Simultaneous determination of fatty, dicarboxylic and amino acids based on derivatization with isobutyl chloroformate followed by gas chromatography—positive ion chemical ionization mass spectrometry

Sobolevsky, Tim; Revelsky, A. I.; Revelsky, I. A.; Miller, Barbara; Oriedo, Vincent

doi:10.1016/j.jchromb.2003.09.013

Cited by 34 publications

(19 citation statements)

References 31 publications

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“…Samples (50 ml) were removed every 30 min over a 2 h period. The amino acid detection was based on derivatization with isobutyl chloroformate followed by GC-MS, as described elsewhere (Sobolevsky et al, 2004). Briefly, reaction mixture (50 ml) was mixed well with deionized H 2 O (50 ml), isobutanol (30 ml), pyridine (10 ml) and isobutyl chloroformate (30 ml).…”

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confidence: 99%

Analysis of the Pseudomonas putida CA-3 proteome during growth on styrene under nitrogen-limiting and non-limiting conditions

et al. 2009

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Pseudomonas putida CA-3 is a styrene-degrading bacterium capable of accumulating mediumchain-length polyhydroxyalkanoate (mclPHA) when exposed to limiting concentrations of a nitrogen source in the growth medium. Using shotgun proteomics we analysed global proteome expression in P. putida CA-3 supplied with styrene as the sole carbon and energy source under N-limiting (condition permissive for mclPHA synthesis) and non-limiting (condition non-permissive for mclPHA accumulation) growth conditions in order to provide insight into the molecular response of P. putida CA-3 to limitation of nitrogen when grown on styrene. A total of 1761 proteins were identified with high confidence and the detected proteins could be assigned to functional groups including styrene degradation, energy, nucleotide metabolism, protein synthesis, transport, stress response and motility. Proteins involved in the upper and lower styrene degradation pathway were expressed throughout the 48 h growth period under both nitrogen limitation and excess. Proteins involved in polyhydroxyalkanoate (PHA) biosynthesis, nitrogen assimilation and amino acid transport, and outer membrane proteins were upregulated under nitrogen limitation. PHA accumulation and biosynthesis were only expressed under nitrogen limitation. Nitrogen assimilation proteins were detected on average at twofold higher amounts under nitrogen limitation. Expression of the branched-chain amino acid ABC transporter was up to 16-fold higher under nitrogen-limiting conditions. Branched chain amino acid uptake by nitrogenlimited cultures was also higher than that by non-limited cultures. Outer membrane lipoproteins were expressed at twofold higher levels under nitrogen limitation. This was confirmed by Western blotting (immunochemical detection) of cells grown under nitrogen limitation. Our study provides the first global description of protein expression changes during growth of any organism on styrene and accumulating mclPHA (nitrogen-limited growth). INTRODUCTIONPseudomonas putida CA-3 has been reported to utilize styrene as a sole source of carbon and energy and to accumulate the biodegradable polymer medium-chainlength polyhydroxyalkanoate (mclPHA) when nitrogen (N) becomes limited in the growth medium (O'Connor et al., 1996;. These two abilities have been employed in the two-step chemo-biotechnological conversion of polystyrene, a non-biodegradable polymer, to mclPHA at laboratory scale (Ward et al., 2006). The process has been improved through the controlled feeding of N to the growth medium, which results in a twofold increase in biomass and a 1.4-fold increase in mclPHA accumulation (Goff et al., 2007).Molecular investigations of the styrene degradation pathway in this organism have been reported (Mooney et al., 2006b;O'Connor et al., 2001). Styrene metabolism in P. putida CA-3 proceeds via initial side chain oxidation and involves an upper pathway converting styrene to phenylacetic acid (PA) (O'Connor et al., 1995), and a lower pathway initiated via activation of PA to phenylace...

