Evaluation of a method for the simultaneous quantification of N‐nitrosamines in water samples based on stir bar sorptive extraction combined with high‐performance liquid chromatography and diode array detection

Abstract

A simple, sensitive, and reliable procedure based on stir bar sorptive extraction coupled with high-performance liquid chromatography was applied to simultaneously extract and determine three semipolar nitrosamines including N-nitrosodibutylamine, N-nitrosodiphenylamine, and N-nitrosodicyclohexylamine. To achieve the optimum conditions, the effective parameters on the extraction efficiency including desorption solvent and time, ionic strength of sample, extraction time, and sample volume were systematically investigated. The optimized extraction procedure was carried out by stir bars coated with polydimethylsiloxane. Under optimum extraction conditions, the performance of the proposed method was studied. The linear dynamic range was obtained in the range of 0.95-1000 ng/mL (r = 0.9995), 0.26-1000 ng/mL (r = 0.9988) and both 0.32-100 ng/mL (r = 0.9999) and 100-1000 ng/mL (r = 0.9998) with limits of detection of 0.28, 0.08, and 0.09 ng/mL for N-nitrosodibutylamine, N-nitrosodiphenylamine, and N-nitrosodicyclohexylamine, respectively. The average recoveries were obtained >81%, and the reproducibility of the proposed method presented as intra- and interday precision were also found with a relative standard deviation <6%. Finally, the proposed method was successfully applied to the determination of trace amounts of selected nitrosamines in various water and wastewater samples and the obtained results were confirmed using mass spectrometry.

Microextraction by packed sorbent of N‐nitrosamines from Losartan tablets using a high‐throughput robot platform followed by liquid chromatography‐tandem mass spectrometry

“…Although fast and straightforward, that methodology entails the injection of dirty extracts into the chromatographic system and can lead to column clogging, instrument contamination, and carry-over effects. There-fore, an appropriate methodology for routine monitoring of N-nitrosamines should be accompanied by an efficient sample preparation technique [21][22][23].…”

Determination of trace polychlorinated biphenyls and organochlorine pesticides in water samples through large‐volume stir bar sorptive extraction method with thermal desorption gas chromatography

“…In 1999, SBSE was introduced as a solvent-less sample preparation method to extract and enrich organic compounds from aqueous matrices [10]. SBSE is typically applied to extract aqueous samples containing low organic compound concentrations [11][12][13][14][15]. The theoretical adsorption capacity F I G U R E 3 Influence of TD time on chromatographic peak area of SBSE is higher than that of SPME because the extraction coating volume of the former is 50 to 250 times of the largest coating amount (0.5 μL) of the latter.…”

Determination of nine volatile N‐nitrosamines in tobacco and smokeless tobacco products by dispersive solid‐phase extraction with gas chromatography and tandem mass spectrometry

“…However, the SLE method requires an organic solvent of over 100 mL in volume and a considerable amount of adsorbent (20 g), rendering the process nonenvironmentally friendly and undesirable for routine use. Recently, pretreatment methods like SPME and dispersive micro‐SPE have also been assessed . However, the low content levels of VNAs in tobacco matrices, as well as the complexity of tobacco matrices, render these methods unavailable.…”