Intra-Laboratory Validation of an Alternative Column Chemistry for the LC-MS/MS Analysis of Pesticides in Fruits and Vegetables Using Method EN 15662

16 Oct 2014

LC-MS/MS methods are very popular for the analysis of pesticides in food. Several methods currently exist for their extraction from a variety of different food matrices. One of the newer methods is known as the QuEChERS, this method employs dispersive solid phase extraction (SPE) for extraction and cleanup. This method is now the European Norm (EN 15662). While this method typically uses C18 HPLC columns, this application note describes an intra-laboratory comparison and validation procedure using an Ascentis® Express RP-Amide column.

Ascentis® Express RP-Amide HPLC Columns

Sigma-Aldrich Supelco

Ascentis Express RP-Amide HPLC columns are the most recent product additions to the Supelco HPLC product line. Combining an embedded polar group (EPG) stationary phase with the Fused-Core particles, Ascentis Express RP-Amide provides a host of useful benefits to the HPLC chromatographer.   Ascentis Express RP-Amide is a blend of modern phase technology and innovative particle technology. The Fused-Core particle provides benefits in terms of speed, resolution, sensitivity, and ruggedness. The one-step RP-Amide bonding chemistry provides benefits in terms of selectivity, aqueous stability, and improved peak shape for bases. Read about how this product was used to analyze Riboflavin and impurities here.     Benefits: Alternative reversed-phase selectivity to C18 Improved peak shape for bases 100% aqueous compatible reversed-phase column Column Details: Chemistry: RP-Amide Particle Size: 2.7, 5.0 μm Pore Size: 90 Å Length: 20, 30, 50, 75, 100, 150, 250 mm ID: 2.1, 3.0, 4.6 mm

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Supel™ QuE Z-Sep QuEChERS Tubes

Sigma-Aldrich Supelco

Supel QuE Z-Sep sorbents enhance sample cleanup for complex matrices by effectively removing more fat and color from sample extracts than traditional phases for QuEChERS. By eliminating problematic matrix interferences, Z-Sep products provide more robust LC-MS and GC-MS methods. This proprietary technology can replace C18 and PSA phases in your current methods without additional method development.Supel QuE Z-Sep/C18, a combination of Discovery® DSC-18 and Z-Sep particles, is recommended for samples containing <15% fat. Supel QuE Z-Sep+, C18 and Z-Sep dual bonded to silica, is recommended for cleanup of samples containing >15% fat. Supel QuE Z-Sep is recommended for the anlysis of hydrophobic analytes in fatty matrices.Features & Benefits: Useful for pesticide residue analysis Proprietary technology, significantly diminishes interference from fatty matrices and pigments Employs “Quick Easy Cheap Effective Rugged Safe” QuEChERS methodology

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LC-MSLC-MS (liquid chromatography-mass spectrometry) systems and equipment are used for separation and quantitative analysis of complex mixtures, combining liquid chromatography and mass spectrometry. Quantify proteins, contaminants, pesticides or screen for drug metabolites with a high level of sensitivity. LC-MS systems and equipment include reverse phase, normal phase and specialized columns integrated with various MS detectors such as time-of-flight (TOF), quadrupole, orbitrap or ion trap mass analyzers. LC-MS/MS instruments equipped with a qTOF or triple quadrupole analyzer give greater sensitivity and resolving power to your analysis. Find the best LC-MS equipment in our peer-reviewed product directory: compare products, check customer reviews and receive pricing direct from manufacturers.Solid-Phase ExtractionSolid-phase extraction (SPE) is used for clean-up, extraction and concentration of semi-volatile or non-volatile analytes from complex mixtures including blood, urine and food samples. Multiple formats are available for conducting SPE, including prepacked SPE cartridges, disks and microplates, as well as SPE sorbent powders for manual packing. SPE systems can be used to automate the process and extract multiple samples at once. Solid-phase microextraction (SPME) and supported liquid extraction (SLE) products are also available in the same formats. Find the best SPE, SLE and SPME equipment in our peer-reviewed product directory: compare products, check customer reviews and receive pricing direct from manufacturers.QuEChERSThe QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method is a streamlined approach that is used to extract multi-residue target compounds from food samples. It is most commonly used by analytical chemists studying pesticide residues in food.PesticidesPesticides are used to protect crops from diseases, pests and unwanted plants. They are classed as persistent organic pollutants (POPs) and can be harmful to humans. The Environmental Protection Agency (EPA) currently regulates the use of pesticides in the USA. Food TestingFood testing refers to a variety experiments including PCR, mass spectrometry, processing, QuEChERS, analyzing and Kjeldahl.