GC Analysis of Pesticides in Beef Kidney on SLB®-5ms (20 m x 0.18 mm I.D., 0.36 μm) after QuEChERS Cleanup using Supel™ Que Z-Sep+, MS in SIM Mode, Fast GC Analysis
CONDITIONS
sample preparation
Dispersive (QuEChERS)
sample/matrix
10 gm homogenized beef kidney spiked at 50 ng/g with pesticides
extraction tube
Supel Que Acetate (AC) Tube (55234-U)
extraction process
add 10 mL of acetonitrile; shake for 1 minute; add contents of Supel Que acetate extraction tube (55234-U); shake immediately for 1 minute; centrifuge at 3200 rpm for 5 minutes; (Sample Pretreatment: Homogenize 10 gm beef kidney and spike with pesticides at 50 ng/g.)
clean-up tube
Supel QuE Z-Sep+ tube (55296-U)
clean-up process
transfer 3 mL of the acetonitrile layer into a Supel QuE Z-Sep+ cleanup tube (55296-U); shake for 1 minute; centrifuge at 3400 rpm for 3 minutes; draw off supernatant for LVI-GCMS analysis
column
F.S. CAP. SLB-5MS 20 m x 0.18 mm I.D., 0.36 μm (28576-U)
oven
70 °C ( 0.5 min), 25 °C/min to 125 °C, 10 °C/min to 200 °C, 5 °C/min to 300 °C/min (1 min)
inj. temp.
programmed, 60 °C (0.28 min), 600 °C/min to 325 °C (5 min)
detector
MSD
MSD interface
325 °C
carrier gas
helium, 1 mL/min constant flow
injection
10 μL LVI, PTV solvent vent, rapid injection speed
liner
4 mm ID FocusLiner with taper
sample
Beef Kidney extract
Description
Analysis Note
Beef kidney was analyzed for pesticides by GC/MS-SIM after extraction and cleanup. Dispersive SPE was used for both extraction and cleanup. Since beef kideny contains approximately 5% fat, Z-Sep + was used for cleanup.
Legal Information
SLB is a registered trademark of Merck KGaA, Darmstadt, Germany
Supel is a trademark of Sigma-Aldrich Co. LLC