Determination of aliphatic amines by gas chromatography–mass spectrometry after in-syringe derivatization with pentafluorobenzoyl chloride

Singh, Deepak Kumar; Sanghi, Sunil Kumar; Gowri, Sorna; Chandra, Navin; Sanghi, Shail Bala

doi:10.1016/j.chroma.2011.06.022

Cited by 22 publications

(9 citation statements)

References 42 publications

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“…Compared with those of the reported direct CE-AD methods, [16][17][18][19] the LOD of EDA was remarkably reduced (13 pg/mL vs. 0.1 μmol/L-10 ng/mL) by the proposed method, which was nearly equivalent to those of HPLC-LIF [8] (0.5 nmol/L) and GC-MS [10] (1 pg/mL); and relatively good repeatability has been obtained based on short separation capillary. Besides, theophylline in Aminophylline Tablets does not interfere with the determination of EDA.…”

Section: Discussionmentioning

confidence: 42%

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Fast Determination of Ethylendiamine in Aminophylline Tablets by Small‐sized Capillary Electrophoresis with Amperometric Detection

Tong

et al. 2013

Chin. J. Chem.

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A novel method for fast determination of ethylendiamine (EDA) in Aminophylline Tablets has been developed by small-sized capillary electrophoresis with amperometric detection (small-CE-AD) coupled with field-amplified sample injection (FASI). Under the optimum conditions, EDA and four aliphatic diamine homologs (1,3-diaminopropane, 1,4-diaminobutane, 1,5-diaminopentane and 1,6-diaminohexane) could be well separated within 6 min at a separation voltage of 2.0 kV in an acetate buffer solution of pH 3.8 with low limit of detection (LOD) of 1.3×10−11 g/mL for EDA (S/N＝3). The proposed method has been successfully applied to direct determination of EDA content in different batches of Aminophylline Tablets. The method does not require off-line preconcentration and derivatization steps, which should find wide application fields including pharmaceuticals as an alternative to conventional and microchip CE approaches.

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Section: Discussionmentioning

confidence: 42%

“…[6][7][8][9][10] High performance liquid chromatography (HPLC) [11] and gas chromatography (GC) [12,13] have been employed for the purpose. However, the above methods still have some drawbacks of low sensitivity, complicated derivatization procedures or high analytical cost.…”

Section: Introductionmentioning

confidence: 99%

Fast Determination of Ethylendiamine in Aminophylline Tablets by Small‐sized Capillary Electrophoresis with Amperometric Detection

Tong

et al. 2013

Chin. J. Chem.

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“…The obtained results also demonstrated that even in cases where the derivatization reaction is performed on the fiber, Although this analysis time is comparable or slightly higher with respect to other derivatization SPME protocols [2,14,[25][26][27], it has the advantage of avoiding the addition of the derivatization agent to each sample which, can potentially constitute an additional source of error in the analysis routine. On the other hand, other extraction techniques such as vortex assisted liquidliquid microextraction [28], micro extraction in packed syringe (MEPS) [29], single drop microextraction (SDME) [30], air-assisted liquid-liquid microextraction (AALLME) [9], in syringe derivatization [6] used for determination of derivatized amines often lack automation options, employ organic solvents and include tedious procedures.…”

Section: Optimization Of Reaction Conditions In Aqueous Phasementioning

confidence: 99%

“…Amines undergo several derivatization reactions, which have been widely reviewed in the literature [3][4][5]. Acylation of the amino group with pentafluorobenzoyl chloride as a derivatization reagent was tested for the first time by Sanghi et al [6]. Silylation reaction was reported by Casal et al for the analysis of heterocyclic aromatic amines (HAAs) as their tert-butyldimethylsilyl (TBDMS) derivatives [7].…”

Section: Introductionmentioning

confidence: 98%

A facile and fully automated on-fiber derivatization protocol for direct analysis of short-chain aliphatic amines using a matrix compatible solid-phase microextraction coating

