Determination of low-molecular-weight amines and ammonium in saline waters by ion chromatography after their extraction by steam distillation

The retention behavior of primary aliphatic amines (homologous series of aliphatic alkyl amines and cycloalkyl amines) and positional isomers of alkylamines in the hydrophilic interaction chromatography mode was studied. The study was carried out on a TSKgel Amide-80 column followed by postcolumn derivatization with fluorescence detection to describe the retention mechanism of tested compounds. The effect of chromatographic conditions including column temperature, acetonitrile content in the mobile phase, mobile phase pH (ranging from 3.5 to 6.8), and salt concentration in the mobile phase was investigated. The final mobile phase consisted of acetonitrile and solution of 20 mM potassium formate pH 3.5 in ratio 80:20 v/v. The analyses were carried out at mobile phase flow rate of 1.0 mL/min and the column temperature of 20°C. The developed method was fully validated in terms of linearity, sensitivity (limit of detection and limit of quantification), accuracy, and precision according to International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use guidelines. The proposed new methods were proved to be highly sensitive, simple, and rapid, and were successfully applied to the determinations of isopropylamine, cyclohexylamine, and cyclopropylamine in relevant active pharmaceutical ingredients.

Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Separation of structurally related primary aliphatic amines using hydrophilic interaction chromatography with fluorescence detection after postcolumn derivatization with o‐phthaldialdehyde/mercaptoethanol

Douša

Doubský

2017

“…Due to their physical and chemical properties (e.g., lack of chromophore, high polarity, and volatility), it is very difficult to determine aliphatic amines at trace level directly from complex matrixes. Determination of aliphatic amines in water samples without derivatization is generally performed by GC , ion chromatography , and MS , combined with various preconcentration techniques. Despite being successfully applied for environmental detection of aliphatic amines, these methods are faced with another specific set of challenges when analyzing complex drug substance samples .…”

Section: Introductionmentioning

confidence: 99%

Simultaneous determination of eight short‐chain aliphatic amines in drug substances by HPLC with diode array detection after derivatization with halonitrobenzenes

Han

Hou

et al. 2017

Short-chain aliphatic amines are a class of hazardous impurities in drug substances. A simple method, involving derivatization followed by high-performance liquid chromatography with diode array detection, has been developed for residue determination of eight aliphatic amines simultaneously in drug substances. Different halonitrobenzenes derivatization reagents were systematically compared. As a result, 1-fluoro-2-nitro-4-(trifluoromethyl)benzene was selected since the derivatization effectively shifted the absorption wavelength to the visible region (400-450 nm), where most drug substances, impurities and even the derivatization reagent absorb very weakly. Due to the redshift effect, interference was minimized and adequately low limits of quantitation were reached (0.24-0.80 nmol/mL). Moreover, the derivatization reaction was readily carried out in dimethyl sulfoxide at room temperature for 1 h using N,N-diisopropylethylamine as catalyst to achieve the highest yield. Without any pre-treatment, the derivatives were analyzed by high-performance liquid chromatography with diode array detection. The high stability of the derivatives within 24 h at room temperature (RSD<1.04%) further facilitated the simultaneous preparation and consecutive analysis of quantities of samples. Finally, the proposed method was successfully applied for residue determination of eight aliphatic amines simultaneously in eight drug substance samples. This study could be helpful for the routine analysis and residue control of aliphatic amines in drug substances.

“… propose an FIA. Some researchers applied ion chromatography , however the sample has to be mightily diluted or distilled or the system was complicated . Despite the fact that the studies of nitrogen determination are particularly often and routinely performed in the laboratory, none of the above solution has found widespread application.…”

Section: Introductionmentioning

confidence: 99%

Simultaneous speciation analysis of inorganic nitrogen with the use of ion chromatography in highly salinated environmental samples

Kurzyca

Niedzielski

Frankowski

2016

We present the development of a method for the simultaneous determination of inorganic nitrogen species in oxidized (NO2 (-) , NO3 (-) ) and reduced (NH4 (+) ) forms using ion chromatography with diode-array detection (205, 208, and 425 nm, respectively). The oxidized forms were determined directly after the separation in the anion exchanger, while the reduced form was determined in the column hold-up time after derivatization with the Nessler reagent. The use of an appropriate modifier (Seignette reagent) and mobile phase (NaCl) enabled the determination of inorganic nitrogen species in highly salinated environmental samples (water, sediments). Moreover, low detection limits were obtained of 0.04 mg/L for NH4 (+) and 0.006 and 0.005 mg/L for NO2 (-) and NO3 (-) , respectively. The analysis of environmental samples indicated NH4 (+) contents of up to 1161 ± 47 mg/kg and NO3 (-) of up to 148 ± 6 mg/kg for sediment samples, as well as the NH4 (+) concentrations of up to 0.98 ± 0.10 mg/L, NO2 (-) of up to 24 ± 1 mg/L and NO3 (-) of up to 20 ± 1 mg/L for water samples.