stakeholder panel on infant formula & adult nutritionals (spifan)

STAKEHOLDER PANEL ON INFANT FORMULA & ADULT NUTRITIONALS
(SPIFAN)
VITAMIN E WORKING GROUP
DRAFT MEETING MINUTES
Meeting Held At:
Hilton Washington DC/Rockville
Hotel & Executive Meeting Center
1750 Rockville Pike
Rockville, MD 20852
Thursday, June 30, 2011
9:00 AM ‐ 12:00 PM
SPIFAN Chair:
Darryl Sullivan, Covance
Vitamin E Working Group Chair:
Jon DeVries, General Mills/ Medallion Labs
Working Group Participants:
Judith Abadiano, Wyeth Pharmaceuticals Marcus Lipp, U.S. Pharmacopeia
John Austad, Covance Laboratories Carla Meija, U.S. Pharmacopeia
Sneh Bhandari, Silliker, Inc. Brian Murphy, Waters Corp.
Jonathan Beck, Thermo Scientific Michael Norman, Phenomenex
Joe Boison, CFIA Curtis Phinney, American College of Nutrition
Anita Burgher, Pfizer Nutrition Jean Rader, U.S. FDA (CFSAN)
Scott Christiansen, PBM Nutritionals Guenther Raffler, CLF (Danone)
Mark Collison, Archer Daniels Co. Robert Rankin, IFC
Michael Gray, Mead Johnson Nutrition Rama Rengarajan, Kellogg Company
Wesley Jacobs, Abbott Nutrition Kathy Sharpless, NIST
Brendon Gill, Fonterra Matthew Sliva, PBM Nutritionals
Don Gilliland, Abbott Nutrition Joseph Thompson, Abbott Nutrition
Guifeng Jiang, ThermoFisher Scientific Marina Torres‐Rodriguez, LATU
Zoe Grosser, PerkinElmer, Inc. Wayne Wolf, USDA (Retired)
Min Huang, Covance Laboratories Dajin Yang,
Greg Jaudzems, NestléErik Konings, Nestlé Lingsu Zhang, USDA (AMS)
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AOAC Staff:
Delia Boyd
Scott Coates
Jennifer Diatz
Anita Mishra
I. WELCOME AND INTRODUCTIONS
Darryl Sullivan, Chair of the Stakeholder Panel on Infant Formula and Adult Nutrition (SPIFAN), welcomed the
attendees/observers and called the meeting to order. Sullivan called attention to the AOAC policy
documents for antitrust and volunteer conflict of interest. He reviewed meeting materials consisting of the
method books that were signed out to each attendee. Sullivan introduced Jon DeVries, chair of the vitamin E
working group and proceeded with the meeting.
II. REVIEW DRAFT SMPR
DeVries began the working group meeting with the applicability statement as described in the draft SMPR. It
was determined that the applicability statement was the greatest concern. The term “methods maybe able
to” should be added to the applicability statement.
1. Applicability
a. Delete the words “should be” and replace with “that are”
b. At the end of paragraph add “may be desirable”
2. Analytical Technique
a. No change, keep as written
3. Definitions
a. No change, keep as written
4. Method Performance Requirements
a. In footnotes change “μ” to “m”
5. System suitability tests and/or analytical quality control
a. No change, keep as written
6. Reference Material(s):
a. No change, keep as written
7. Validation Guidance:
a. No change, keep as written
8. Maximum Time‐To‐Signal:
a. No change, keep as written
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III. REVISED DRAFT SMPR
DRAFT AOAC SMPR 2011.XXX; Version 5; June 29, 2011
Method Name: Determination of Vitamin E in Infant and Adult/Pediatric Nutritional Formula
Approved by: Stakeholder Panel for Infant Formula and Adult Nutritionals
Final version date:
Effective date:
Intended Use:
1. Applicability:
Determination of vitamin E in all forms of infant, adult, and/or pediatric formula (powders, ready-to-feed liquids, and
liquid concentrates). For the purpose of this SMPR, vitamin E is focused on DL-alpha-tocopherol (CAS-10191-41-
0) and all-racemic-tocopherol (CAS 1406-18-4) and their esters. Other compounds of accepted vitamin E activity
can be included in a method if the requirements of the SMPR are met. Methods that are capable of reporting
alpha-tocopherol and alpha-tocopherol esters separately may be desirable.
2. Analytical Technique:
Any analytical technique that meets the following method performance requirements is acceptable.
3. Definitions:
Adult/Pediatric Formula
Nutritionally complete, specially formulated food, consumed in liquid form, which may constitute the sole
source of nourishment 1 , made from any combination of milk, soy, rice, whey, hydrolyzed protein, starch, and
amino acids, with and without intact protein.
Infant formula
Breast-milk substitute specially manufactured to satisfy, by itself, the nutritional requirements of infants during
the first months of life up to the introduction of appropriate complementary feeding 2 , made from any
combination of milk, soy, rice, whey, hydrolyzed protein, starch, and amino acids, with and without intact
protein.
Limit of Detection (LOD)
The minimum concentration or mass of analyte that can be detected in a given matrix with no greater than 5%
false positive risk and 5% false negative risk.
