LC–MS/MS Determination of Catecholamines in Urine Using FMOC-Cl Derivatization on Solid-Phase Extraction Cartridge

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


2005 ◽  
Vol 88 (3) ◽  
pp. 679-683 ◽  
Author(s):  
Matthew J Gramse ◽  
Paul E Jacobson

Abstract A liquid chromatographic method was developed for the determination of penicillin G in feeds. The method involves extraction of penicillin G with methanol, concentration under a stream of nitrogen, and cleanup using Phenomenex Strata-X solid-phase extraction cartridge. Analyte separation and quantification were achieved by gradient reversed-phase liquid chromatography and ultraviolet absorbance at 230 nm. Average spike recoveries for samples prepared at 3 spiking levels (25, 50, and 200 g/ton) were 96.3, 92.1, and 88.6%, respectively. The overall method precision at each of the 3 spiking levels was ≤5.39% relative standard deviation. The limits of detection and quantititation (g/ton formulation) were 3.89 and 13.0 g/ton, respectively.


2020 ◽  
Vol 165 ◽  
pp. 03044
Author(s):  
Liangliang Tian ◽  
Yongfu Shi ◽  
Dongmei Huang ◽  
Huijuan Yu ◽  
Shuai Wang ◽  
...  

In this study, a special method was developed for the determination of 7 kinds of polychlorinated biphenyls (PCBs) residues in dried kelp by gas chromatography (GC) with electron capture detector (ECD). The PCBs were extracted with hexane/dichloromethane (1/1, v/v) by ultrasonic extraction. Clean-up methods were used by concentrated sulphuric acid, neutral alumina oxide solid phase extraction cartridge and silica solid phase extraction cartridge. The analytical compounds were quantified by an internal standard method. Under optimal experimental conditions, good linearity was observed in the range of 5~200ng/mL, and the correlation coefficients were 0.9993~0.9998. The limit of quantification (LOQ) for target analytical compounds ranged from 6.0 to 7.5μg/kg. At the spiked levels of 10,20,50 μg/kg,the average recoveries ranged from 81.8% to 105% with the relative standard deviations 3.05%~11.2%. The result showed that the proposed method was accurate and could be used for the determination of the PCBs in dried kelp.


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