Multiplug Filtration Cleanup Research Articles

The effects of oxygenation aeration treatment on dissipation behaviors of tricaine mesylate in carp (Cyprinus carpio) muscle and water

Tricaine mesylate (MS-222) is one of the most used anesthetics in fish. It can be absorbed by the human body via food consumption, with related detriments to human health. In this study, a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method was developed for the determination of MS-222 in carp muscle and water samples using liquid chromatography-tandem mass spectrometry (LC-MS/MS). For cleanup procedure, multiplug filtration cleanup (m-PFC) method with n-Hexane delipidation was adopted. The extraction solvent, cleanup methods and sorbents were optimized. All method validation parameters were in the acceptable range. The dissipation behavior study was followed by the method development. Firstly, the anesthesia dose and time were optimized in application study. Secondly, carps were revived for different period of time with (experimental group) and without (control group) the oxygenation aeration treatment to compare the dissipation rate of MS-222. After being anesthetized for 6 h at 50 mg/L and 12 h of elimination, the concentrations of MS-222 in crap muscle and water of experimental group was lower than those of control group. After 36 h of elimination under oxygenation aeration, over 90% of MS-222 was dissipated in carp muscle. The results showed that the half-life of MS-222 in carp muscle was 6.2 h. The findings suggested that the commonly-used oxygenation aeration treatment in aquaculture production had potential effects in accelerating the dissipation of MS-222 in carp and water. In this study, three days of withdrawal period was recommended in carps after MS-222 administration under oxygenation aeration.

Rapid multiplug filtration cleanup method for the determination of 124 pesticide residues in rice, wheat, and corn.

A simple and rapid multiplug filtration cleanup method based on multiwalled carbon nanotubes was developed to determine 124 pesticide residues in rice, wheat, and corn, which could be done in a few seconds without conditioning and elution steps. Various combinations of sorbents were optimized for each matrix with a dispersive solid-phase extraction procedure to get a satisfactory recovery and clean-up performance. Good linearity was obtained for all pesticides with calibration curve coefficients larger than 0.9958. Most recoveries for the majority pesticides were between 70 and 120% (n = 5) with relative standard deviations below 20%. The limit of detection was 0.1-1.3 μg/kg, and the limit of quantification was 0.2-4.3 μg/kg for the pesticides in all matrices. The work suggests that the multiplug filtration cleanup method is better than the dispersive solid-phase extraction method and it could be applied to routinely monitor pesticide residues in market samples.

Use of Carbon Nanotubes for the Analysis of Pesticide Residues in Fruits and Vegetables.

This review presents the application of carbon nanotubes as sorbent materials in the analysis of pesticide residues in fruits and vegetables. The advantages, limitations, and challenges of carbon nanotubes, with respect to their use in analytical chemistry, are presented. The efficiency of their application as extraction sorbent materials (in terms of LOD, LOQ, linearity, relative recovery, and RSD) in SPE, solid-phase microextraction, multi-plug filtration clean-up, matrix solid-phase dispersion, and the quick, easy, cheap, effective, rugged and safe method is reported. The synthesis, functionalization, purification, and characterization methods of carbon nanotubes are also discussed.

Automated multi-plug filtration cleanup for liquid chromatographic–tandem mass spectrometric pesticide multi-residue analysis in representative crop commodities

An automated multi-plug filtration cleanup (m-PFC) method on modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) extracts was developed. The automatic device was aimed to reduce labor-consuming manual operation workload in the cleanup steps. It could control the volume and the speed of pulling and pushing cycles accurately. In this work, m-PFC was based on multi-walled carbon nanotubes (MWCNTs) mixed with other sorbents and anhydrous magnesium sulfate (MgSO4) in a packed tip for analysis of pesticide multi-residues in crop commodities followed by liquid chromatography with tandem mass spectrometric (LC–MS/MS) detection. It was validated by analyzing 25 pesticides in six representative matrices spiked at two concentration levels of 10 and 100μg/kg. Salts, sorbents, m-PFC procedure, automated pulling and pushing volume, automated pulling speed, and pushing speed for each matrix were optimized. After optimization, two general automated m-PFC methods were introduced to relatively simple (apple, citrus fruit, peanut) and relatively complex (spinach, leek, green tea) matrices. Spike recoveries were within 83 and 108% and 1–14% RSD for most analytes in the tested matrices. Matrix-matched calibrations were performed with the coefficients of determination >0.997 between concentration levels of 10 and 1000μg/kg. The developed method was successfully applied to the determination of pesticide residues in market samples.

