scholarly journals Effect of flow rate and freezing on cyanocobalamin recovery using a commercial solid phase extraction cartridge

2020 ◽  
pp. 014-018
Author(s):  
Lees Lauren ◽  
Bland Alison M ◽  
DiTullio Giacomo R ◽  
Janech Michael G ◽  
Lee Peter A
2019 ◽  
Author(s):  
Lauren Lees ◽  
Alison M. Bland ◽  
Giacomo R. DiTullio ◽  
Michael G. Janech ◽  
Peter A. Lee

AbstractAnalysis of vitamin B12 in sea water is laborious, time consuming, and often requires storage of relatively large-volume water samples. Alleviating these major limitations will increase the throughput of samples and, as a consequence, improve our understanding of the distribution and role of vitamin B12 in the oceans. Previous studies have indicated that target analyte recovery is negatively affected at flow rates exceeding 1 mL min−1 using home-made C18 Solid Phase Extraction (SPE) cartridges. In this study, the effect of flow rate on recovery of vitamin B12 was tested across a range of flow rates between 1 and 37 mL min−1 using a commercial SPE cartridge containing surface-modified styrene divinylbenzene. Recovery of vitamin B12 at flow rates up to the maximum rate tested did not statistically differ from 1 mL min 1. A second study was conducted to determine whether storage of the SPE cartridges at −20°C had a negative impact on vitamin B12 recovery. Recovery of vitamin B12 from SPE cartridges stored up to 13 days did not differ from unfrozen SPE cartridges. These data suggest that rapid extraction and cold storage of vitamin B12 on commercial SPE cartridges does not negatively affect recovery and offers an economical alternative to field studies.


1995 ◽  
Vol 78 (4) ◽  
pp. 971-977 ◽  
Author(s):  
Sherri B Turnipseed ◽  
José E Roybal ◽  
Jeffrey A Hurlbut ◽  
Austin R Long

Abstract A gas chromatographic/mass spectrometric (GC/MS) method was developed to confirm the presence of leucomalachite green (LMG), a metabolite of the triphenylmethane dye malachite green (MG), in catfish tissue. Residues were isolated according to a previously described liquid chromatographic (LC)A/IS spectrometric analysis of MG and LMG in fish. In our isolation procedure, analytes are extracted from tissue with acetonitrile–buffer, partitioned into CH2CI2, and applied to neutral alumina and propylsulfonic acid solid-phase extraction cartridges. Before GC/MS analysis, extracts prepared for the LC determinative method are eluted from a cyano solid-phase extraction cartridge, extracted into organic solvent, and concentrated for GC/MS analysis. Selected ion monitoring was performed by using 5 diagnostic ions (m/z 330,329,253,210, and 165) of LMG. The method was validated by confirming LMG in tissue fortified with mixtures of MG and LMG (5 and 10 ng/g each) and in tissue from fish that had been exposed to low levels of MG.


2019 ◽  
Vol 62 (4) ◽  
pp. 190-197 ◽  
Author(s):  
Mitja Kovac ◽  
Tunde Miklovicz ◽  
Lei Li ◽  
Joseph Russell ◽  
Roberto Canales Candela ◽  
...  

2011 ◽  
Vol 2011 ◽  
pp. 1-6 ◽  
Author(s):  
Vanessa N. Alves ◽  
Simone S. O. Borges ◽  
Waldomiro B. Neto ◽  
Nívia M. M. Coelho

In this study, a method for the determination of low concentrations of lead in beer samples using solid-phase extraction with a flow injection analysis system and detection by flame atomic absorption spectrometry (FAAS) was developed.Moringa oleiferaseeds were used as a biosorbent material. Chemical and flow variables of the online preconcentration system, such as sample pH, preconcentration flow rate, eluent flow rate, eluent concentration, particle size, and sorbent mass, were studied. The optimum extraction conditions were obtained using a sample pH of 6.0, sample flow rate of 6.0 mL min−1, 63.0 mg of sorbent mass, and 2.0 mol L−1HNO3at a flow rate of 2.0 mL min−1as the eluent. With the optimized conditions, the preconcentration factor, precision, detection limit, consumption index, and sample throughput were estimated as 93, 0.3% (10.0 μg L−1,n=7), 7.5 μg L−1, 0.11 mL, and 23 samples per hour, respectively. The method developed was successfully applied to beer samples and recovery tests, with recovery ranging from 80% to 100%.


2018 ◽  
Vol 81 (11) ◽  
pp. 1487-1494 ◽  
Author(s):  
A. Azaryan ◽  
T. Ligor ◽  
B. Buszewski ◽  
A. Temerdashev ◽  
E. Dmitrieva ◽  
...  

2021 ◽  
Vol 6 (1) ◽  
pp. 14-19
Author(s):  
Yuniar Yuniar ◽  
◽  
Siti Nuraini

The Pre-concentration of Cd(II) in water samples was carried out by using column solid phase extraction DOWEX 50WX2 prior to flame atomic absorption spectrometry analyzed. The analytical parameters consist of pH, flow rate, volume of eluent and volume of sample were determined.The optimum conditions were obtained pH was 5, sample flow rate was 1 mL min−1, volume of eluent nitric acid 1N was 10 mL and sample volume was 50 mL. The optimum conditions obtained were used to determine the detection limit and the accuracy of the method using tap water samples. Determination of detection limit used tap water which contain Cd 0.001 mg L-1 and the accuracy (recovery,%R) with concentration of Cd 0.01 mg L-1. The detection limit was found 0.2697±0.0899 µg L− 1 (n=7) and accuracy (n=7) was 93±6%. The result showed the accuracy still meets the acceptance criteria for accuracy (70%-125%) and the RSD 6% is smaller than the Horwitz value of 20.8%. Based on the accuracy (R%) and % RSD values obtained, it can be concluded that this method provides effective results for pre-concentration to increase the detection limit of Cd (II)in clean water using SSA-flame.


2004 ◽  
Vol 87 (2) ◽  
pp. 341-345 ◽  
Author(s):  
Matthew J Gramse ◽  
Paul E Jacobson ◽  
James C Selkirk

Abstract A method was developed for the determination of tylosin in feeds. The method involves extraction of tylosin with methanol, concentration under a stream of nitrogen, and cleanup using Phenomenex C18 solid-phase extraction cartridge. Analyte separation and quantitation were achieved by gradient reversed-phase liquid chromatography and UV absorbance at 285 nm with a reference wavelength of 320 nm with column temperature of 45°C. Average spike recoveries for samples prepared at 4 spiking levels (22.7, 181, 907, and 1000 g/ton) were 111.0, 94.9, 96.2, and 98.6%, respectively. The overall method precision at each of the 4 spiking levels was ≤ 7.85% relative standard deviation. The limits of detection and quantitation (g/ton) were 2.16 and 7.20 g/ton, respectively.


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