www.restek.com 7.5-Min Screening Analysis of Multiresidue Pesticides in Brown Rice Flour Featured Application: Multiresidue Pesticide Mix Extracted from Brown Rice Flour Using QuEChERS Extraction and Cleanup • 7.5-min analysis with complete analytical cycle time of less than 10 min. • Over 90% of the 200+ residues analyzed exhibit recoveries between 70-120%. • Compatible with both traditional HPLC and modern UHPLC instruments. Analysis of multiresidue pesticides is no easy task, and it’s made even more difficult by complex sample matrices and the sophistication of the LC- MS/MS instrumentation commonly used for analysis. An LC-MS/MS can provide remarkable sensitivity, even allowing a degree of chromatographic coelutions to exist and still quantitatively monitor analytes of interest. However, too many coelutions can overwhelm the mass spectrometer, so a good chromatographic method is still essential. The optimized chromatographic method described here allows the analysis of hundreds of com- pounds in as little as 7.5 minutes with a total cycle time under 10 minutes, ensuring fast, accurate sample screening and increased lab productivity. As detailed below, a sample of brown rice flour was fortified with all of the components included in the Restek LC multiresidue pesticide kit, ex- tracted with Q-sep QuEChERS extraction salts, cleaned up using dSPE, and analyzed using a 2.7 µm Raptor ARC-18 column. The inherent efficiency of a 2.7 µm superficially porous particle column produces narrow peaks, which permits more compounds to be fit into a given unit of time. The selectivity of the Raptor ARC-18 stationary phase ensures that compounds elute throughout the entire length of the analysis, which avoids crowd- ing compounds in time and potentially taxing the mass spectrometer’s ability to monitor all the relevant ions effectively. Note that it is important to keep internal system volume down to a minimum, so selecting narrow-bore LC tubing and avoiding excess lengths of tubing will help produce the narrowest peaks and achieve the quickest, most efficient chromatography. This analysis of multiresidue pesticides in brown rice flour uses straightforward mobile phases that are mass spec friendly and a flow rate that keeps the back pressure within the operating range of conventional HPLC instruments. These advantages make it possible to analyze over 200 pesticides, surrogates, and internal standards—even in such a challeng- ing matrix—in a matter of minutes.
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www.restek.com
7.5-Min Screening Analysis of Multiresidue Pesticides in Brown Rice Flour
Featured Application: Multiresidue Pesticide Mix Extracted from Brown Rice Flour Using QuEChERS Extraction and Cleanup
• 7.5-min analysis with complete analytical cycle time of less than 10 min.
• Over 90% of the 200+ residues analyzed exhibit recoveries between 70-120%.
• Compatible with both traditional HPLC and modern UHPLC instruments.
Analysis of multiresidue pesticides is no easy task, and it’s made even more difficult by complex sample matrices and the sophistication of the LC-MS/MS instrumentation commonly used for analysis. An LC-MS/MS can provide remarkable sensitivity, even allowing a degree of chromatographic coelutions to exist and still quantitatively monitor analytes of interest. However, too many coelutions can overwhelm the mass spectrometer, so a good chromatographic method is still essential. The optimized chromatographic method described here allows the analysis of hundreds of com-pounds in as little as 7.5 minutes with a total cycle time under 10 minutes, ensuring fast, accurate sample screening and increased lab productivity.
As detailed below, a sample of brown rice flour was fortified with all of the components included in the Restek LC multiresidue pesticide kit, ex-tracted with Q-sep QuEChERS extraction salts, cleaned up using dSPE, and analyzed using a 2.7 µm Raptor ARC-18 column. The inherent efficiency of a 2.7 µm superficially porous particle column produces narrow peaks, which permits more compounds to be fit into a given unit of time. The selectivity of the Raptor ARC-18 stationary phase ensures that compounds elute throughout the entire length of the analysis, which avoids crowd-ing compounds in time and potentially taxing the mass spectrometer’s ability to monitor all the relevant ions effectively. Note that it is important to keep internal system volume down to a minimum, so selecting narrow-bore LC tubing and avoiding excess lengths of tubing will help produce the narrowest peaks and achieve the quickest, most efficient chromatography. This analysis of multiresidue pesticides in brown rice flour uses straightforward mobile phases that are mass spec friendly and a flow rate that keeps the back pressure within the operating range of conventional HPLC instruments. These advantages make it possible to analyze over 200 pesticides, surrogates, and internal standards—even in such a challeng-ing matrix—in a matter of minutes.
• Analyze hundreds of pesticides in less than 10 minutes.
• LC multiresidue pesticide kit simplifies standard preparation.