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

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 50μg/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 0.50μg/kg. Matrix-matched calibrations were performed with the coefficients of determination >0.998 between concentration levels of 0.5 and 200μg/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.

Analytical method for 44 pesticide residues in spinach using multi-plug-filtration cleanup based on multiwalled carbon nanotubes with liquid chromatography and tandem mass spectrometry detection.

Spinach is one of the most commonly planted vegetables worldwide. A high chlorophyll content makes spinach a complicated matrix in pesticide residue analysis. In this study, a rapid clean-up method was developed for the analysis of pesticide multi-residues in spinach followed by liquid chromatography with tandem mass spectrometry. A modified QuEChERS method with multiwalled carbon nanotubes and carbon material was adopted in the multi-Plug Filtration Cleanup procedure. This method was validated for 44 representative pesticides spiked at two concentration levels of 10 and 100 μg/kg. The pesticides of different physicochemical properties were registered on spinach in China. The recoveries were between 76 and 114% for major pesticides with relative standard deviations of less than 15%, except for quizalofop-P-ethyl, pyrimethanil, and carbendazim. Matrix-matched calibration curves were performed with the coefficients of determination higher than 0.995 for the studied pesticides for concentration levels of 10-500 μg/kg. The limits of quantitation ranged from 2 to 10 μg/kg. The developed method was successfully applied to determine pesticide residues in Chinese market spinach samples.

Determination of Sulfoxaflor in Animal Origin Foods Using Dispersive Solid-Phase Extraction and Multiplug Filtration Cleanup Method Based on Multiwalled Carbon Nanotubes by Ultraperformance Liquid Chromatography/Tandem Mass Spectrometry.

In the present study, a rapid analytical method was developed to determine the residue of sulfoxaflor in milk, pork, eggs, porcine liver, porcine kidney, porcine fat, and chicken. The dispersive solid-phase extraction (d-SPE) and multiplug filtration cleanup (m-PFC) based on multiwalled carbon nanotubes (MWCNTs) were compared for sulfoxaflor in the above matrix and then detected by ultraperformance liquid chromatography coupled with tandem mass spectrometry. The analyte was eluted within 5 min using a Waters Acquity UHPLC HSS T3 column under ESI(+) conditions. The limits of detection were 1 μg kg(-1) for all of the matrices. Good linearities of sulfoxaflor were obtained in the range of 1-100 μg L(-1), and the correlation coefficients (R(2)) were higher than 0.9988 in all matrices. The average recoveries of the target compound were between 75.5% and 114.9%, and the intraday and interday relative standard deviation values were <14%. Both methods have purification ability. While considering the cost of analysis and the applicability of the method, d-SPE was selected to purify the samples in the present study. The method was successfully used to analyze the residue of sulfoxaflor in foods of animal origin.

Use of Carbon Nanotubes for the Analysis of Pesticide Residues in Fruits and Vegetables.

This review presents the application of carbon nanotubes as sorbent materials in the analysis of pesticide residues in fruits and vegetables. The advantages, limitations, and challenges of carbon nanotubes, with respect to their use in analytical chemistry, are presented. The efficiency of their application as extraction sorbent materials (in terms of LOD, LOQ, linearity, relative recovery, and RSD) in SPE, solid-phase microextraction, multi-plug filtration clean-up, matrix solid-phase dispersion, and the quick, easy, cheap, effective, rugged and safe method is reported. The synthesis, functionalization, purification, and characterization methods of carbon nanotubes are also discussed.

