Page 30 - Application Handbook - Liquid Chromatography

Application No.L503
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n Extraction and Analysis of Residual Pesticides in Soil Mix 1 g of dehydrating agent with 1 g of soil
Soil was spiked with 200 ng/g each of eight pesticide
components, which were then extracted by SFE using Add mixture to extraction vessel
the conditions indicated in Table 1. Eluent was added to
the extract obtained to make 2 mL, which was then Collect extract from SFE
analyzed by LC-MS/MS using the conditions indicated in
Table 1. Repeatability and recovery rate values for the Add eluent to make 2 mL
eight pesticide components are shown in Table 2. Analyze by LC-MS/MS
Recovery rates were determined by comparing the area
of pesticide peaks measured from the extract obtained Fig. 3 Process Flow from Pretreatment to Analysis
from the soil spiked with pesticide and measured from
the extract obtained from unspiked soil to which the
pesticides were added after extraction. This system uses
a simpler and faster pretreatment process than liquid-
liquid extraction, which enables it to finish extraction in
about 30 minutes per sample. It also uses less organic
solvent, so it is superior in terms of the environment
and cost as well.

Table 1 Extraction and Analytical Conditions
[SFE] Nexera UC SFE System [LC] Nexera X2 System
Solvent : A) Supercritical fluid of CO2 Column : Shim-pack UC-RP (150 mm L. × 2.1 mm I.D., 3 μm)
B) Methanol Mobile Phase : A) 10 mM Ammonium formate
Flowrate : 5 mL/min B) 10 mM Ammonium formate in methanol
Extraction : 4 min (Static mode → Dynamic mode) Time Program : B.Conc. 0 % (0 min) → 100 % (14-17 min) →
Extraction : 40 °C 0 % (17.1-20 min)
Vessel Temp. Flowrate : 0.4 mL/min
BPR Pressure : 15 MPa Column Temp. : 40 °C
Trap Column : Shim-pack VP-ODS (50 mm L. × 4.6 mm I.D., 5 μm) Injection Volume : 3 μL
Column : 40 °C
Oven Temp. [MS] LCMS-8060 (MRM mode)
Elution Solvent : Acetone/Hexane = 50/50 (2 mL/min, 2 min) Ionization : ESI (positive or negative)
DL Temp. : 200 °C
Block Heater Temp. : 400 °C
Interface Temp. : 300 °C
Nebulizing Gas Flow : 2 L/min
Drying Gas Flow : 10 L/min
Heating Gas Flow : 10 L/min

Table 2 Repeatability and Recovery
8500000
8000000 Compounds Repeatability Recovery (%)
7500000 (%RSD, n=6)
7000000
6500000 Alachlor 1.9 87.0
6000000
5500000 Atrazine 1.3 75.8
5000000 Diflufenican 1.2 86.2
4500000
4000000 Fipronil 1.5 80.6
3500000
3000000 Flumioxazin 3.8 70.1
2500000 Fluxapyroxad 2.2 72.9
2000000
1500000 Pyraclostrobin 1.8 73.3
1000000
500000 Trifloxystrobin 1.5 87.7
0
10.0 10.5 11.0 11.5 12.0 12.5 13.0 13.5 14.0 14.5 min
Fig. 4 MRM Chromatogram of Extract from Soil Spiked with Pesticides

First Edition: Feb. 2016

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