Simultaneous Determination of 13-cis and all-trans Vitamin A Palmitate (Retinyl Palmitate), Vitamin A Acetate (Retinyl Acetate), and Total Vitamin E (α-Tocopherol and DL-α-Tocopherol Acetate) in Infant Formula and Adult Nutritionals by Normal Phase HPLC: First Action 2012.10

2013 ◽  
Vol 96 (5) ◽  
pp. 1073-1081 ◽  
Author(s):  
Adrienne McMahon ◽  
Scott Christiansen ◽  
Lynsey Shine ◽  
Calvin Loi ◽  
Dawn Dowell
Keyword(s):  
Vitamin E ◽  
Vitamin A ◽  
Simultaneous Determination ◽  
Infant Formula ◽  
Normal Phase ◽  
Total Vitamin ◽  
Validation Data ◽  
Tocopherol Acetate ◽  
Selection Of

Abstract This HPLC method, with both variable UV and fluorescence detection, allows for the simultaneous determination of vitamin A palmitate, vitamin A acetate, and total vitamin E in infant, pediatric, and adult nutritional formulas. The concentration of each vitamin form is calculated by comparison with standards of known concentration. Following hydrolysis, the vitamins are extracted into iso-octane and analyzed by normal phase (NP) HPLC. The method was evaluated for linearity, precision, and accuracy using a selection of the Stakeholder Panel on Infant Formula and Adult Nutritionals (SPIFAN) matrixes, including milk-based, soy-based, and hydrolyzed protein, as well as high- and low-fat products. A single-laboratory validation has been completed for all analytes using a selection of SPIFAN matrixes. Performance parameters included a working range of 2–450 μg/100 g ready-to-feed for vitamin A and 0.03–8.0 mg/100 g reconstituted final product for vitamin E. LOD was <1.0 μg and <0.1 mg/100 g reconstituted final product for vitamins A and E, respectively; RSD was 1.08–8.70% over a range of concentration; and average recoveries of 97.4–101.3%. Repeatability of <4% for vitamin A and <8% for vitamin E was calculated from five laboratories using this method. Results indicate that this method is suitable for the analysis of vitamins A and E in all forms of infant, adult, and pediatric formulas (powders, ready-to-feed liquids, and liquid concentrates). The Expert Review Panel (ERP) of Infant Formula reviewed this method separately for vitamins A and E, including all available method validation data at the AOAC INTERNATIONAL Annual Meeting on September 29, 2012. Following evaluation of the data for both methods, the ERP agreed that both methods met the standard method performance requirements articulated by SPIFAN. The ERP granted First Action status to both methods, and recommended that a single method be published for the simultaneous determination of vitamin A palmitate, vitamin A acetate, and total vitamin E (DL-α-tocopherol and DL-α-tocopherol acetate) in infant formula and adult nutritionals by NP HPLC.

Determination of Vitamin E and Vitamin A in Infant Formula and Adult Nutritionals by Normal-Phase High-Performance Liquid Chromatography: Collaborative Study, Final Action 2012.10

2016 ◽  
Vol 99 (1) ◽  
pp. 223-241 ◽  
Author(s):  
Adrienne McMahon ◽  
S Christiansen ◽  
F-F Chee ◽  
A Chua ◽  
H Braddock ◽  
...  
Keyword(s):  
Vitamin E ◽  
Vitamin A ◽  
Infant Formula ◽  
Collaborative Study ◽  
Retinyl Palmitate ◽  
Normal Phase ◽  
Retinyl Acetate ◽  
Total Vitamin ◽  
Normal Phase Hplc

Abstract The main objective of the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals (SPIFAN) project is to establish international consensus methods for infant formula and adult nutritionals, which will benefit intermarket supply and dispute resolution. A collaborative study was conducted on AOAC First Action Method 2012.10 Simultaneous Determination of 13-cis and All-trans Vitamin A Palmitate (Retinyl Palmitate), Vitamin A Acetate (Retinyl Acetate), and Total Vitamin E (α-Tocopherol and D-α-tocopherol acetate) in Infant Formula and Adult Nutritionals by Normal-Phase HPLC. Fifteen laboratories from 11 countries participated in an interlaboratory study to determine 13-cis and all-trans vitamin A palmitate (retinyl palmitate), vitamin A acetate (retinyl acetate), and total vitamin E (α-tocopherol and D-α-tocopherol acetate) in infant formula and adult nutritionals by normal-phase HPLC and all laboratories returned valid data. Eighteen test portions of nine blind duplicates of a variety of infant formula and adult nutritional products were used in the study. The matrixes included milk-based and soy-based hydrolyzed protein as well as a low fat product. Each of the samples was prepared fresh and analyzed in singlicate. As the number of samples exceeded the recommended number to be prepared in a single day, analysis took place over 2 days running 12 samples on day one and 10 samples on day two. The reference standard stock was prepared once and the six-point curve diluted freshly on each day. Results obtained from all 15 laboratories are reported. The RSDR for total vitamin A (palmitate or acetate) ranged from 6.51 to 22.61% and HorRat values ranged from 0.33 to 1.25. The RSDR for total vitamin E (as tocopherol equivalents) ranged from 3.84 to 10.78% and HorRat values ranged from 0.27 to 1.04. Except for an adult low fat matrix which generated reproducibility RSD >40% for some isomers, most SPIFAN matrixes gave results within the acceptance criteria of <16% RSD as stated in the respective Standard Method Performance Requirements.

