wasch

Poelmans

et al. 2004

Rapid Comm Mass Spectrometry

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A multi-residue liquid chromatography/tandem mass spectrometry method (LC/MS2) was developed for the detection of the non-steroidal anti-inflammatory drugs acetylsalicylic acid (via the marker residue salicylic acid), flunixin, phenylbutazone, tolfenamic acid, meloxicam and ketoprofen, in bovine muscle. After extraction of the bovine muscle with acetonitrile, the cleanup was performed using a Oasis HLB column. The evaporated eluate was reconstituted and analysed by LC/MS2. To obtain optimal detection of salicylic acid and phenylbutazone, the ion trap mass spectrometric parameters activation q and maximum ion injection time, respectively, were optimised. The activation q for salicylic acid was increased to obtain reliable detection of both salicylic acid and its product ion. The maximum ion injection time for the time segment containing phenylbutazone was decreased since there were not enough scans across the chromatographic peak of this compound. The multi-residue method was able to detect the different analytes below or at the maximum residue limit (MRL) or minimum required performance limit (MRPL) or, in the case of phenylbutazone and ketoprofen, at 100 and 20 microg kg(-1), respectively.

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Detection of flunixin in equine urine using high-performance liquid chromatography with particle beam and atmospheric pressure ionization mass spectrometry after solid-phase extraction

Cited by 23 publications

References 16 publications

Sensitive determination of acidic drugs and triclosan in surface and wastewater by ion‐pair reverse‐phase liquid chromatography/tandem mass spectrometry

Sensitive determination of acidic drugs and triclosan in surface and wastewater by ion‐pair reverse‐phase liquid chromatography/tandem mass spectrometry

Sample Pretreatment and Determination of Non Steroidal Anti-Inflammatory Drugs (NSAIDs) in Pharmaceutical Formulations and Biological Samples (Blood, Plasma, Erythrocytes) by HPLC-UV-MS and μ-HPLC

Multi‐residue liquid chromatography/tandem mass spectrometry method for the detection of non‐steroidal anti‐inflammatory drugs in bovine muscle: optimisation of ion trap parameters

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