Gionfriddo

Passarini

Pawliszyn

2016

Journal of Chromatography A

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Solid-phase microextraction (SPME) analysis of short-chain aliphatic amines (C3-C6) in aqueous solutions was investigated using pentafluorobenzaldehyde (PFBAY) as on-fiber derivatization reagent. A standard gas generating vial agent was used for on-fiber loading of the derivatization agent so as to avoid the need for its regeneration at each derivatization cycle. Several parameters such as loading time, reaction temperature, and reaction/extraction time were optimized for headspace and direct sampling in aqueous solutions. Three different coating chemistries were tested and their performances compared in order to achieve the best compromise between sensitivity and analysis throughput. The newly developed PDMS/DVB/PDMS coating showed superior performance in terms of extraction efficiency while the capability to prevent on-fiber degradation of the derivatizing products. The optimized method was used for quantitation of short-chain aliphatic amines in aqueous samples and provided detection limits in the low ppb range for all the amines tested with accuracy values between 79 and 120%. The method was applied towards the analysis of environmental water samples and the accuracy of the results was evaluated by different calibration approaches.

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“…Sample preparation remains one of the more time-consuming and error-prone aspects of analytical chemistry. To overcome drawbacks of conventional extraction techniques, alternative miniaturized methods have been proposed both as solid phase microextraction, as Solid Phase MicroExtraction (SPME) [7][8][9], MicroExctraction by Packed Sorbent (MEPS) [10], Stir Bar Sorptive Extraction (Twister, SBSE) [11], Solid Phase Dynamic Extraction (Magic Needle, SPDE) [12], In-Tube Extraction (ITEX) [13] and liquid phase microextraction like Single-Drop MicroExtraction (SDME) [14], Hollow Fiber LiquidPhase Microextraction (HF-LPME) [15,16], Dispersive Liquid-Liquid Microextraction (DLLME) [17], Solvent Bar MicroExtraction (SBME) [18]. On-sample derivatizations applied in miniaturized extraction systems and their simultaneous GC and liquid chromatography analysis has been described for the determination of analytes in aqueous matrices [19,20].…”

Section: Introductionmentioning

confidence: 99%

Polymerization Inhibitors and Promoters for Unsaturated Polyester Resins; Use of Solid Phase MicroExtraction and Gas Chromatography Coupled to Mass Spectrometry for the Determination of 4-tert-Butyl Catechol and Acetylacetone

Dugheri¹,

Gentili²,

Bonari³

et al. 2017

Eurasian J Anal Chem

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This paper reports a contribution of three on-sample derivatization sampling techniques for acetylacetone, 4-tert-butyl catechol and its oxidated derivatives 4-tert-butyl-1,2-benzoquinone determination in unsaturated polyester resins. The use of O- (2,3,4,5,6, pentafluorobenzyl)-hydroxylamine, trimethyloxonium tetrafluoroborate and O-methylhydroxylamine is combined with automated head space/solid phase microextraction and gas chromatography/mass spectrometry analysis. For an innovative powerful meaning in high-throughput routine, the generality of the structurally informative mass spectrometry fragmentation patterns together with the chromatographic separation are also investigated. The detection limits for these polymerization inhibitors and promoters are less than 27 pg for one mg of unsaturated polyester resin. In this study a new autosampler platform is proposed by using the Multi Fiber Exchange device in a xyz robotic system. We promote these methods as the analytical reference in the polyester resin field. The introduction of dedicated, automated, and robotic systems allowed a friendly use of MS apparatus for high-throughput screening and it reduces the costs of monitoring campaigns.

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Determination of aliphatic amines by gas chromatography–mass spectrometry after in-syringe derivatization with pentafluorobenzoyl chloride

Cited by 22 publications

References 42 publications

Fast Determination of Ethylendiamine in Aminophylline Tablets by Small‐sized Capillary Electrophoresis with Amperometric Detection

Fast Determination of Ethylendiamine in Aminophylline Tablets by Small‐sized Capillary Electrophoresis with Amperometric Detection

A facile and fully automated on-fiber derivatization protocol for direct analysis of short-chain aliphatic amines using a matrix compatible solid-phase microextraction coating

Polymerization Inhibitors and Promoters for Unsaturated Polyester Resins; Use of Solid Phase MicroExtraction and Gas Chromatography Coupled to Mass Spectrometry for the Determination of 4-tert-Butyl Catechol and Acetylacetone

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