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Yan H.,Food Laboratory of Beijing Inspection and Quarantine Testing Center | Liu X.,Food Laboratory of Beijing Inspection and Quarantine Testing Center | Cui F.,Food Laboratory of Beijing Inspection and Quarantine Testing Center | Yun H.,Food Laboratory of Beijing Inspection and Quarantine Testing Center | And 4 more authors.
Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences | Year: 2013

A novel sample pretreatment method was developed for the quantitative determination of amantadine and rimantadine in chicken muscle tissues by ultra high performance liquid chromatography coupled with high resolution LTQ Orbitrap mass spectrometry (UHPLC-LTQ Orbitrap MS). The samples were pretreated by modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method, using acetonitrile (1% acetic acid, v/v) as extraction solution and C18 sorbent for clean-up. The separation was carried out on a Waters ACQUITY UPLC HSS T3 column (150mm×2.1mm, 1.8μm particle), using a mobile phase of acetonitrile and 0.1% aqueous formic acid solution. LTQ Orbitrap MS with resolving power of 60000 was applied for analysis of the samples. Amantadine and rimantadine were identified from their accurate mass (within 5ppm) and retention times from the acquired full-scan chromatogram and quantified by their peak areas. The linear range for the determination of the analytes was 1-100μg/kg. Limits of detection (LODs) for amantadine and rimantadine were 1.02μg/kg and 0.67μg/kg, respectively. The intra- and inter-day accuracy ranged from 87.5% to 102.4%, and 82.5% to 105.8% for amantadine, and 95.3% to 97.4%, and 89.4% to 93.2% for rimantadine, respectively. The precision of intra- and inter-day was between 3.9-6.3% and 5.95-13.9% for amantadine, 6.0-7.45% and 7.8-12.4% for rimantadine, respectively. Finally, the method was applied for the determination of these antiviral agents in routine samples, and amantadine residue was detected in some cases. © 2013 Elsevier B.V.


Zhang H.-Y.,Wenzhou Medical College | Zhang H.-Y.,Food Laboratory of Beijing Inspection and Quarantine Testing Center | Liu X.,Food Laboratory of Beijing Inspection and Quarantine Testing Center | Yan H.,Food Laboratory of Beijing Inspection and Quarantine Testing Center | And 6 more authors.
Journal of Chinese Mass Spectrometry Society | Year: 2013

MS/MS isotope ratio and accuracy mass measure were used to further confirm the elemental composition and structural information of molecular formula by performing on an LTQ/Orbitrap. The light and heavy isotopes of target parent ion were detected when setting the ion trap's isolation width at 6 u. The MS/MS isotope ratio and accuracy mass measure were used to elucidate the fragments pathway. Sulfamerazine was used as an example, most of the fragmentations were analyzed by isotopic abundance ratio and peak shape information, the result is as same as literature reported. However, the fragment ion at m/z 65 is different from previous report. According to its accuracy mass measure and isotope abundance ratio, there is no S atom in this ion. The result shows that the proposed isotope distribute fragmentation method is a powerful trick to provide large amounts of the necessary elemental composition to the fragment news of compounds.

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