2016 OMB Summer Meeting

AOAC OMB Meeting Book

36

CAROTENOID METHODS 

Methods Submitted 1/2015 ‐ No Subs

Screening Team  Review 6/2015 12/2015 2/2016

Call for Methods Sept 2014 April 2015 Oct 2015

ERP Review 3/2015 ‐ NA

WG launched March 2014

SMPR Approved Sept 2014

What is Next ?

8/2015 ‐ Car01 2/2016 ‐ Car01,  Car02

9/2015 ‐ No OMA 2/2016 ‐ No OMA

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 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 

Method uses sound methodology  

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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 

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 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