Modifying QuEChERS for complicated matrices- Dry Samples
25 May 2020Before getting in to this discussion, I recommend reading my previous blog post first regarding classical applications for methods based on Quechers.
QuEChERS methods were originally written to analyze pesticides in fruit and vegetable matrices, most of which have high water content and low fat content. More recently, the technique has been used for a greater variety of food and agricultural products, as well as other environmental matrices. It has also been adapted for analytes other than pesticides in some cases. We will discuss some of the possible modifications you may need to make for complicated matrices. For all of the sample types we will discuss, the best general references I can give are from the official QuEChERS website (quechers.eu), maintained by CVUA Stuttgart, specifically QuEChERS: About the method.
For greater detail, I found this reference useful: https://www.degruyter.com/view/journals/chem/open-issue/article-10.1515-chem-2015-0109/article-10.1515-chem-2015-0109.xml
For many samples, particularly food products, you may find it helpful to use the USDA database at https://fdc.nal.usda.gov/ to obtain a listing of content for water (as well as protein, total lipids, fatty acids, carbohydrates, sugars, and cholesterol). We will discuss techniques for dry sample matrices in this blog post. Other types of sample matrices will be discussed in subsequent posts.
For samples with little or no water content, water must be added before using Quechers extraction salts. For these samples, reduce the sample weight from 10 g to 5 g or less and add 10 mL of water prior to adding acetonitrile and QuEChERS extraction salts. (For those using the AOAC QuEChERS method, the sample size is reduced from 15 g to 7.5 g or less and 15 mL of water is added.) The sample weight should be adjusted according to the amount of chromatographic interference anticipated (or how “dirty” the matrix is perceived to be). Here are several examples of this technique. In some cases, such as cannabis, you might see total water volumes less than or greater than 10 ml, but the sample weights are adjusted accordingly as well.
- Brown rice flour and honey: Optimizing a 190+ Pesticides Multiresidue Screening Workflow for the Preparation and Analysis of Produce by LC-MS/MS
- Herbal tea: Multi-Residue Pesticide Analysis in Herbal Teas Using The Quechers Method and Two-Dimensional GC Time of Flight Mass Spec
- Botanical supplements: Using Modified QuEChERS for the Extraction and Analysis of Pesticide Residues in Botanical Ingredients Using GC-MS/MS
- Dried cannabis flower: Pesticide analysis for cannabis flower: method and data overview and Cannabis Plant Quechers Protocol 2016 Kowalski
- Cigarette tobacco: Evaluation of Dispersive and Cartridge Solid Phase Extraction (SPE) Cleanups for Multiresidue Pesticides in QuEChERS Extracts of Finished Tobacco Using GCxGC-TOFMS
- Ginseng (dried herbs, botanicals): Residual Pesticides Analysis of Botanical Ingredients Using Gas Chromatography Triple Quadrupole Mass Spectrometry
- Yerba mate tea (PAHs): Analytical Method for Polycyclic Aromatic Hydrocarbons (PAHs) in Yerba Mate Tea Using Modified QuEChERS, Solid Phase Extraction and GC-TOFMS and GC-MS/MS
- Potato chips (acrylamide): The Analysis of Acrylamide Using an Aqueous Compatible Reversed-Phase Column by LC-MS/MS Detection
For samples that contain a little bit of water but less than 80%, the amount of water can be adjusted accordingly to estimate a combined water content of 10 mL. Some good examples of this technique are shown below.
- Orange Peel: Optimizing a 190+ Pesticides Multiresidue Screening Workflow for the Preparation and Analysis of Produce by LC-MS/MS, Optimizing Sample Preparation for the Analysis of over 200 Multiresidue Pesticides in Produce by GC-MS/MS
- Orange peel: Analyzing orange: peel and pulp separately or as whole?
- Avocado: Analyzing avocado: How to deal with lack of water and keep the fats out
- Raisins: A Comprehensive Approach to Pesticide Residue Monitoring, Including Non-target Analysis, for Fruits, Vegetables, and Nuts, Using QuEChERS, LC-MS/MS, and GCxGC-TOFMS
Additional Resources:
- “How to choose the right dSPE for QuEChERS” video
- “Did you know QuEChERS was made to be modified” video
- QuEChERS Sample Preparation Procedures
- QuEChERS Made Even Easier
- “QuEChERS-Where to start”
This concludes discussion of dry sample matrices. Please look for the next post on samples containing high amounts of lipids and waxes.