Page 45 - Application Notebook - Solution for Food Safety

Application No.C99
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n Acetonitrile Extraction Efficiency Using QuEChERS
Method
To check the efficiency of acetonitrile extraction by the with and without the addition of matrix. However,
QuEChERS method, standard solution was added at relatively poor recoveries were seen for highly polar
stage (2) of Fig. 1 to obtain a concentration of 10 µg/L, compounds such as tetracycline and quinolone. For
and the recoveries were determined. Good recoveries these compounds, it is necessary to examine the use of
of approximately 80 % were obtained in cases both a separate extraction solvent and extraction reagent.

Table 2 Recoveries (Pre-Spike)
Recovery Without Matrix With Matrix (Pork) Compounds with Poor Recovery
< 50 % 17 (19 %) 13 (15 %)
Tetracyclines Quinolones
50 % - 70 % 1 (1 %) 8 (9 %)
> 70 % 71 (80 %) 68 (76 %)

n Robustness
We checked the long-term stability of the instrument measurement of an extremely complex matrix over a
using a solution of pork crude extract (spiked with period of 3 days, we were able to obtain stable data.
10 µg/L standard solution). Even after continuous

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Fig. 6 Area Plot and %RSD of Typical Compounds with Continuous Analysis

Table 3 Analytical Conditions
Column : Shim-pack XR-ODS Ⅱ (75 mm × 2.0 mm I.D., 2.2 µm)
Mobile Phase A : 0.1 % Formic Acid - Water
Mobile Phase B : Acetonitrile
Time Program : 1 %B (0 min) → 15 %B (1 min) → 40 %B (6 min) → 100 %B (10-13 min) → 1 %B (13.01-16 min)
Flowrate : 0.2 mL/min.
Injection Volume : 2 µL (2 µL sample solution + 10 µL water)
Oven Temperature : 40 °C
Ionization Mode : ESI (Positive / Negative)
Probe Voltage : +2.0 kV / -1.0 kV
Neburizing Gas Flow : 3.0 L/min.
Drying Gas Flow : 10.0 L/min.
Heating Gas Flow : 10.0 L/min.
Interface Temperature : 400 °C
DL Temperature : 200 °C
Block Heater Temperature : 400 °C

First Edition: Jan. 2015

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