Methodology For Determination Of Parabens,Sulfonamides, And Triphenylmethane Dyes In Aquatic Products

Drug residues in food caused much attetion since this problem exert much threaten to human health. Meanwhile, the current methods for determination of parabens, sulfonamide, and triphenylmethane dyes, were tedious and less accuracy. High through put methods are urgently need.The chromatographic performance of superficially porous particles was compared to that of sub-2μm fully porous particles. Halo fused-core C18column (50mm×2.1mm,2.7μm) and Acquity BEH C18(50mm×2.1mm,2.7μm), were used for analysis of four kinds of parabens in seafood sauce van Deemter, Knox and Poppe plots were constructed for both columns to compare their kinetic performance under the same operating conditions. Other chromatographic parameters such as retention time and pressure drop were also studied. The fused-core column, made by fusing a0.5μm porous silica layer onto1.7μm nonporous silica cores, was found to provide better analyte shape selectivity and similar efficiency to sub-2μm particles, without any high pressure. Based on these factors, a novel, simple and ultra-fast high-performance liquid chromatographic method has been established and validated for the determination of methylparaben, ethylparaben, propylparaben and butylparaben, using Halo fused-core C18column for separation. The method was sensitive with a limit of detection (LOD) of20ng/mL, with good linearity (R2ranging from0.9996to0.9999) over the linear range of50～1000ng/mL. The intra-day and inter-day precision was less than7.08%and accuracy ranged from100.3%to103.5%for quality control samples at three concentrations of100,200and500ng/mL. The successful practical application of the proposed method to real samples indicated that the developed method is sensitive and useful for detection, quantification and confirmation of these parabens in seafood sauce and can be used for residue control programs.A novel analytical protocol based on interfacing on-line matrix solid-phase dispersion (MSPD) with high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) was developed for extraction and determination of13sulfonamide residues in grass carp tissues. The target analytes were separated on a fused-core C18-silica column with a period of7min and quantified by a triple-quadrupole linear ion-trap mass spectrometer in positive ion multiple-reaction monitoring (MRM) mode. The proposed method was optimized and validated according to Commission Decision2002/657/EC. The matrix-matched calibration curves were performed at six concentration levels and good linear relationship (R2=0.993-0.998) was observed within the range of0.1-100ng/mL. The mean values of relative standard deviation of intra-and inter-day ranging from1.8%to7.8%and from2.8%to10.3%were obtained, respectively. Moreover, satisfied recoveries (69.0-96.3%) of all studied sulfonamides were demonstrated in different spiked levels, with RSDs≤13.2%. The proposed method has been applied successfully to the analysis of sulfonamides in several grass carp samples, and the results indicated that this novel instrumental coupling was fast, sensitive, reliable and environmental friendly with good prospects.In this study an on-line column-switching fast LC-MS/MS method was described for the identification and the quantitative determination of the triphenylmethane dyes, malachite green (MG), crystal violet (CV), brilliant green (BG) and leuco malachite green (LMG) and leuco crystal violet (LCV). The analytes were isolated from the matrix by solid-phase extraction with acetonitrile online. Determination was performed using LC-MS/MS with positive electrospray ionisation.4different deuterated internal standards were introduced to improve the quantitative performance of the method. The method has been validated in line with the EU criteria of Commission Decision2002/657/EC in accordance with the minimum required performance limit (MRPL) setting at2μg/kg for the sum of MG and LMG. For all the monitored compounds, accuracy, intra-day and inter-day precision were determined at each level of fortification (0.5,0.75,1.0and2.0μg/kg). Decision limits CCa and detection capabilities CCβwere calculated according to the standard ISO11843-2. A study on the applicability of the method was conducted on various aquacultured species with the aim to assess the matrix effects. The presence of residues of leuco brilliant green in fish has also been confirmed from experimental study performed on trout treated with brilliant green, using LTQ-Orbitrap mass spectrometer.