TABLE I

Operating Parameters for the LC/MS/MS Method for Measuring DEHP in the Lipid Test Extracts

Operating ParameterOperational Condition
ColumnPhenomenex Kinetex C18, 50 × 4.6 mm, 2.6 μ particle size
Column Temperature30 °C
Injection Size10 μL
Mobile Phase A10 mM Ammonium acetate
Mobile Phase B1/1 (v/v) Isopropyl alcohol/cyclohexane
Mobile Phase CAcetonitrile
Mobile Phase D1/1 (v/v) Isopropyl alcohol/acetonitrile
Mobile Phase GradientTime (min)% A% B% C% D
0300700
0.53003040
5.010990
6.0000100
12.5a010000
17.5a010000
18.0a000100
20.0a000100
21.0b300700
Mobile Phase Flow Rate1.2 mL/min
MS Operating ModeAPCI, + ion
MS/MS Scan SegmentsFor DEHP, m/z = 413.4/301.2 amu
  • Notes:

  • a These steps are column washing for removal of entrained lipid.

  • b Column equilibration.