Determination of volatile N-nitrosamines in meat products by microwave-assisted extraction coupled with dispersive micro solid-phase extraction and gas chromatography – Chemical ionisation mass spectrometry

Huang, Man Chun; Chen, Hsin‐Chang; Fu, Ssu Chieh; Wang, Ding

doi:10.1016/j.foodchem.2012.09.119

Cited by 71 publications

(31 citation statements)

References 23 publications

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“…The polarities of the target NAs are quite different; some are of high polarity, whereas some are of medium polarity, and in previous studies, dichloromethane, acetonitrile, water and methanol were used as extraction solvents. 1,3,7,11 In the present work, on the basis of the matrix properties of soy sauce, the negative samples (samples that do not contain the target NAs) were selected to perform the recovery experiment, and in the meantime, the extraction effects of dichloromethane (CH 2 Cl 2 ), acetonitrile, ethyl acetate and hexane were compared with each other. Recoveries were calculated by the ratio of spiked sample extraction solution versus the same NA concentration of the matrix calibration solution prepared with the negative matrix extraction solution.…”

Section: Extraction Conditionsmentioning

confidence: 99%

“…The determination of NAs has mainly focused on meat products and some other foods, 1,[9][10][11][12][13][14][15] drinking water, 2,[6][7][8]17,18 cosmetics, 3 and environmental media. 16,19 The traditional detection method is gas chromatography coupled with thermal energy analysis (GC-TEA), 12,15 but TEA is very expensive and its applications are narrow.…”

Section: Introductionmentioning

confidence: 99%

“…2,6,7,14 Dispersive micro-solid phase (D-m-SPE) extraction that used Carboxen™ 1000 as the adsorbing material was used in the sample pretreatment and a preferable purication effect was obtained. 11 To the best of our knowledge, few studies have been reported in the determination of NAs in soy sauce and there are no studies on the application of the QuEChERS-based purication method in NA determination. In the present study, six NAs (chemical structures are presented in Fig.…”

Section: Introductionmentioning

confidence: 99%

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Application of QuEChERS-based purification coupled with isotope dilution gas chromatography-mass spectrometry method for the determination of N-nitrosamines in soy sauce

et al. 2016

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A sensitive and rapid method involving an improved approach called the quick, easy, cheap, effective, rugged, and safe (QuEChERS) purification method and isotope dilution gas chromatography-mass spectrometry (GC-MS) was established to determine six N-nitrosamines (NAs) in soy sauce. Samples were firstly extracted by ethyl acetate. Then the extraction solution was concentrated by slow nitrogen gas blowing and subsequently purified using the QuEChERS-based purification method. Separation of six target NAs was performed on an INNOWAX polar capillary chromatographic column. All of the samples were detected by selected ion monitoring (SIM) mode of GC-MS and N-nitrosodimethylamine-d 6 (NDMA-d 6 ) and N-nitrosodipropylamine-d 14 (NDPA-d 14 ) were used as internal standards. The developed method was validated in terms of the linearity, limit of detection (LOD), matrix effects, specificity, accuracy and precision. Results indicated that this method is of good specificity with almost negligible matrix effects. Linear relations of six NAs were favourable in the range of 2.0-200 mg L À1 and the correlation coefficients were greater than 0.9994. The LODs were lower than 1 mg kg À1 (0.4-0.9 mg kg À1 ) and the limits of quantitation (LOQs) of the method were within the range of 1.2-3.0 mg kg À1 . The mean recoveries for negative light and dark soy sauce samples at three spiked concentration levels were in the range of 80.2-112% with overall relative standard deviation (RSD) values (n ¼ 6) of 2.5-6.8%. The validated method was simple and rapid, with good repeatability, and was successfully applied to determine the concentrations of NAs in soy sauce.

