Multiplug filtration cleanup method with multi-walled carbon nanotubes for the analysis of malachite green, diethylstilbestrol residues, and their metabolites in aquatic products by liquid chromatography–tandem mass spectrometry

Abstract

The food safety supervision in aquatic products has raised public concern in recent years. In this study, a liquid chromatographic-tandem mass spectrometric (LC-MS/MS) method for the simultaneous quantification and identification of four residues of the ever widely used analytes (including malachite green, leucomalachite green, diethylstilbestrol, and dienestrol) in aquaculture samples was developed. For sample preparation, a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method was used, which was initially developed for pesticide residue analysis. For cleanup procedure, low-temperature cleanup method was combined with multiplug filtration cleanup (m-PFC) method based on multi-walled carbon nanotubes (MWCNTs). The volume of water, extraction solvent, cleanup sorbents, and m-PFC procedure were optimized for carp, striped bass, and giant salamander matrices. It was validated by analyzing four residues in each matrix spiked at three concentration levels of 0.5, 5, and 50 μg/kg (n = 5). The method was successfully validated according to the 2002/657/EC guidelines. After optimization, spike recoveries were within 73-106 % and <15 % relative standard deviations (RSDs) for all analytes in the tested matrices. Limits of quantification (LOQs) for the proposed method ranged from 0.10 to 0.50 μg/kg. Matrix-matched calibrations were performed with the coefficients of determination >0.998 between concentration levels of 0.5 and 200 μg/kg. The developed method was successfully applied to the determination of residues in market samples. Graphical abstract Flow chart of multi-plug filtration cleanup combined with low-temperature cleanup method.

Advanced materials on sample preparation for safety analysis of aquatic products

“…Liu et al [57] fabricated CNTsmagnetic NPs by a simple one-step synthesis method for MSPE and the determination of polyether antibiotic and s-triazine drug residues in animal food. Besides, CNTs are often combined with MIPs by covalent or noncovalent binding model in SPE to improve adsorptivity and selectivity [58][59][60], which is mainly attributed to the increased π-π stacking, hydrogen-bonding, dipole-dipole and ion dipole, and hydrophobic interactions [27]. Active carbon, an important absorbent material, has attracted considerable interest in separation science due to their low cost, large surface area (1200 m 2 /g [61]), and high fat capacity.…”

Development and evaluation of an automated multi-channel multiplug filtration cleanup device for pesticide residue analysis on mulberry leaves and processed tea

“…In our previous studies, we focused on optimizing the times of pull and push of m-PFC column. [23][24][25] In this study, an automated multi-channel multiplug ltration cleanup device was developed, which could improve the efficiency and precision and avoid the error causing by manual operation. In order to evaluate the automated device, the recoveries of 82 pesticides in mulberry leaf and mulberry processed tea were investigated under different parameters.…”

Determination of Diethylstilbestrol in Water Samples by Dispersive Liquid-Liquid Microextraction Based on Solidification of Floating Organic Droplet Followed UV Spectrometry

“…However, DES can be bio-accumulated in the food chain and remain in organisms for a long time, having a serious impact on the organism even at very low concentrations [1]. A number of reports have highlighted its potentially dangerous consequences to human and wild life, such as breast and prostate cancer [2,3]. In addition, it has been recognized that DES are widely present in the environmental waters, sediments and some aquatic matrices, through industrial, agricultural and municipal effluents [4].…”

“…Therefore, it is imperative to urgently develop simple, fast, and effective methods for monitoring and determining DES. In recent years, several extraction-determination methods have been developed for DES including solid phase extraction-high performance liquid chromatography [1], solid phase extraction-electrochemiluminescence [2], QuE ChERS-liquid chromatography-tandem mass spectrometry [3], dispersive liquid-liquid microextraction (DLLME)-capillary electrophoresis [4], gold nanoparticles immunoassay [5] and QuEChERS-ultraliquid chromatography-tandem mass spectrometry [6]. In these extraction methods, DLLME method is a novel miniaturized sample pre-treatment technique which requires smaller amounts of organic solvents and reduces the analysis cost more compared with other methods, such as LLE and SPE which have involved drawbacks (e.g.…”