MCPD WG Meeting Book (May 18, 2017)

50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 70 71 72 73 74 75 76 77 78 79 80 81 82 83 84

there is no detectable blank signal). See reference to Appendix L in section 7. Validation

Guidance.

Limit of Quantitation (LOQ)

The minimum concentration or mass of analyte in a given matrix that can be reported as a quantitative result. Determined as: LOQ = blank mean + 10 standard deviations of ten independent analyses with spiked concentration of blank to be <10% of the estimated LOQ.

See reference to Appendix L in section 7. Validation Guidance.

3-MCPD

3-MCPD = 3-monochloropropane-1,2-diol or 3-chloropropane-1,2-diol. CAS NO. 96-24-2.

See figure 1 for molecular structure.

2-MCPD

Include definition

glycidol

Include definition

glycidyl esters

Include definition (include general)

Repeatability

Variation arising when all efforts are made to keep conditions constant by using the same instrument and operator, and repeating during a short time period. Expressed as the

repeatability standard deviation (SD r

); or % repeatability relative standard deviation

(%RSD r

).

Reproducibility

The standard deviation or relative standard deviation calculated from among-laboratory data. Expressed as the reproducibility relative standard deviation (SD R ); or % reproducibility

relative standard deviation (% RSD R ).

4. Method Performance Requirements:

3-MCPD Powders 25 – 500 *

3-MCPD Liquid 3 – 60 *

Analytical range

LOD LOQ

N/A

N/A ≤ 3*

≤ 25*

Accuracy (from spiked recovery)

75-110%

75-110%

% RSD r %RSD R

≤ 14%

≤ 14% ≤ 20%

Selectivity Study *μg/kg

85 86 87 88 89

5. System suitability tests and/or analytical quality control:

Suitable methods will include blank check samples, and check standards at the lowest point

and midrange point of the analytical range.

2

Made with