Limit of Quantitation (LOQ)
The minimum concentration or mass of analyte in a given matrix that can be reported as a quantitative result
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 (SDr); or
% repeatability relative standard deviation (%RSDr).
Reproducibility
The standard deviation or relative standard deviation calculated from among-laboratory data. Expressed as the
reproducibility relative standard deviation (SDR); or % reproducibility relative standard deviation (% RSDR).
Recovery
The fraction or percentage of spiked analyte that is recovered when the test sample is analyzed using the
entire method.
1 AOAC Stakeholders Panel for Infant Formula and Adult Nutritionals (SPIFAN); 2010.
2 Codex Standard 72 – 1981.
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4. Method Performance Requirements:
Analytical range 0.2 - 8*
Limit of Detection (LOD)
Limit of Quantitation
(LOQ)
Repeatability (RSDr)
Recovery Factor
Reproducibility (RSDR)
0.5*
2.0*
4 *
8 *
≤ 0.1*
≤ 0.2*
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≤ 8%
≤ 6%
90% to 110% of mean spiked
recovery over the range of the
assay.
0.5* ≤ 22%
1.0 *
2.0 *
3.0 *
4.0 *
8.0 *
≤ 16%
Concentrations apply to: a) ‘ready-to-feed” liquids “as is”; b) reconstituted
powders (25 g into 200 g of water); and c) liquid
concentrates diluted 1:1 by weight.
* mg /100 g reconstituted final product.
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.
6. Reference Method(s): AOAC Official Methods of Analysis SM 992.03, Vitamin E Activity (All-rac-alpha-Tpcopherol)
in Milk-Based Infant Formula may be used with the following caveat: OMA 992.03 has been validated for milkbased
formula only.
7. Reference Material(s): NIST Standard Reference Material ® 1849; Infant/Adult Nutritional Formula - or equivalent.
The SRM is a milk-based, hybrid infant/adult nutritional powder prepared by a manufacturer of infant formula and
adult nutritional products. A unit of SRM 1849 consists of 10 packets, each containing approximately 10 g of
material. NIST 1849 assigned the following values for vitamin E vitamers: 369 ± 16 mg/Kg of alpha-tocopherol;
189 ± 13 mg/Kg of gamma-tocopherol; 79 ± 2.4 mg/Kg of delta-tocopherol; and 5.77 ± 0.79 mg/Kg of betatocopherol.
8. Validation Guidance:
Recommended level of validation: Official Methods of Analysis SM
9. Maximum Time-To-Signal: No maximum time.
IV. REVIEW OF METHODS
a. Proposed methods (see Table 1)
b. The working group recommended the following candidate methods along with potential study
directors (see Table 2).

Table 1‐ Proposed Methods
VITAMIN A METHODS
File No. MANUSCRIPT TITLE AND
PUBLICATION INFORMATION
VITA‐01 Vitamins A and E by UPLC‐UV or
FLD submitted by Campos‐
Gimenez
VITA‐02 Immunoassay Method for
Determination of Vitamin A in
Infant Formula Submitted by:
SciMed Technologies Inc.
VITA‐03 Off‐line coupling of pressurized
liquid extraction and LC/ED for the
determination of retinyl acetate
and tocopherol in infant formula
Delgado‐Aamarreno, Bustamante‐
Rangel, M, Garcia‐Jimenez, M.
Sanchez‐Perez, A, & Carabias‐
Martinez, R. (2006) Talanta 70,
1094‐1099
VITA‐04 Simultaneous analysis of Vitamins
A and E in infant milk‐based
formulae by normal phase HPLC
DAD using a short narrow‐bore
column Chavez‐Servin, JL,
Castellote, AI, Lopez‐Sabater, MC
(2006) J. Chormatogr A 1122, 138‐
143
VITA‐05 Rapid determination by reversed‐
phase HPLC of Vitamins A and E in
infant formulas Rodas Mendoza,
B., Morera Pons, S, Castellote
Bargallo, AI, & Lopez‐Sabater, MC
(2003) J Chromatogr A 1018, 197‐
202
VITA‐06 Development of methods for the
determination of vitamins A, E and
beta‐carotene in processed foods
based on supercritical fluid
extraction: a collaborative study
Mathiasson, L, Turner, C., Berg, H.,
Dahlberg, L., Theobald, A., Anklam,
E., Ginn, R., Sharman, M., Ulberth,
F., & Gabernig, R. (2002) Food Add
& Cont. 19(7) 632‐646
VITA‐07 Interlaboratory verified liquid
chromatographic method for
analysis of Vitamins A and E in Soy
Based Infant Formula Powder
Chase, WG, Ye, L, Stoakes, VC,
Eitenmiller, RR, & Long, AR (2004)
87(6) 1329‐1333
Source Comments method description Rank*
CALL FOR
METHODS
CALL FOR
METHODS
CHAIR
RECOMMEND
CHAIR
RECOMMEND
CHAIR
RECOMMEND
CHAIR
RECOMMEND
CHAIR
RECOMMEND
Well written, recently
developed method. Request
data. Undated: current.