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confidence: 99%

Analysis of the Pseudomonas putida CA-3 proteome during growth on styrene under nitrogen-limiting and non-limiting conditions

et al. 2009

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“…The reagent IBCF is also reported to react with carboxylic group of amino acid and to secondary amino groups to form derivative with extension of carbon chain length [36] and increase in the sensitivity of FID detection. Both the reactions are carried out in aqueous medium.…”

Section: Resultsmentioning

confidence: 99%

Gas Chromatographic Determination of Amino Acids and Polyamines in Human Skin Samples using Trifluoroacetylacetone and Isobutyl Chloroformate as Derivatizing Reagents

Soomro¹,

Khuhawar²,

Soomro³

2014

J Chromatogr Sep Tech

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An analytical method has been developed with improved sensitivity for the determination of amino acids and polyamines after precolumn derivatization with trifluoroacetylacetone and isobutyl chloroformate. 28 compounds comprising of 20 amino acids, five polyamines (1,3 diaminopropane, putrescine, cadverine, spermindine and spermine) and three biogenic compounds (4-aminobutyric acid, histamine and dopamine) separated completely with linear calibration range 1-10 µg/ml and limits of detection 60 -200 ng/ml. The separation was obtained within 11 min from HP-5 (30 m × 0.32 mm id) with column temperature 100°C for 2 min, followed by ramping at the rate of 20°C / min upto 250°C. The nitrogen flow rate was 3.0 ml/min. The method was applied for the analysis of the compounds in human skin samples after acid hydrolysis. The variation in their contents were examined in the affected skin samples from pemphigus vulgaris, psoriasis, leishmaniasis and eczema patients and result were compared with unaffected skin samples from healthy volunteers. The extraction of amino acids and polyamines from samples calculated by standard addition was within 95-102 % with RSDs 1.23-6.75 %.

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“…The DMA, DEA, PA and BA approach their maximum derivatization efficiencies at the IBCF / amine molar ratios > 100, while the molar ratios are > 250 in the case of MA and EA. Given that IBCF can also react with certain amino acids (Sobolevsky et al, 2004), an equivalent molar ratio of IBCF / amine of 500 was selected for the analysis of real samples.…”

Section: Effect Of Ph On the Derivatizationmentioning

confidence: 99%

Determination of alkylamines in atmospheric aerosol particles: a comparison of gas chromatography–mass spectrometry and ion chromatography approaches

Huang

Wang

et al. 2014

Atmos. Meas. Tech.

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Abstract. In recent years low molecular weight alkylamines have been recognized to play an important role in particle formation and growth in the lower atmosphere. However, major uncertainties are associated with their atmospheric processes, sources and sinks, mostly due to the lack of ambient measurements and the difficulties in accurate quantification of alkylamines at trace level. In this study, we present the evaluation and optimization of two analytical approaches, i.e., gas chromatography-mass spectrometry (GC-MS) and ion chromatography (IC), for the determination of alkylamines in aerosol particles. Alkylamines were converted to carbamates through derivatization with isobutyl chloroformate for GC-MS determination. A set of parameters affecting the analytical performances of the GC-MS approach, including reagent amount, reaction time and pH value, was evaluated and optimized. The accuracy is 84.3-99.1 %, and the limits of detection obtained are 1.8-3.9 pg (or 0.02-0.04 ng m −3 ). For the IC approach, a solid-phase extraction (SPE) column was used to separate alkylamines from interfering cations before IC analysis. 1-2 % (v/v) of acetone (or 2-4 % (v/v) of acetonitrile) was added to the eluent to improve the separation of alkylamines on the IC column. The limits of detection obtained are 2.1-15.9 ng (or 0.9-6.4 ng m −3 ), and the accuracy is 55.1-103.4 %. The lower accuracy can be attributed to evaporation losses of amines during the sample concentration procedure. Measurements of ambient aerosol particle samples collected in Hong Kong show that the GC-MS approach is superior to the IC approach for the quantification of primary and secondary alkylamines due to its lower detection limits and higher accuracy.

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Simultaneous determination of fatty, dicarboxylic and amino acids based on derivatization with isobutyl chloroformate followed by gas chromatography—positive ion chemical ionization mass spectrometry

Cited by 34 publications

References 31 publications

Analysis of the Pseudomonas putida CA-3 proteome during growth on styrene under nitrogen-limiting and non-limiting conditions

Analysis of the Pseudomonas putida CA-3 proteome during growth on styrene under nitrogen-limiting and non-limiting conditions

Gas Chromatographic Determination of Amino Acids and Polyamines in Human Skin Samples using Trifluoroacetylacetone and Isobutyl Chloroformate as Derivatizing Reagents

Determination of alkylamines in atmospheric aerosol particles: a comparison of gas chromatography–mass spectrometry and ion chromatography approaches

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