LC/MS Analysis of Glyphosate in Oatmeal on ApHera™ NH2 after SPE using Supel™ Select HLB
材料
SPE 管或板
分析色谱柱
标准
配件
Supel™ QuE
Empty Centrifuge Tube with Lid, centrifuge tube volume 50 mL, pk of 50, suitable for EN 15662:2008 per BSCertified Vial Kit, Low Adsorption (LA), 2 mL, pk of 100
volume 2 mL, amber glass vial (with marking spot), natural PTFE/silicone septa, thread for 9 mmCONDITIONS
sample/matrix
instant oatmeal, ground
SPE tube/cartridge
Supel-Select HLB SPE, 30 mg/1 ml (54181-U)
condition
1 mL methanol, 1 mL 50:50 methanol:water
sample addition
0.5 mL extract
elution
collect the second loaded aliquot of the extract
eluate post-treatment
filter into low absorption vials
column
apHera NH2, 15 cm x 4.6 mm I.D., 5 μm particles (56401AST)
mobile phase
[A] water; [B] 20 mM ammonium carbonate, pH 9; [C] methanol:water (50:50)
gradient
100% A for 2 min, to 90% B, 10% C in 0.1 min, held until 10 min, to 100% A in 0.1 min, held for 5 min
flow rate
0.5 mL/min
pressure
3191 psi (220 bar)
column temp.
35 °C
detector
MS/MS, ESI negative, 168/63, 168/79
injection
60 μL
说明
分析说明
Direct analysis of glyphosate with LC-MS detection using the presented method is possible for oat, corn and rice products. Polymeric SPE was used for sample cleanup. Polymer-based apHera NH2 HPLC column provided stable and robust separation at basic pH.
其他说明
Sample pretreatment: 5 g of homogenized cereal was mixed wtih 10 mL water and let sit for at least 30 minutes. 10 mL 1% (v/v) formic acid in acetonitrile was added, shaken for 15 minutes on a laboratory shaker, and centrifuged.5 g of homogenized cereal was mixed wtih 10 mL water and let sit for at least 30 minutes. 10 mL 1% (v/v) formic acid in acetonitrile was added, shaken for 15 minutes on a laboratory shaker, and centrifuged.
法律信息
Supel is a trademark of Sigma-Aldrich Co. LLC
apHera is a trademark of Sigma-Aldrich Co. LLC