AOAC SPIFAN Nutrients ERP-Final Review (Dec. 2018)
2015.10 (Dec. 2018) Carn-07 MLT Report FOR ERP USE ONLY DO NOT DISTRIBUTE
corresponding internal standard peak areas to obtain relative analyte responses (normalized to IS). Relative responses of each analyte in the calibration standards are plotted on the y-axis against their corresponding concentrations on the x-axis to generate calibration curves with linear fit and 1/x 2 weighting for all compounds. Analyte concentrations in the sample extracts are derived from the calibration curves and their concentrations in the samples are determined using the following equation:
C x V x D W x 1000
= mg/kg
Where: C
= = = =
Analyte concentration in sample (ng/mL).
V D
Final volume (mL). Dilution (mL/mL). Sample weight (g).
W
1000 =
Conversion from ng/g into mg/kg
Table 2015.10A. Preparation of working standard solutions
MS grade water (mL) 6.00
Concentration (µg/mL) Extracted (ng/mL)
Source solution ID Stock solutions Stock solutions Stock solutions
Source concentration (mg/mL)
Source volume (mL)
Final volume
Standard Solution
STD6
25.0
2.00 each 1.60 each 0.800 each 1.00 0.400 0.200
10.0
5000
STD5
25.0
6.80
10.0
4000
STD4
25.0
8.40
10.0
2000
STD3 STD2 STD1
STD6 STD3 STD3
5.00 0.500 0.500
9.00 9.60 9.80
10.0 10.0 10.0
500
20 10
Note: Alternate weights or volumes may be used to scale these preparations
Table 2015.10B. HPLC parameters
Column:
Zorbax 300-SCX, 3.0 x 50 mm, 5 µm (Agilent, Santa Clara, CA) 5 mM Ammonium Formate in water:ACN (50:50, v:v) with 0.2% Formic Acid 30 mM Ammonium Formate in water:ACN (50:50, v:v) with 0.2% Formic Acid
Mobile phase A:
Mobile phase B:
Injection Volume:
5-10 μL
Run Time:
4.2 minutes
Gradient program:
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