Some repeatability data
(misidentified as
reproducibility) for IF. Good
% CV. Not sure if method can
detect at proposed LOQ.
Undated: current.
Some recovery data for
retinyl acetate in IF. 2006
Good LOQ; recovery; and
precision data. 2006
Precision. sensitivity,
linearity, and recovery data
for IF. 2003
Precision, reproducibility, and
recovery data for IF. 2002
Alcoholic saponifcation; SPE 3
w/ diatomaceous earth;
evaporation; HILIC‐UPCL or
UV
ELISA 2
Methanol extraction;
pressurize liquid extraction
(PLE); saponification with
KOH; liquid chromatography.
Ethanol extraction, hexane
re‐extraction; HPLC‐diode
array (DAD).
Ethanol extraction, hexane
re‐extraction; reverse‐phase
HPLC; photo diode array.
Ethanol saponification;
supercritical fluid extraction;;
HPLC; UV or fluorescence
detection
Recovery data for IF. 2004 Dehydration w/ MgSO 4;
extracted w/ isopropanol and
hexane‐ethyl acetate;
evaporated, filtered; LC; with
fluorescence detector.
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VITA‐08 An interlaboratory‐verified
method for the determination of
vitamins A and E in milk‐ and soy‐
based infant formula by LC with
matrix solid phase dispersion
extraction
Chase, WG, Ye, L, Stoakes, VC,
Eitenmiller, RR, & Long, AR (2004) J
AOAC Int. 87(5) 1173‐1178
VITA‐09 Determination of Vitamins A
(retinol) and E (alpha‐tocopherol in
foods by liquid chromatography:
collaborative study
VITA‐10 Foodstuffs – Determination of
vitamin A by high performance
liquid chromatography Part 1:
Measurement of all‐trans‐retinol
and 13‐cis‐retinol Submitted by:
Güenther Raffler
VITA‐11 Foodstuffs – Determination of
vitamin A by high performance
liquid chromatography Part 2:
Measurement of ß‐carotene
Submitted by: Guenther Raffler
VITA‐12 Simultaneous Determination of 13‐
CIS and All‐Trans Vitamin A
Palmitate and Alpha Vitamin E
Acetate by HPLC and Column
Switching: Submitted by Abbott
VITA‐13 Determination of Vitamin A in
Infant/Adult Formula by HPLC‐
Isotope Dilution Mass
Spectrometry
VITA‐14 Determination of Vitamins A
(Retinol) and E (alpha‐Tocopherol)
in foods by LC: Collaborative Study
2001.13
VITA‐15 Determination of Vitamin A
(retinol, vitamin E (tocopherol),
and B‐carotene in food stuff by
HPLC‐UV
CHAIR
RECOMMEND
CHAIR
RECOMMEND
CALL FOR
METHODS
CALL FOR
METHODS
CALL FOR
METHODS
CHAIR
RECOMMEND
SMPR
Table 2 ‐ Candidate Methods Recommended by Working Group
Recovery data for IF. 2004 Matrix solid‐phase
dispersion; evaporation;
filtration; normal‐phase LC ;
fluorescent detector.
Recovery data for IF. Use of
ZCM. 2002
No data on IF. Precision and
Reproducibility data for
butter and milk powder.
2000
For β‐carotene; SPIFAN WG
decided not to include β‐
carotene in its scope. 2000
Good precision and recovery
data for IF.
Uncertainty, expanded
uncertainty, and trueness
data using NIST 1849.
LOD, accuracy, and expanded
uncertainty, trueness data.
Some IF data.
Saponification w/ ethanol‐
water; LC; UV detector.
Saponification by alcoholic
KOH; extraction w/ diethyl
ether; HPLC; UV or
fluorescent detector.
Saponification by alcoholic
KOH; extraction w/ diethyl
ether or acetonitrile; HPLC;.
Methanol extraction;
centrifugal separation; HPLC
w/UV detector.
Saponification w/pyrogallol
and KOH; extraction w/
petroleum ether; filtered
through Na SO4; HPLC ‐
isotope dilution mass spec
[HPLC‐IDMS].
Saponification w/ KOH;
extraction w/ petroleum
ether; HPLC ‐ UV/VIS
File No. Manuscript Title & Publication Information Working Group Comments
VITE‐01 Vitamins A and E by UPLC‐UV or FLD submitted by Campos‐
Gimenez
VITE‐09 Determination of Vitamins A (retinol) and E (alpha‐tocopherol in
foods by liquid chromatography: collaborative study
Well written, recently developed method. Request data.
Undated: current.
Recovery data for IF. Use of ZCM. 2002
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VITE‐12 Simultaneous Determination of 13‐CIS and All‐Trans Vitamin A
Palmitate and Alpha Vitamin E Acetate by HPLC and Column
Switching: Submitted by Abbott
VITE‐15 Determination of Vitamin A (retinol, vitamin E (tocopherol), and
B‐carotene in food stuff by HPLC‐UV
Good precision and recovery data for IF.
LOD, accuracy, and expanded uncertainty, trueness data.
Some IF data.
No study director was identified during meeting
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