Column Raptor ARC-18 (cat.# 9314A12)Dimensions: 100 mm x 2.1 mm IDParticle Size: 2.7 µmPore Size: 90 ÅGuard Column: Raptor ARC-18 EXP guard column cartridge 5 mm, 2.1 mm ID, 2.7 µm (cat.# 9314A0252)Temp.: 50 °CSample LC multiresidue pesticide kit (cat.# 31971)Diluent: Water:acetonitrile 9:1Conc.: 1 ng/mL see notes for detailsInj. Vol.: 5 µLMobile Phase A: 0.2% Formic acid, 2 mM ammonium formate in waterB: 0.2% Formic acid, 2 mM ammonium formate in methanol Time (min) Flow (mL/min) %A %B 0.00 0.4 95 5 2.00 0.4 40 60 4.00 0.4 25 75 6.00 0.4 0 100 7.50 0.4 0 100 7.51 0.4 95 5 9.50 0.4 95 5 Detector MS/MSIon Mode: ESI+/ESI-Mode: Scheduled MRMInstrument UHPLCNotes Although the ten LC multiresidue pesticides kit mixes are formulated to ensure maximum long-term
stability and reliability as packaged, stability may become an issue when a large number of compounds with different chemical functionalities are combined together into a single mix. This should be taken into consideration for quantitative analysis.
Sample Preparation: Brown rice flour (10 g), purchased from a local market, was mixed with 10 mL water. After mixing for 10
min, the brown rice flour was fortified at 10 ng/g with all residues from the LC multiresidue pesticide kit (cat.# 31971), which had been previously combined into a single mixture that day. The fortified brown rice flour suspension was then mixed for 30 min to ensure uniform dispersion of the added pesticide residues in the brown rice flour suspension. Extraction was performed using 10 mL of acetonitrile and original unbuf-fered QuEChERS salts (cat.# 25848). After centrifugation, 1 mL supernatant was added to a 2 mL dSPE vial containing magnesium sulfate, PSA, and C18 (cat.# 26125) for cleanup. After centrifugation, 100 µL of the 10 ng/mL extract was diluted with 900 µL water and injected onto the UHPLC.
tR Precursor Product Product Peaks (min) Ion Ion 1 Ion 2
tR Precursor Product Product Peaks (min) Ion Ion 1 Ion 2
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kit
LC Multiresidue Pesticide Kit
Contains 1 mL each of these mixtures. cat.# 31971 (kit)
Quantity discounts not available.* Note: When combining a large number of compounds with different chemical functionalities, mix stability can be an issue. In formulating these standards, we extensively studied the 204 compounds involved, then grouped them into as few mixes as possible while still ensuring maximum long-term stability and reliability. For quantitative analysis, we recommend analyzing each mix separately to ensure accurate results for every compound.** Note: In this standard, fluazinam should only be used for qualitative analysis. A single-component standard (cat.# 31982) is available for quantitative analysis.
Cat.# 31972: LC Multiresidue Pesticide Standard #1 (13 components)
Organophosphorus Compounds100 µg/mL each in acetonitrile,
Maximum cartridge pressure: 1,034 bar/15,000 psi* (UHPLC), 600 bar/8,700 psi (2.7 µm); 400 bar/5,800 psi (5 µm) * For maximum lifetime, recommended maximum pressure for UHPLC particles is 830 bar/12,000 psi.Hybrid Ferrule U.S. Patent No. 8201854, EXP Holders U.S. Patent No. 8696902, EXP2 Wrench U.S. Patent No. D766055. Other U.S. and Foreign Patents Pending. The EXP, Free-Turn, and the Opti- prefix are registered trademarks of Optimize Technologies, Inc.
Raptor EXP Guard Column Cartridges
Description Method Material qty. cat.#
Q-sep QuEChERS Extraction Kit original unbuffered 4 g MgSO4, 1 g NaCl with 50 mL Centrifuge Tube
50 packets & 50 tubes 25848
Q-sep QuEChERS Extraction Salts
Method Material Volume qty. cat.#Foodstuffs with fats and waxes (e.g., cereals, avocado, nuts, seeds, and dairy)AOAC 2007.01 150 mg MgSO4, 50 mg PSA, 50 mg C18-EC 2 mL 100-pk. 26125
PSA—primary and secondary amineGCB—graphitized carbon black
Q-sep QuEChERS dSPE Tubes for Extract Cleanup Fast, Simple Sample Prep for Multiresidue Pesticide Analysis
Multiple sorbents are used to extract different types of interferences.MgSO4—removes excess water.PSA—removes sugars, fatty acids, organic acids, and anthocyanine pigments.C18-EC (end-capped)—removes nonpolar interferences.GCB—removes pigments, sterols, and nonpolar interferences.
Note: No entry in the Method column refers to dSPE formulations not specifically included in one of the cited references. These products can be used to accommodate the various needs of specific matrices not directly met by the cited references.
Length2.1 mm
cat.#3.0 mm
cat.#4.6 mm
cat.#1.8 µm Columns30 mm 9314232 — —50 mm 9314252 931425E —100 mm 9314212 931421E —150 mm 9314262 — —2.7 µm Columns30 mm 9314A32 9314A3E 9314A3550 mm 9314A52 9314A5E 9314A55100 mm 9314A12 9314A1E 9314A15150 mm 9314A62 9314A6E 9314A655 µm Columns30 mm — 931453E —50 mm 9314552 931455E 9314555100 mm 9314512 931451E 9314515150 mm 9314562 931456E 9314565250 mm — — 9314575
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