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Quantitation of Acrylamide in Food Samples on the Finnigan TSQ Quantum Discovery by LC/APCI-MS/MS

Offset: 6 V
Scan Mode: Selective Reaction Monitoring
Q2 Pressure: 1.0 mTorr argon
SRM Transitions: m/z 72→55 for acrylamide; m/z 75→58 for d3-acrylamide
Collision Energy: 13 eV
Scan Width: 1.0 u
Scan Time: 0.3 s (each SRM transition)
Q1, Q3 Resolution: Unit (0.7 u FWHM)

Results and Discussion
Prior to the acquisition of acrylamide standards, it was important to determine if there was any detectable native acrylamide contribution originating from the deuterated internal standard. As shown in Figure 1, there is no acrylamide signal observed for the m/z 72→55 SRM transition at the same retention time as the 50 ng/mL d3-acrylamide standard.

The limit of quantitation (LOQ) for acrylamide on the Finnigan TSQ Quantum Discovery was 0.25 ng/mL acrylamide or 2.5 pg on column (Figure 2). This compares favorably to LOQs previously reported by other research groups, including an 8-fold improvement over the mass LOQ by LC/ESI-MS/MS (20 pg)1 and a 40-fold improvement over the concentration LOQ on the TSQ 7000 (10 ng/mL),5 which used an LC/APCI-MS/MS method.

The calibration curve for acrylamide from 0.25 ng/mL to 2500 ng/mL is displayed in Figure 3. This calibration curve was generated using the column-switching LC method just prior to the acquisition of the food extracts data. A linear regression fit to these data using 1/x weighting yielded the following equation: y = 5.5997 104 + 0.0206125x. The correlation coefficient for this curve was r2 =0.9999, indicating excellent linearity across the four order-of-magnitude dynamic range. Table 1 lists the statistical results for the acrylamide calibration curve. At the LOQ, the accuracy, as a percent relative error, is 1.1% and the precision, as a percent coefficient of variance (%
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