Determination of Vitamins A and E in Infant Formula and Adult/Pediatric Nutritional Formula by HPLC with UV and Fluorescence Detection: First Action 2012.09

2013 ◽  
Vol 96 (6) ◽  
pp. 1407-1413 ◽  
Author(s):  
Linda Butler Thompson ◽  
Karen Schimpf ◽  
Steve Baugh
Keyword(s):  
Vitamin E ◽  
Vitamin A ◽  
Infant Formula ◽  
Methylene Chloride ◽  
Lipid Fraction ◽  
Intermediate Precision ◽  
Silica Column ◽  
Vitamin E Acetate ◽  
Uv And Fluorescence Detection

Abstract The method presented is for quantification of α-tocopherol (vitamin E), vitamin E acetate, vitamin A acetate, and vitamin A palmitate in infant formula and adult/pediatric nutritionals. The entire lipid fraction, including vitamins A and E, is extracted from product with iso-octane after products are mixed with methanol, which precipitates proteins and disrupts micelles freeing lipids for extraction. Vitamin A palmitate, vitamin A acetate, and vitamin E acetate are separated from α-tocopherol on a 3 cm silica column with a 1% methylene chloride, 0.06% isopropanol in iso-octane mobile phase; eluted onto a 20 cm silica column; and, after a column switch, further separated on the 20 cm column before UV detection at 325 nm (vitamin A palmitate and vitamin A acetate) and 285 nm (vitamin E acetate). α-Tocopherol is further separated from other extraneous compounds on the 3 cm silica column and detected by fluorescence at excitation and emission wavelengths of 295 and 330 nm, respectively. Quantification limits in ready-to-feed products were estimated to be 80 IU/L for vitamin A palmitate, 207 International Units (IU)/L for vitamin A acetate, 2.4 mg/L for vitamin E acetate, and <0.15 mg/L for α-tocopherol. Over-spike recoveries and intermediate precision averaged 100.4 and 2.09% RSD for vitamin A palmitate, 100.4 and 1.52% RSD for vitamin E acetate, and 99.6 and 3.02% RSD for α-tocopherol. Vitamin A acetate spike recovery data averaged 96.6%, and the intermediate precision for the only product fortified with vitamin A acetate was 2.75% RSD.

Determination of Vitamin A (Retinol) in Infant Formula and Adult Nutritionals by Liquid Chromatography: First Action 2011.15

2012 ◽  
Vol 95 (2) ◽  
pp. 322-328
Author(s):  
Jonathan W DeVries ◽  
Karlene R Silvera ◽  
Elliot McSherry ◽  
Dawn Dowell
Keyword(s):  
Liquid Chromatography ◽  
Vitamin A ◽  
Infant Formula ◽  
Collaborative Study ◽  
Alpha Tocopherol ◽  
Powdered Infant Formula ◽  
Food Matrix ◽  
Validation Data ◽  
Method Performance

Abstract During the “Standards Development and International Harmonization: AOAC INTERNATIONAL Mid- Year Meeting,” held on June 29, 2011, an Expert Review Panel (ERP) reviewed the method for the “Determination of Vitamins A (Retinol) and E (alpha-Tocopherol) in Foods by Liquid Chromatography: Collaborative Study,” published by Jonathan W. DeVries and Karlene R. Silvera in J. AOAC Int. in 2002. After evaluation of the original validation data, an ERP agreed in June 2011 that the method meets standard method performance requirements (SMPRs) for vitamin A, as articulated by the Stakeholder Panel on Infant Formula and Adult Nutritionals. The ERP granted the method First Action status, applicable to determining vitamin A in ready-to-eat infant and adult nutritional formula. In an effort to achieve Final Action status, it was recommended that additional information be generated for different types of infant and adult nutritional formula matrixes at varied concentration levels as indicated in the vitamin A (retinol) SMPR. Existing AOAC LC methods are suited for specific vitamin A analytical applications. The original method differs from existing methods in that it can be used to assay samples in all nine sectors of the food matrix. One sector of the food matrix was powdered infant formula and gave support for the First Action approval for vitamin A in infant and adult nutritional formula. In this method, standards and test samples are saponified in basic ethanol–water solution, neutralized, and diluted, converting fats to fatty acids and retinol esters to retinol. Retinol is quantitated by an LC method, using UV detection at 313 or 328 nm for retinol. Vitamin concentration is calculated by comparison of the peak heights or peak areas of retinol in test samples with those of standards.

Simultaneous determination of eight vitamin E isomers and α-tocopherol acetate in functional foods and nutritional supplements by gas chromatography – mass spectrometry

2015 ◽  
Vol 7 (8) ◽  
pp. 3353-3362 ◽  
Author(s):  
Dan Lu ◽  
Yi Yang ◽  
Xin Wu ◽  
Li Zeng ◽  
Yongxin Li ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Vitamin E ◽  
Simultaneous Determination ◽  
Functional Foods ◽  
Nutritional Supplements ◽  
Gas Chromatography Mass Spectrometry ◽  
Tocopherol Acetate ◽  
Chromatography Mass Spectrometry

A gas chromatography-mass spectrometry (GC-MS) has been developed for the simultaneous determination of eight VE isomers and α-tocopherol acetate in functional foods.

scholarly journals Simultaneous Determination of Vitamin A and E in Infant Formula by HPLC with Photodiode Array Detection

2011 ◽  
Vol 31 (2) ◽  
pp. 191-199 ◽  
Author(s):  
Hong-Min Lee ◽  
Byung-Man Kwak ◽  
Jang-Hyuk Ahn ◽  
Seung-Hwan Jeong ◽  
Sung-Lye Shim ◽  
...  
Keyword(s):  
Vitamin A ◽  
Simultaneous Determination ◽  
Infant Formula ◽  
Photodiode Array Detection ◽  
Photodiode Array ◽  
Array Detection
Sign in / Sign up

Export Citation Format

Share Document