scholarly journals Determination of Dodine in Fruit Samples by Liquid Chromatography Electrospray Ionization-Tandem Mass Spectrometry

2011 ◽  
Vol 94 (1) ◽  
pp. 300-306 ◽  
Author(s):  
Rozenn Le Grand ◽  
Franck Saint-Marcoux ◽  
Sylvain Dulaurent ◽  
François-Ludovic Sauvage ◽  
Christian Moesch ◽  
...  

Abstract A rapid and sensitive LC/electrospray ionization-MS/MS method has been developed for the determination of dodine in fruit samples. Based on a liquid–liquid extraction of 10 g solid fruit homogenate using an acetone–dichloromethane– hexane mixture and acetate ammonium buffer (pH 4.5), this LC/MS/MS procedure was characterized by recoveries above 50%, with good intra-assay precision (RSD <13%) and interassay precision (RSD <18%) for seven different matrixes (apple, apricot, cherry, peach, pear, plum, and quince). This method was validated from 5 to 500 μg/kg according to standard guidelines. Its LOD (1 μg/kg) and LOQ (5 μg/kg) were in accordance with recommendations of the European legislation defined for infant food [maximum residue level (MRL) = 10 μg/kg]. The whole procedure was finally tested on 1022 fruit samples intended for commercialization, both infant food samples and samples not intended in particular for babies. In this study, dodine was detected in 27 samples; none exhibited a concentration higher than the MRL.

INDIAN DRUGS ◽  
2012 ◽  
Vol 49 (02) ◽  
pp. 37-44
Author(s):  
J Valarmathy ◽  
◽  
T. Sudha ◽  
K. L. Kumar ◽  
S. L Joshua

A sensitive and efficient method was developed for the determination of carvedilol and its metabolite in human plasma by LC-MS/MS. Plasma samples were hydrolysed with beta-glucuronidase and the target compounds were extracted with liquid liquid extraction using diethyl ether in dichloro methane as solvent. The extracts were completely derivatized and analysed by LC-MS/MS. The linearity of the assay ranges from 0.250 ng/mL to 200.0 ng/mL for carvedilol and from 0.500 ng/mL to 30.0 ng/mL for 4-hydroxy carvedilol. The absolute recovery of carvedilol and its metabolite added to blank plasma sample was 70.28 82.90%. The reproducibility was from 0.96 to 8.28 for the intraday assay and from 1.65 to 6.09 for the interday assay precision. Repetitive thawing and freezing did not have an affect on metabolite through a minimum of three cycles. Thawed samples remaining in plasma for 4h before extraction were with 5% of theoretical value. Stability of the extracted samples on the auto sampler at room temperature was evaluated for 34 h and was observed to with in 12% of a fresh analytical sample for 4 hydroxy carvedilol. The proposed LC-MS/MS method was effective for the determination of carvedilol and it metabolite in human plasma.


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