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Vendor Seminar

New Techniques to Simplify the Analysis of Pesticides: A New Hybrid Phase for Mini-Screenings of Very Polar Analytes and In-Line Sample Preparation for a Variety of Sample Matrices.

 

For some time now, polar contaminants have been experiencing increased interest because they are not easily accessible with existing analytical methods, such as GC or reversed-phase LC.  Polar pesticides, for example, cannot be included into the large panels for screening methods in food safety analysis.


Various suppliers have now successfully applied novel mixed-mode separation phases to the analysis of polar compounds like polar pesticides or polar, short-chain PFAS.

In this vendor seminar, Dr. Emanuele Ceccon will show how such a mixed-mode column can be applied in mini-screenings for even larger groups of similar components.


Up to 17 polar pesticides, including glyphosate, can be detected in one run, which has led to a method based on this column recently being included in the QuPPe document of the European Reference Laboratory for Single Residue Analysis.

Sample preparation stays a key in pesticide analysis. In the past, QuEChERS, invented by Michelangelo Anastasiadis and Steve Lahotey, has shown to be a good compromise to extract compounds of interest from difficult matrices like food commodities.

Nevertheless, QuEChERS stays difficult to be automized. In the second part of this vendor seminar, Dr. Emanuele Ceccon will report about an in-line sample prep (ILSP) approach that provides a semiautomated cleanup procedure for the analysis of pesticide residues in food by LC-MS/MS. ILSP selectively retains matrix components from the sample extract and can be utilized as a standalone workflow or integrated into an existing QuEChERS workflow.

Following this vendor seminar, Restek invites you to stay for a typical Italian aperitivo for a refreshing start to the conference.

Information:
 16:35 - 17:00
 19 September 2022
Authors:
  1. Emanuele Ceccon
Affiliations:
Restek Corporation
Presenters:
Emanuele Ceccon
 

Poster Presentation

GC-MS/MS 200+ Multiresidue Pesticide Screening Workflow—Comparison of Conventional 30 m Column and LPGC Kit

Sample throughput is one of the most important productivity goals for most testing labs. While there are several ways to increase the speed of GC analysis, the low-pressure gas chromatography (LPGC) technology is unique in using a shorter, wide-bore column rather than a shorter, narrow-bore column. Low-pressure GC-MS (LPGC-MS) is a technique that uses the MS vacuum system along with a specially designed column setup to lower pressure inside the entire column, thereby significantly speeding up analysis. By using a 0.53 mm ID analytical column that is inserted directly into the MS and is connected to a narrow-bore guard column acting as a flow restrictor on the GC inlet side, low pressure can be maintained throughout the 0.53 mm ID analytical column. Using LPGC-MS, some efficiency is traded for speed; however, because a mass spectrometer is used, most coeluting components can be deconvoluted by the MS detector. The analytical column's wider ID and thicker film also provide higher capacity, robustness, and inertness. To demonstrate the technique, spinach was spiked with over 200 pesticides at two levels,100 ppb and 10 ppb.  Spinach samples were prepared using a QuEChERS procedure followed by analyses comparing the conventional 30 m x 0.25 mm x 0.25 μm column to the LPGC-MS column set.  Using this technique, a conventional GC pesticides analysis is three to four times faster delivering a significant increase in throughput and lab productivity.
Authors:
  1. Hansjorg Majer
Affiliations:
Restek Corporation
Presenters:
Hansjorg Majer
 
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LC-MS/MS Analysis of Glyphosate and Polar Contaminants in Food Using a Hybrid Ion-Exchange/HILIC Column

The safety residual level of glyphosate in food is regulated in the U.S., Europe, and other global regions. Direct analysis of underivatized glyphosate, however, can be challenging due to its minimum retention on a reversed-phase or hydrophilic interaction chromatography (HILIC) column and severe adsorption onto the stainless flow path. On the other hand, glyphosate and other polar anionic contaminants tend to strongly retain on an anion-exchange column and require high salt mobile phase to elute, which is not friendly to mass spectrometric analysis.


These challenges motivated the invention of a hybrid ion-exchange/HILIC column offering balanced retention and separation of ionic and other highly polar compounds. An LC-MS/MS solution was developed for the direct analysis of underivatized glyphosate, aminomethylphosphonic acid (AMPA), and glufosinate, as well as other 14 highly polar contaminants listed in the Quick Polar Pesticides Extraction (QuPPe) method in seven food matrices (rice, baby cereal, soybean, lemon grass, oregano, tea, and strawberry). All 17 compounds were analyzed simultaneously in a single run with a total analysis time of less than 19 minutes. This method was able to chromatographically separate components sharing the same mass fragments, including AMPA/fosetyl aluminum and fosetyl aluminum/phosphonic acid. This approach enabled by unique column selectivity allows for the analysis of multiple polar pesticides in a simple method suitable for routine analysis.


Authors:
  1. Emanuele Ceccon
Affiliations:
Restek Corporation
Presenters:
Emanuele Ceccon
 
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PDF

Semiautomated Method for In-Line Removal of Matrix Components from Food for the Analysis of Residual Pesticides by LC-MS/MS

In-line sample prep (ILSP) provides a semiautomated cleanup procedure for the analysis of pesticide residues in food by LC-MS/MS. ILSP selectively retains matrix components from the sample extract and can be utilized as a standalone workflow or integrated into an existing QuEChERS workflow. In these experiments, ILSP was applied to multiple challenging commodities representing a wide range of compositions, including soy meal, avocado, whole orange, black tea, and hibiscus tea for the analysis of 61 pesticides. This solution provides a novel, semiautomated approach to reduce the abundance of matrix components entering the analytical column and MS source, resulting in a decrease in instrument contamination and an improvement in data quality. Recoveries were tested at 10 ng/g for each commodity and returned acceptable values (70-120% recovery with %RSD ≤20%) for 98% of pesticides in soy meal, 95% in avocado, 98% in black tea, 82% in hibiscus tea, and 87% in whole orange. The semi-automation of the methodology reduces error, simplifies sample preparation, and increases throughput compared to traditional extraction and cleanup techniques for a streamlined approach for the analysis of pesticide residues in food commodities.
Authors:
  1. Emanuele Ceccon
Affiliations:
Restek Corporation
Presenters:
Emanuele Ceccon
 
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PDF