Ammonium chloride salting out extraction/cleanup for trace-level quantitative analysis in food and biological matrices by flow injection tandem mass spectrometry

Nanita, Sergio C.; Padivitage, Nilusha

doi:10.1016/j.aca.2013.01.011

Cited by 53 publications

(17 citation statements)

References 34 publications

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“…Many of them are based on solid-phase extraction (SPE) (Carabias-Martinez et al 2004;Seccia et al 2011), dispersive solid-phase extraction (DSPE) combined with dispersive liquid-liquid microextraction (DLLME) (Wu et al 2009), molecularly imprinted SPE (She et al 2010), or matrix soil-phase dispersion (MSPD) (Liang et al 2014;Łozowicka et al 2009). Most published methods involve liquid-soil extraction (LLE) Noche et al 2011) or salting-out liquid-liquid extraction (SALLE) (Nanita and Padivitage 2013).…”

Section: Introductionmentioning

confidence: 99%

One-Step QuEChERS-Based Approach to Extraction and Cleanup in Multiresidue Analysis of Sulfonylurea Herbicides in Cereals by Liquid Chromatography–Tandem Mass Spectrometry

Kaczyński

Łozowicka

2016

Food Anal. Methods

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A one-step quick, easy, cheap, effective, rugged, and safe (QuEChERS)-based approach to extraction and cleanup in multiresidue pesticide analysis is presented for the first time. The experiment was designed to detect 23 sulfonylurea herbicides in a complex cereal matrix. The challenge was to choose the optimal conditions of one-step extraction and cleanup. Chitin, diatomaceous earth, and octadecyl were investigated as cleanup sorbents. Chitin, citrate buffer, and 1 % formic acid in acetonitrile yielded the best results. The effectiveness of sulfonylureas extraction was evaluated at three different spiking levels (0.005, 0.05, and 0.5 mg kg −1 ) in wheat, rye, and oat using liquid chromatography-tandem mass spectrometry. The one-step QuEChERS provided recoveries in the 70-120 % range for 23 sulfonylureas in all cereal matrices. Matrix effects were evaluated and were not significant for all herbicides, showing suppression or enhancement (between −19 and 13 %). Precision, calculated as relative standard deviation (RSD), was below 20 %. A linear dependence was observed in the range of 0.005-2.0 mg kg −1 , and the correlation coefficient was R 2 > 0.999. Expanded measurement uncertainty was estimated to be between 9 and 24 %, on average. The validated method was employed in analysis of 89 real grain samples.

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Section: Introductionmentioning

confidence: 99%

One-Step QuEChERS-Based Approach to Extraction and Cleanup in Multiresidue Analysis of Sulfonylurea Herbicides in Cereals by Liquid Chromatography–Tandem Mass Spectrometry

Kaczyński

Łozowicka

2016

Food Anal. Methods

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“…Because EI‐LC‐MS with SMB has no matrix related ion suppression effects, it does not always require LC for sample separation from the matrix, and thus a new approach is enabled for achieving ultra‐fast flow injection (FI) EI‐MS‐MS with SMB analysis. Recently, the topic of flow injection MS‐MS as an alternative to lengthy LC‐MS analysis received significant attention in the world of pesticides analysis in agricultural products …”

Section: Results—cold Ei Mass Spectra Features and Selected Applicatmentioning

confidence: 99%

“…Recently, the topic of flow injection MS-MS as an alternative to lengthy LC-MS analysis received significant attention in the world of pesticides analysis in agricultural products. [49][50][51][52][53] In these and in other experiments with electrospray ionization, [49][50][51][52][53][54] the sample extracts were diluted about 100-200 times to reduce or eliminate ion suppression effects and analyzed by flow injection, electrospray ionization MS-MS. However, as known, electrospray cannot serve for the ionization of all pesticides, especially with 100 times dilution, and its sensitivity is not sufficient for a few groups of pesticides, particularly those that currently require GC-MS analysis such as the organo-chlorine pesticides.…”

