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2
there is no detectable blank signal). See reference t
o Appendix Lin section 7. Validation
50
Guidance.
51
52
Limit of Quantitation (LOQ)
53
The minimum concentration or mass of analyte in a given matrix that can be reported as a
54
quantitative result. Determined as: LOQ = blank mean + 10 standard deviations of ten
55
independent analyses with spiked concentration of blank to be <10% of the estimated LOQ.
56
See reference to Appendix L in section 7. Validation Guidance.
57
58
3-MCPD
59
3-MCPD = 3-monochloropropane-1,2-diol or 3-chloropropane-1,2-diol. CAS NO. 96-24-2.
60
See figure 1 for molecular structure.
61
62
2-MCPD
63
Include definition
64
65
glycidol
66
Include definition
67
68
glycidyl esters
69
Include definition (include general)
70
71
Repeatability
72
Variation arising when all efforts are made to keep conditions constant by using the same
73
instrument and operator, and repeating during a short time period. Expressed as the
74
repeatability standard deviation (SD
r
); or % repeatability relative standard deviation
75
(%RSD
r
).
76
77
Reproducibility
78
The standard deviation or relative standard deviation calculated from among-laboratory
79
data. Expressed as the reproducibility relative standard deviation (SD
R
); or % reproducibility
80
relative standard deviation (% RSD
R
).
81
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4.
Method Performance Requirements:
83
84
3-MCPD
Powders
3-MCPD
Liquid
Analytical range
25 – 500 *
3 – 60 *
LOD
N/A
N/A
LOQ
≤ 25*
≤ 3*
Accuracy (from spiked recovery)
75-110%
75-110%
% RSD
r
≤ 14%
≤ 14%
%RSD
R
≤ 20%
Selectivity Study
*μg/kg
85
86
5.
System suitability tests and/or analytical quality control:
87
Suitable methods will include blank check samples, and check standards at the lowest point
88
and midrange point of the analytical range.
89