UHPLC Analysis of Bisphenol A and Analogous Compounds in Infant Formula on Titan C18 with Fluorescence Detection after SPE using SupelMIP® Bisphenol A
Materials
SPE tube or plate
Standard
accessory
sample prep
Supel™ QuE
Empty Centrifuge Tube with Lid, centrifuge tube volume 50 mL, pk of 50, suitable for EN 15662:2008 per BSCONDITIONS
sample/matrix
liquid infant formula
SPE well plate
SupelMIP Bisphenol A, 100 mg/3 mL (52775-U)
condition
3 mL 2% formic acid in methanol, 3 mL acetonitrile, 3 mL water
sample addition
as prepared
washing
9 mL of water, 6 mL of acetonitrile:water (40:60); vacuum was pulled for 3 min after the last wash
eluate post-treatment
Sample was evaporated to dryness at 45 °C, reconstuituted in 0.5 mL of acetonitrile:water (40:60). All samples were filtered through Durapore membrane filter units prior to analysis.
column
Titan C18, 10 cm x 2.1 mm I.D., 1.9 μm particles (577124-U)
mobile phase
[A] water; [B] acetonitrile
gradient
40 to 80% B in 2.5 min; held for 4.5 min; to 100%B in 0.1 min; held for 2.4 min; to 40% B in 0.1 min; held for 2.9 min
flow rate
0.25 mL/min for 7 min; to 0.40 mL/min in 0.1 min; held for 2.4 min; to 0.25 mL/min in 0.1 min.; held for 2.9 min
pressure
3916 psi (270 bar)
column temp.
35 °C
detector
fluorescence, ex: 230 nm, em: 315 nm
injection
5 μL
elution
3 mL of methanol:acetonitrile (75:25) (A017)
Description
Analysis Note
BPA can leach into foods from the contact between food and the packaging. Structurally analogous compounds could also be used in place of BPA during package manufacturing as BPA comes under more stringent regulations. The presented method was developed for analysis of this class of compounds and applied to infant formula analysis. The use of molecularly imprinted polymers during cleanup produced samples that can be analysed by fluoresent detection.
Other Notes
Sample Prep: 5 mL of liquid infant formula was spiked with 10 ppb of analytes, mixed with 5.5 mL of acetonitrile, centrifuged at 4500 rpm for 10 minutes, top 3 mL were diluted with 3 mL water to load into SPE
Legal Information
SupelMIP is a registered trademark of Sigma-Aldrich Co. LLC
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