Page 45 - Application Handbook - Liquid Chromatography

Application No.L502
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Table 1 Analytical Conditions
[SFE] Nexera UC SFE System [GC-MS] GCMS-TQ8040
®
Extraction : A) Supercritical fluid of CO2 Column : Rxi -5Sil MS 30 m × 0.25 mm I.D., df = 0.25 µm
Solvent B) Methanol Column Temp. : 50 ˚C (1 min) → (25 ˚C/min) → 125 ˚C → (10 ˚C/min)

Flowrate : 5 mL/min → 300 ˚C (15 min)
Extraction : 8 min (Static mode → Dynamic mode) Carrier Gas : He (Constant linear velocity mode)
Extraction Linear Velocity : 47.2 cm/sec
Vessel Temp. : 40 ˚C Injection Mode : Splitless (Sampling time 1.00 min)
BPR Pressure : 15 MPa High Press Inj. : 250 kPa (1.5 min)
Trap Column : Shim-pack VP-ODS (50 mm L. × 4.6 mm I.D., 5 µm) Injection Volume : 1 µL
Elution Solvent : Acetone/Hexane = 50/50 (2 mL/min, 2 min) Interface Temp. : 250 ˚C
Ion Source Temp. : 200 ˚C
MS Mode : MRM
Loop Time : 0.3 sec
n Analysis of Brown Rice
A mixed standard solution of pesticides for GC/MS
analysis (Hayashi Pure Chemical PL2005 Pesticide GC/
MS Mix I-VI, 7) was added to pulverized brown rice to a
concentration of 100 ng/g, and SFE was performed
using the conditions shown in Table 1. The extraction
liquid obtained was made up to 2 mL using eluate, and
analyzed by GC/MS. The MRM chromatogram obtained
from GC/MS analysis is shown in Fig. 4. Good
repeatability (relative standard deviation of quantitation
concentration <10 %) and recovery (70-120 %) were
obtained for the 301 components. Repeatability and
recovery for the 301 pesticides are shown in Table 2.
This system uses a very simple pretreatment process,
and can perform automated extraction from a single
sample in approximately 30 minutes. Fig. 3 Recovery in Brown Rice Analysis

Fig. 4 MRM Chromatogram of Extraction Liquid from Brown Rice

Table 2 Repeatability and Recovery
Repeatability Repeatability
Compounds Recovery (%) Compounds Recovery (%)
(%RSD, n = 6) (%RSD, n = 6)
2-Phenylphenol 3.8 87.0 Azinphos-ethyl 5.3 84.3
Acetochlor 5.9 93.1 Azinphos-methyl 2.7 83.1
Acrinathrin-1 6.8 73.8 Benalaxyl 7.0 84.9
Acrinathrin-2 3.1 100.6 Benfluralin 5.2 90.1
Alachlor 3.6 88.7 Benfuresate 4.1 91.5
Allethrin-3,4 5.9 102.0 Benoxacor 3.2 90.8
Allidochlor 5.3 86.4 beta-BHC 5.3 87.8
alpha-BHC 4.6 88.9 beta-Endosulfan 6.5 90.7
alpha-Endosulfan 9.5 98.7 Bifenox 4.1 84.5
Ametryn 4.1 86.3 Bifenthrin 3.3 89.2
Anilofos 4.7 86.3 Biphenyl 3.5 80.5
Atrazine 4.8 86.7 Bromobutide 4.6 90.4
Azaconazole 5.5 70.5 Bromophos 5.4 90.1
Azamethiphos 9.9 78.4 Bromophos-ethyl 6.0 86.6