Section: Results-cold Ei Mass Spectra Features and Selected Applicatmentioning

confidence: 99%

Electron ionization LC‐MS with supersonic molecular beams—the new concept, benefits and applications

et al. 2015

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A new type of electron ionization LC-MS with supersonic molecular beams (EI-LC-MS with SMB) is described. This system and its operational methods are based on pneumatic spray formation of the LC liquid flow in a heated spray vaporization chamber, full sample thermal vaporization and subsequent electron ionization of vibrationally cold molecules in supersonic molecular beams. The vaporized sample compounds are transferred into a supersonic nozzle via a flow restrictor capillary. Consequently, while the pneumatic spray is formed and vaporized at above atmospheric pressure the supersonic nozzle backing pressure is about 0.15 Bar for the formation of supersonic molecular beams with vibrationally cold sample molecules without cluster formation with the solvent vapor. The sample compounds are ionized in a fly-though EI ion source as vibrationally cold molecules in the SMB, resulting in 'Cold EI' (EI of vibrationally cold molecules) mass spectra that exhibit the standard EI fragments combined with enhanced molecular ions. We evaluated the EI-LC-MS with SMB system and demonstrated its effectiveness in NIST library sample identification which is complemented with the availability of enhanced molecular ions. The EI-LC-MS with SMB system is characterized by linear response of five orders of magnitude and uniform compound independent response including for non-polar compounds. This feature improves sample quantitation that can be approximated without compound specific calibration. Cold EI, like EI, is free from ion suppression and/or enhancement effects (that plague ESI and/or APCI) which facilitate faster LC separation because full separation is not essential. The absence of ion suppression effects enables the exploration of fast flow injection MS-MS as an alternative to lengthy LC-MS analysis. These features are demonstrated in a few examples, and the analysis of the main ingredients of Cannabis on a few Cannabis flower extracts is demonstrated. Finally, the advantages of EI-LC-MS with SMB are listed and discussed.

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“…As a result, only non-polar contaminants, e.g., trace pesticide residues, may be extracted and concentrated in the non-polar organic solvents chosen. How-ever, LLE procedure can be modified for further extending its applications for enabling efficient extraction of polar pesticide residues from various water samples [22] [23]. This can be achieved by addition of appropriate quantities of a salt to the mixture of the aqueous sample and water-miscible organic solvent, for causing formation of a two-phase system and simultaneous separation of the target analytes into the organic phase [24] [25].…”

Section: Introductionmentioning

confidence: 99%

Salting-Out Assisted Liquid-Liquid Extraction Combined with HPLC for Quantitative Extraction of Trace Multiclass Pesticide Residues from Environmental Waters

Alemayehu¹,

Tolcha²,

Megersa³

2017

AJAC

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In this study, salting-out assisted liquid-liquid extraction combined with high performance liquid chromatography diode array detector (SALLE-HPLC-DAD) method was developed and validated for simultaneous analysis of carbaryl, atrazine, propazine, chlorothalonil, dimethametryn and terbutryn in environmental water samples. Parameters affecting the extraction efficiency such as type and volume of extraction solvent, sample volume, salt type and amount, centrifugation speed and time, and sample pH were optimized. Under the optimum extraction conditions the method was linear over the range of 10 -100 μg/L (carbaryl), 8 -100 μg/L (atarzine), 7 -100 μg/L (propazine) and 9 -100 μg/L (chlorothalonil, terbutryn and dimethametryn) with correlation coefficients (R 2 ) between 0.99 and 0.999. Limits of detection and quantification ranged from 2.0 to 2.8 μg/L and 6.7 to 9.5 μg/L, respectively. The extraction recoveries obtained for ground, lake and river waters were in a range of 75.5% to 106.6%, with the intra-day and inter-day relative standard deviation lower than 3.4% for all the target analytes. All of the target analytes were not detected in these samples. Therefore, the proposed SALLE-HPLC-DAD method is simple, rapid, cheap and environmentally friendly for the determination of the aforementioned herbicides, insecticide and fungicide residues in environmental water samples.

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Ammonium chloride salting out extraction/cleanup for trace-level quantitative analysis in food and biological matrices by flow injection tandem mass spectrometry

Cited by 53 publications

References 34 publications

One-Step QuEChERS-Based Approach to Extraction and Cleanup in Multiresidue Analysis of Sulfonylurea Herbicides in Cereals by Liquid Chromatography–Tandem Mass Spectrometry

One-Step QuEChERS-Based Approach to Extraction and Cleanup in Multiresidue Analysis of Sulfonylurea Herbicides in Cereals by Liquid Chromatography–Tandem Mass Spectrometry

Electron ionization LC‐MS with supersonic molecular beams—the new concept, benefits and applications

Salting-Out Assisted Liquid-Liquid Extraction Combined with HPLC for Quantitative Extraction of Trace Multiclass Pesticide Residues from Environmental Waters

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