Liquid-Solid Extraction and Fast Atom Bombardment High-Resolution Mass Spectrometry for the Determination of Hydroxyatrazine in Water at Low-ppt Levels

1994 ◽  
Vol 66 (23) ◽  
pp. 4202-4209 ◽  
Author(s):  
Zongwei. Cai ◽  
V. M. Sadagopa. Ramanujam ◽  
M. L. Gross ◽  
S. J. Monson ◽  
D. A. Cassada ◽  
...  
1996 ◽  
Vol 79 (4) ◽  
pp. 929-935 ◽  
Author(s):  
Zongwei Cai ◽  
Steven J Monson ◽  
Roy F Spalding

Abstract Agricultural surface water samples were collected after the first 2 major runoff events in 1994 for determination of atrazine (ATR, 2-chloro-4-ethylamino-6-isopropylamino-s-triazine) and hydroxyatrazine (HA, 2-ethylamino-4-hydroxy-6-isopropylamino-striazine). After addition of. 13C3-labeled ATR and 13C3-labeled HA as internal standards, the chemicals were quantitatively extracted and eluted from water samples by liquid-solid extraction with a carbon black cartridge. Liquid chromatography and fast atom bombardment-high resolution mass spectrometry were used to analyze the sample extracts. Concentrations of ATR ranged from 8.2 to 15.1 parts per billion (ppb) in the samples collected after both runoff events from a highly agricultural watershed in south-central Nebraska. HA concentrations ranged from 0.25 to 2.7 ppb in the water samples. Results obtained from both analytical procedures agreed within a 15% deviation. As predicted from runoff events, the highest levels occurred in samples from the first collection on June 24,1994, for both ATR and HA, whereas samples collected on July 5,1994, contained much lower levels of HA.


2020 ◽  
Vol 86 (8) ◽  
pp. 23-31
Author(s):  
V. G. Amelin ◽  
D. S. Bolshakov

The goal of the study is developing a methodology for determination of the residual amounts of quaternary ammonium compounds (QAC) in food products by UHPLC/high-resolution mass spectrometry after water-acetonitrile extraction of the determined components from the analyzed samples. The identification and determination of QAC was carried out on an «UltiMate 3000» ultra-high-performance liquid chromatograph (Thermo Scientific, USA) equipped with a «maXis 4G» high-resolution quadrupole-time-of-flight mass spectrometric detector and an ion spray «ionBooster» source (Bruker Daltonics, Germany). Samples of milk, cheese (upper cortical layer), dumplings, pork, chicken skin and ground beef were used as working samples. Optimal conditions are specified for chromatographic separation of the mixture of five QAC, two of them being a mixture of homologues with a linear structure (including isomeric forms). The identification of QAC is carried out by the retention time, exact mass of the ions, and coincidence of the mSigma isotopic distribution. The limits for QAC detection are 0.1 – 0.5 ng/ml, the determination limits are 1 ng/ml for aqueous standard solutions. The determinable content of QAC in food products ranges within 1 – 100 ng/g. The results of analysis revealed the residual amount of QAC present in all samples, which confirms data of numerous sources of information about active use of QAC-based disinfectants in the meat and dairy industry. The correctness of the obtained results is verified by introduction of the additives in food products at a level of 10 ng/g for each QAC. The relative standard deviation of the analysis results does not exceed 0.18. The duration of the analysis is 30 – 40 min.


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