In
this work, a stable isotope dilution ultrahigh-performance liquid
chromatography triple quadrupole tandem mass spectrometry (UHPLC–QqQ-MS/MS)
method was developed and validated for simultaneous determination
of N
ε-(carboxymethyl)lysine (CML), N
ε-(carboxyethyl)lysine (CEL), and acrylamide
(AA) in baked and fried foods. Ground food samples were extracted
with acetone followed by two parallel assays. In assay A, a cleanup
procedure based on dispersive solid-phase extraction was conducted
for AA, free CML, and CEL analysis using the supernatant. In assay
B, a multistep process including reduction, protein precipitation,
acid hydrolysis, and solid-phase extraction was conducted for bound
CML and CEL analysis using precipitation. The developed method was
validated in terms of linearity, sensitivity (limit of detection,
LOD; limit of quantitation, LOQ), accuracy, and precision. The results
showed that the method had a wide linear range (0.25–500 ng/mL
for CML and CEL, 0.5–500 ng/mL for AA), low LOD and LOQ (0.47–0.94
and 1.52–1.91 μg/kg, respectively), and good linearity
(R
2 > 0.999). The recovery test on
baby
biscuit and French fries samples showed the recovery rates of 90.2–108.3%
for CML, 89.0–106.1% for CEL, and 94.5–112.3% for AA
with satisfactory precision (relative standard deviation (RSD) <
10%). Finally, the developed method was successfully applied to 11
baked and fried food samples, and total CML, CEL, and AA contents
varied in the ranges of 4.07–35.88 mg/kg, 1.99–14.49
mg/kg, and 5.56–506.64 μg/kg, respectively. Therefore,
the isotope dilution UHPLC–QqQ-MS/MS method developed herein
is promising for routine analysis of CML, CEL, and AA in baked and
fried foods.