productivity enhancement for sample preparation using

Productivity Enhancement for Sample Preparation Using
Accelerated Solvent Extraction with In-cell Clean-up and
Complementary Batch Evaporation
S. Henderson, R. Carlson, E. Francis, B. Murphy, B. Dorich, J. Peterson, and B. Richter
Thermo Fisher Scientific, Salt Lake, UT, USA
Improved sample preparation
techniques can reduce sample
handling
Many sample preparation techniques lack consistency between steps.
A system designed to combine sample prep tasks such as extraction,
filtration, and clean-up can reduce sample handling and speed up the total
sample preparation process. Specifically, reduced sample handling can:
• Minimize sample ID recording errors
• Minimize quantitative transfer and minimize analyte loss
• Eliminate additional processing steps such as post-extraction
clean-up
• Decrease labor and improve throughput
• Reduce consumable expenditure and waste
What Is ACCELERATED SOLVENT
EXTRACTION?
Load Cell
Pump
Solvent
Fill with
solvent
0.5–1 min
Purge Valve
Heat and
pressurize
Static
Extraction
5 min
Oven
Extraction
Cell
5 min
Cycle
N2
Flush with
0.5 min
fresh solvent
Purge with
nitrogen
1–2 min
Extract
ready
Total
12–18 min
Nitrogen
Static
Valve
Collection
Vial
17567-01
Figure 1. Accelerated solvent extraction schematic.
Accelerated solvent extraction is an automated extraction technique that
uses liquid solvents and solvent mixtures including organic solvents,
aqueous buffers, and water to extract solid or semisolid samples including
soils, sludges, sediments, vegetation, tissues, plastics, polymers, tablets,
and consumer products. Accelerated solvent extraction uses elevated
temperatures (40–200 °C) and pressures (500–3000 psi) to increase
diffusion rates of analytes from the matrix to the solvent.
Thermo Scientific™
Dionex™ ASE™ 100 Accelerated
Solvent Extractor
Dionex ASE 200
Accelerated Solvent Extractor
Dionex ASE 300
Accelerated Solvent Extractor
Dionex SE 500 and SE 400 Extractors
1
ACCELERATED SOLVENT EXTRACTION
BENEFITS
Time/Labor Comparison of Accelerated Solvent
Extraction versus Sonication for Extraction of Soils
• Recovery of compounds listed under U.S. EPA Method 8270C,
spiked at 100 ppb: results from Laboratory Control Samples (LCS)
16 matrix spike compounds
– Recoveries for sonication: average 70.2%; 12.9% RSD
– Recoveries for accelerated solvent extraction: average 69.8%;
6.8% RSD
Table 1. Sonication vs. ASE
Sonication—Non-Dionex
Sonication 3550
(Four Horns)
Accelerated solvent extraction
—Dionex ASE 200 Extractor
Weigh Mix and Spike
3 min per sample;
labor intensive
3 min per sample;
labor intensive
Extract with Solvent
4 samples in 15 min;
labor intensive
1 sample in 15 min;
automated
Filtration
10 min per sample;
labor intensive
Included in extraction;
automated
Concentration on
TurboVap® II/SE 500
Transfer 2 min per sample;
300 mL to 1 mL;
90 min for 12 samples
No transfer required;
50 mL to 1 mL;
30 min for 12–24 samples
Total Time for 12 Samples
315 min;
255 min labor
256 min;
66 min labor
Time and Labor Comparison for Extraction of
Perchlorate in Soil with In-Cell Clean-Up
• Perchlorate recoveries by sonication; avg. 11.5 µg/kg; RSD 0.4%
• Perchlorate recoveries by accelerated solvent extraction; avg.
12.7 µg/kg; RSD 0.2%
Extraction
Sample and
Dispersant
Absorbents added
to cell to retain
interferences
Table 2. Extraction of Perchlorate in Soil
Sonication Bath and
Cartridge Clean-Up
Weigh Mix and Spike
3 min per sample;
labor intensive
Add absorbent to cell;
5 min per sample;
labor intensive
Vortex Samples
12 samples in 15 min;
labor intensive
—
Extract with Solvent
12 samples in 30 min;
sonication
1 sample in 15 min;
automated
Centrifuge
4 samples in 15 min;
—
Filtration and Clean-Up
Prep C18 cartridges;
run extract through cartridge;
10 min per sample;
labor intensive;
Included in extraction;
automated
Total Time for 12 Samples
251 min;
labor intensive
labor = 221 min
250 min;
automation;
labor = 60 min
EXPERIMENTAL
Sample Preparation with Integrated Clean-Up and
Compatible Solvent Evaporation for Polybrominated
Flame Retardants (PBDE)
Integrated Clean-up of Salmon Extracts; Accelerated Solvent
Extraction PBDE Results
Salmon fillets were spiked with known quantities of BPDE compounds
and allowed to sit overnight. They were then extracted using Dionex ASE
Extraction and in-cell clean-up followed by solvent evaporation to 1 mL.
Accelerated Solvent Extraction PBDE Recoveries
Accelerated solvent extraction recoveries range from 36% to 105%.
6 g alumina and 4 g of silica gel were used per 3.5 g of salmon tissue.
(The amount of alumina and silica gel is critical for optimum lipid
absorption.) Dionex ASE Extractor extracts required no additional
clean-up.
• Analyzed by Agilent Tech., (GC) 6890N, with a GCMate™ II (MS),
ionization mode, electron-capture negative ionization (ECNI),
monitoring bromines (79 and 81 m/z).
• DB5-HT column (30 m).
• Figure 4A is the calibration check.
Fiqure 2. Schematics of in-cell clean-up for selective extractions.
2
Dionex ASE 200 Extractor with
In-Cell Clean-Up
Productivity Enhancements for Sample Preparation Using Accelerated Solvent Extraction with
In-Cell Clean-Up and Complementary Batch Evaporation
Table 3. Accelerated Solvent
Extraction PBDE Recoveries
PBDEs
Target ng/mL
BDE-28
57
%Recovery
–47
57
71
–100
57
81
78
–99
57
78
–154
57
62
–153
57
61
–140
57
104
–183
57
56
–209
570
36
Figure 3. Extracts with and without in-cell
clean-up of fish tissue using alumina, silica
gel, and acidic silica gel (40% H2SO4).
Figure 4. PBDE recoveries. (A) Calibration check and (B) salmon sample extract
with in-cell clean-up.
3
Conclusions
Acknowledgments
Sample preparation time can be decreased by 10–30% using the Dionex
ASE Accelerated Solvent Extractor due to improved consistency, reduced
sample handling, and increased sample throughput. Labor for sample
processing can be decreased by 50–75%. Additionally, reduced sample
handling will minimize sample transfer errors and analyte loss.
Rosanne Slingsby, Dionex Corporation (now part of Thermo Scientific);
Don Cogswell, Utah Department of Health; Mark LaGuardia, Virginia
Institute of Marine Science (PBDE extraction data); Dale Hoover, Axys
Laboratory; Greg Hess, American West Analytical Laboratory.
Minimize Labor
• 50–75% reduction
Reduce Sample Handling
• Minimize transfer errors.
• Reduce analyte loss due to quantitative transfers.
www.thermoscientific.com/dionex
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