Determination of 19 sulfonamides residues in pork samples by combining QuEChERS with dispersive liquid-liquid microextraction followed by UHPLC-MS/MS

Abstract

A new simple and rapid pretreatment method for simultaneous determination of 19 sulfonamides in pork samples was developed through combining the QuEChERS method with dispersive liquid-liquid microextraction followed by ultra-high performance liquid chromatography with tandem mass spectrometry. The sample preparation involves extraction/partitioning with QuEChERS method followed by dispersive liquid-liquid microextraction using tetrachloroethane as extractive solvent and the acetonitrile extract as dispersive solvent that obtained by QuEChERS. The enriched tetrachloroethane organic phase by dispersive liquid-liquid microextraction was evaporated, reconstituted with 100 μL acetonitrile/water (1:9 v/v) and injected into an ultra-high performance liquid chromatography with a mobile phase composed of acetonitrile and 0.1% v/v formic acid under gradient elution and separated using a BHE C column. Various parameters affecting the extraction efficiency were investigated. Matrix-matched calibration curves were established. Good linear relationships were obtained for all analytes in a range of 2.0-100 μg/kg and the limits of detection were 0.04-0.49 μg/kg. Average recoveries at three spiking levels were in the range of 78.3-106.1% with relative standard deviations less than 12.7% (n = 6). The developed method was successfully applied to determine sulfonamide residues in pork samples.

Trends in sensitive detection and rapid removal of sulfonamides: A review

“…QuEChERS combined with other sample preparation techniques is another useful approach to achieve simplicity, a high enrichment efficiency, and a relatively short analysis time. QuEChERS coupled with dispersive liquid-liquid microextraction (DLLME) has been used for the separation and preconcentration of trace-level sulfonamides from pork samples, F I G U R E 8 Successive steps to illustrate the DLLME process demonstrating the potential for enrichment of sulfonamides in food samples at the trace level [102].…”

Sample preparation for large‐scale bioanalytical studies based on liquid chromatographic techniques

“…Some applications in bioanalysis are reported, but they are not used in large‐scale studies. For example, this technique has been applied to extraction of metabolites in biomatrices (Kim et al, ), or in combination with other extraction techniques (dispersive liquid–liquid microextraction) for isolation of sulfonamide residues in pork samples (X. Li, Yu, Peng, & Gan, ).…”

Determination of sulfonamides in milk by capillary electrophoresis with PEG@MoS 2 as a dispersive solid-phase extraction sorbent

“…By another method, a new type of automatic online SPE procedure coupled with CE, was developed to analyse SAs in sewage [ 36 ]. To improve the speed and reduce the cost, a QuEChERS (quick, easy, cheap, effective, rugged and safe) and liquid–liquid micro-extraction method was used for the extraction of 19 types of SAs in pork samples, and an ultra-high-performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS) method was used to achieve good linearity and recovery [ 37 ]. Some novel materials, including metal-organic frameworks and graphene-based materials, were used for the enrichment of SAs in different samples [ 19 , 21 , 38 , 39 ].…”