2016 OMB Summer Meeting

38-39 / 435

Screening Team Review: Consists of a preliminary review by Working Group Chair, ERP Chair, and CSO
ERP Reviews Comments
Car‐01 – 9/2015 Car‐01 – 2/2016 Car‐02 – 2/2016
 Method uses best of the technology
available for Carotenoids
 Use of internal standards & PKB columns
could improve
 Need safety comments for the isopropyl
ether/ peroxides
 determination of the beta carotene stock
solution needs a second step
 Mobil phase D has to be stirred constantly
 A working standard injection is specified, but
nothing on how to prepare or any
chromatograms
o Information provided on six (6) samples
and one (1) lab
o Awaiting additional data
 Good method, but needs additional work
and clarification on standards (include
control sample) and purity checks
 Need to see a standard chromatogram
(including reference)
 Method needs enough samples of
Carotenoids to do an SLV
Temperature is very high (85˚)
 Method uses sound methodology
 It is clearly written and should be easy to follow
 Has description of spectrophotometric as well as chromatographic determination of
standards purity
 Uses internal standard (Apocarotenal)
 Saponification step is short and done at room temperature
 No details about how to make up a‐carotene, lutein, lycopene standards, or mixed
calibration standards.
 Clear equations describing how the standards and samples are quantitated is required.
 No data are presented for alpha‐carotene and Lycopene – doesn’t meet the scope specified
in SMPR
 Not enough validation data:
o Accuracy by spike recovery of SRM1849a at 2 levels of all‐trans lutein and all‐trans
b‐carotene – meet SMPR for recoveries and repeatability (no reference or certified
carotenoid values is available from NIST)
o Repeatability determined for only 2 SPIFAN matrices for cis and trans lutein and cis
and trans b‐carotene –data meet SMPR
 No safety concerns are noted by the authors
 Not all carotenoids specified by SMPR are determined by this method
 Only SRM 1849a and 2 SPIFAN (?) matrices were analyzed
 No details on System Suitability
 Method has issues with lycopene and
alpha carotene
 Method is clearly written and has sound
methodology, but doesn’t meet the scope
o Expand scope to include α‐carotene
and lycopene
 No data provided on alpha carotene
 No safety concerns
 Method has the potential to meet the
SMPR®
 Method only analyzed three (3) matrices
 Reassemble the working group to review
the comments for the SMPR®
 This nutrient may require four (4) SMPRs®
or some variation
 Set order of priority
 SLV may be requirement for beta carotene
and lutein
WG launched
March 2014
SMPR Approved
Sept 2014
Call for Methods
Sept 2014
April 2015
Oct 2015
Methods Submitted
1/2015 ‐ No Subs
8/2015 ‐ Car01
2/2016 ‐ Car01,
Car02
Screening Team
Review
6/2015
12/2015
2/2016
ERP Review
3/2015 ‐ NA
9/2015 ‐ No OMA
2/2016 ‐ No OMA
What is Next ?
CAROTENOID METHODS
AOAC OMB Meeting Book 36