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Section: Extraction Conditionsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Application of QuEChERS-based purification coupled with isotope dilution gas chromatography-mass spectrometry method for the determination of N-nitrosamines in soy sauce

et al. 2016

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“…The primary NAs extraction procedures from meat products (including the official method) employ distillation in alkaline medium and combination of liquid-liquid extraction using relatively low polarity organic solvents (usually dichloromethane), followed by concentration of the extract on Kuderna-Danish (K-D) and a two-step SPE method with Extrelut and Florisil as sorbents (AOAC 1990;Huang et al 2013). These extraction procedures can be extremely long and consume large amounts of organic solvent.…”

Section: Introductionmentioning

confidence: 99%

“…Even though it is a simple method that allows fast analysis, SPME without the use of solvents requires careful optimisation of various parameters, the equilibrium of NAs between the sample and the fibre is not always reached despite the use of lengthy extraction times, and the extraction efficiency appears to be too low for most major NAs (Sen et al 1997;Ventanas et al 2006). Other methods have been alternatively developed for VNAs determination in meat products, including microwave-assisted extraction (Campillo et al 2011;Huang et al 2013;Ramezani et al 2014), supercritical fluid extraction (Sanches Filho et al 2007), and superheated water extraction (Chienthavorn et al 2014). However, these methods require the availability of specific apparatus that is limited to laboratories that can afford it.…”

Section: Introductionmentioning

confidence: 99%

Determination ofN-nitrosamines in processed meats by liquid extraction combined with gas chromatography-methanol chemical ionisation/mass spectrometry

Scheeren

Sabik

Gariépy

et al. 2015

Food Additives & Contaminants: Part A

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A simple, accessible and reproducible method was developed and validated as an alternative for the determination of nine volatile N-nitrosamines (NAs) in meat products, using a low volume of organic solvent and without requiring specific apparatus, offering the possibility of practical implementation in routine laboratories. The NAs were extracted with dichloromethane followed by a clean-up with phosphate buffer solution (pH 7.0). The extracts were analysed by gas chromatography-chemical ionisation/mass spectrometry (GC-CI/MS) in positive-ion mode using methanol as reagent. Limits of detection and quantification, recovery and reproducibility were determined for all NAs (N-nitrosodimethylamine, N-nitrosomethylethylamine, N-nitrosodiethylamine, N-nitrosopyrrolidine, N-nitrosodipropylamine, N-nitrosomorpholine, N-nitrosopiperidine, N-nitrosodibutylamine and N-nitrosodiphenylamine). Satisfactory sensitivity and selectivity were obtained even without concentrating the extract by solvent evaporation, avoiding the loss of the nine NAs studied. Limits of detection ranged from 0.15 to 0.37 µg kg(-1), whereas limits of quantification ranged from 0.50 to 1.24 µg kg(-1). Recoveries calculated in cooked ham that had been spiked at 10 and 100 µg kg(-1) were found to be between 70% and 114% with an average relative standard deviation of 13.2%. The method was successfully used to analyse five samples of processed meat products on the day of purchase and 7 days later (after storage at 4°C). The most abundant NAs found in the analysed products were N-nitrosodipropylamine and N-nitrosopiperidine, which ranged from 1.75 to 34.75 µg kg(-1) and from 1.50 to 4.26 µg kg(-1), respectively. In general, an increase in the level of NAs was observed after the storage period. The proposed method may therefore be a useful tool for food safety control once it allows assessing the profile and the dietary intake of NAs in food over time.

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Dispersive Solid‐Phase Extraction

Socas‐Rodríguez

Herrera‐Herrera

Asensio‐Ramos

et al. 2015

Analytical Separation Science

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Dispersive solid‐phase extraction ( dSPE ) is a sorbent‐based technique widely applied in sample preparation for both sample clean up or analite preconcentration. It shows considerable benefits over conventional SPE , especially in terms of the simplicity of the procedure. This chapter aims at providing a general overview of dSPE , its different extraction approaches ( dSPE , µ‐ dSPE and magnetic‐ dSPE ), and the principal factors which influence the extraction process (including the sorbents most frequently used) as well as its most common applications.

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Determination of volatile N-nitrosamines in meat products by microwave-assisted extraction coupled with dispersive micro solid-phase extraction and gas chromatography – Chemical ionisation mass spectrometry

Cited by 71 publications

References 23 publications

Application of QuEChERS-based purification coupled with isotope dilution gas chromatography-mass spectrometry method for the determination of N-nitrosamines in soy sauce

Application of QuEChERS-based purification coupled with isotope dilution gas chromatography-mass spectrometry method for the determination of N-nitrosamines in soy sauce

Determination ofN-nitrosamines in processed meats by liquid extraction combined with gas chromatography-methanol chemical ionisation/mass spectrometry

Dispersive Solid‐Phase Extraction

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