The comparison of dispersive solid phase extraction and multi-plug filtration cleanup method based on multi-walled carbon nanotubes for pesticides multi-residue analysis by liquid chromatography tandem mass spectrometry

In this study, dispersive-Solid Phase Extraction (d-SPE) cleanup and multi-plug filtration cleanup (m-PFC) methods were compared for 25 representative pesticides in six matrices (wheat, spinach, carrot, apple, citrus and peanut) by QuEChERS-LC-ESI-MS/MS detection. The type of sorbents in dispersive-SPE (d-SPE) was optimized for the above matrices. Multi-walled carbon nanotubes (MWCNTs), which mixed other materials like PSA (Primary Secondary Amines), GCB (Graphitized Carbon Black) and C18 (Octadecyl-silica), showed brilliant cleanup performance in multi residue monitoring (MRM) pesticide residue analysis. Cleanup effects with d-SPE and m-PFC methods were examined. When spiked at 3 concentration levels of 10, 100, 500μg/kg in above matrices, for both d-SPE and m-PFC methods, the recoveries ranged from 70 to 110% with relative standard deviations (RSDs) lower than 20%. Limits of quantification (LOQs) for both cleanup methods ranged from 1 to 25μg/kg. Matrix-matched calibrations were performed with the coefficients of determination more than 0.99 between concentration levels of 10–1000μg/kg. It was found that m-PFC was more convenient and effective than d-SPE with the same sorbents, due to the increased contact time and contact area between the extracts and compressed sorbents. The study demonstrated that m-PFC method could be used as a rapid, convenient and high-throughput cleanup method for analysis of pesticide residues.

Rapid Multiplug Filtration Cleanup with Multiple-Walled Carbon Nanotubes and Gas Chromatography–Triple-Quadruple Mass Spectrometry Detection for 186 Pesticide Residues in Tomato and Tomato Products

This study reports the development and validation of a novel rapid cleanup method based on multiple-walled carbon nanotubes in a packed column filtration procedure for analysis of pesticide residues followed by gas chromatography-triple-quadruple tandem mass spectrometry detection. The cleanup method was carried out by applying the streamlined procedure on a multiplug filtration cleanup column with syringes. The sorbent used for removing the interferences in the matrices is multiple-walled carbon nanotubes mixed with anhydrous magnesium sulfate. The proposed cleanup method is convenient and time-saving as it does not require any solvent evaporation, vortex, or centrifugation procedures. It was validated on 186 pesticides and 3 tomato product matrices spiked at two concentration levels of 10 and 100 μg kg(-1). Satisfactory recoveries and relative standard deviations are shown for most pesticides using the multiplug filtration cleanup method in tomato product samples. The developed method was successfully applied to the determination of pesticide residues in market samples.

Multiplug filtration clean‐up with multiwalled carbon nanotubes in the analysis of pesticide residues using LC–ESI‐MS/MS

A novel design for a rapid clean-up method was developed for the analysis of pesticide residues in fruit and vegetables followed by LC-ESI-MS/MS. The acetonitrile-based sample extraction technique was used to obtain the extracts, and further clean-up was carried out by applying the streamlined procedure on a multiplug filtration clean-up column coupled with a syringe. The sorbent used for clean-up in this research is multiwalled carbon nanotubes, which was mixed with anhydrous magnesium sulfate to remove water from the extracts. This method was validated on 40 representative pesticides and apple, cabbage, and potato sample matrices spiked at two concentration levels of 10 and 100 μg/kg. It exhibited recoveries between 71 and 117% for most pesticides with RSDs < 15%. Matrix-matched calibrations were performed with the coefficients of determination >0.995 for most studied pesticides between concentration levels of 10-500 μg/L. The LOQs for 40 pesticides ranged from 2 to 50 μg/kg. The developed method was successfully applied to the determination of pesticide residues in market fruit and vegetable samples.