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Additive 467 m1

This document provides information on the specifications for dl-α-tocopherol, including its chemical and physical properties, functional uses, characteristics, identification tests, purity standards, and assay method. It establishes a group acceptable daily intake (ADI) of 0.15-2 mg/kg body weight for dl-α-tocopherol and defines it as a slightly yellow to amber, nearly odorless, viscous oil that functions as an antioxidant. The document also describes gas chromatography as the method for assaying dl-α-tocopherol content using an internal standard.

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59 views3 pages

Additive 467 m1

This document provides information on the specifications for dl-α-tocopherol, including its chemical and physical properties, functional uses, characteristics, identification tests, purity standards, and assay method. It establishes a group acceptable daily intake (ADI) of 0.15-2 mg/kg body weight for dl-α-tocopherol and defines it as a slightly yellow to amber, nearly odorless, viscous oil that functions as an antioxidant. The document also describes gas chromatography as the method for assaying dl-α-tocopherol content using an internal standard.

Uploaded by

LMNAVA
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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dl- α -TOCOPHEROL

Prepared at the 30th JECFA (1986), published in FNP 37 (1986) and in


FNP 52 (1992). Metals and arsenic specifications revised at the 61st
JECFA (2003). A group ADI of 0.15-2 mg/kg bw for dl-α-tocopherol and d-
α-tocopherol, concentrate, singly or in combination, was established at the
30th JECFA (1986).

SYNONYMS Vitamin E; INS No. 307c

DEFINITION

Chemical names dl-5,7,8-Trimethyltocol, dl-2,5,7,8-tetramethyl-2-(4',8',12'- trimethyltridecyl)-


6-chromanol

C.A.S. number No single definite C.A.S. number is for this substance. No. 59-02-9 is for
vitamin E, 1406-18-4 is for alpha-tocopherol, 2074-53-5 is for all-rac-alpha-
tocopherol, and 10191-40-0 is for racemic-alpha-tocopherol synthesized
from natural phytol or its derivative.

Chemical formula C29H50O2

Structural formula

Formula weight 430.71

Assay Not less than 96% and not more than 102%

DESCRIPTION Slightly yellow to amber, nearly odourless, clear, viscous oil (It oxidizes and
darkens in air and on exposure to light.)

FUNCTIONAL USES Antioxidant

CHARACTERISTICS

IDENTIFICATION

Solubility (Vol. 4) Insoluble in water, freely soluble in ethanol, miscible with ether

Specific rotation (Vol. 4) [alpha] 20, D: 0±0.05o (1 in 10 soln in chloroform)

Spectrophotometry In absolute ethanol the maximum absorption is about 292 nm


(Vol. 4)
Colour reaction Dissolve about 0.01 g of the sample in 10 ml of absolute ethanol. Add, with
swirling, 2 ml of nitric acid and heat at about 75o for 15 min. A bright red to
orange colour develops

PURITY

Refractive index n (20, D): 1.503 - 1.507

Spectrophotometry E (1%, 1 cm) (292 nm): 71-76 (0.01 g in 200 ml of absolute ethanol)
(Vol. 4)

Sulfated ash (Vol. 4) Not more than 0.1%


Test 1 g of the sample (Method II)

Acidity Dissolve 1 g of the sample in 25 ml of a mixture of equal volumes of


ethanol and ether that has been neutralized to phenolphthalein TS with 0.1
N sodium hydroxide, add 0.5 ml of phenolphthalein TS, and titrate with 0.1
N sodium hydroxide until the solution remains faintly pink after shaking for
30 sec. Not more than 1.0 ml of 0.1 N sodium hydroxide is required.

Lead (Vol. 4) Not more than 2 mg/kg


Determine using an atomic absorption technique appropriate to the
specified level. The selection of sample size and method of sample
preparation may be based on the principles of the method described in
Volume 4, “Instrumental Methods.”

METHOD OF Gas Liquid Chromatographic Method


ASSAY
Reagents and solutions
Internal Standard Solution: Prepare a solution in n-hexane containing a 3
mg of hexadecyl hexadecanoate, accurately weighed, in each ml.
Standard Preparation: dissolve about 30 mg of USP Alpha Tocopherol
Reference Standard, accurately weighed, in 10.0 ml of the Internal
Standard Solution.

Assay Preparation: dissolve about 30 g of the sample accurately weighed,


in 10.0 ml of the International Standard Solution.

Chromatographic System
Use a gas chromatograph equipped with a flame-ionization detector and a
glass-lined sample- introduction system or on-column injection. Under
typical conditions, the instrument contains a 2-m x 4-mm boro-silicate glass
column packed with 2% methylpolysiloxane gum on 80- to 100-mesh acid-
base washed silinized chromatographic diatomaceous earth. The column is
maintained isothermally between 240o and 260o, the injection port at about
290o, and the detector block at about 300o. The flow rate of dry carrier gas
is adjusted to obtain a hexadecyl hexadecanoate peak approximately 18 to
20 min after sample introduction when a 2% column is used, or 30 to 32
min when a 5% column is used. (NOTE: Cure and condition the column as
necessary).
System Suitability
Chromatograph a sufficient number of injections of a mixture in n-hexane of
1 mg per ml each of USP Alpha Tocopherol Reference Standard and USP
Alpha Tocopheryl Acetate Reference Standard, as directed under
Calibration, to assure that the resolution factor, R, is not less than 1.0.

Calibration
Chromatograph successive 2- to 5-µl portions of the Standard Preparation
until the relative response factor, F, is constant (i.e., within a range of
approximately 2%) for three consecutive injections. If graphic integration is
used, adjust the instrument to obtain at least 70% maximum recorder
response for the hexadecyl hexadecanoate peak. Measure the areas under
the major peaks occurring at relative retention times of approximately 0.51
(alpha-tocopherol) and 1.00 (hexadecyl hexadecanoate), and record the
values as As and A1, respectively. Calculate the relative response factor, F,
by the formula (As/A1) x (C1/Cs), in which C1 and Cs are the exact
concentrations, in mg per ml, of hexadecyl hexadecanoate and of USP
Alpha Tocopherol Reference Standard in the Standard Preparation,
respectively.

Procedure
Inject a suitable portion (2 to 5 µl) of the Assay Preparation into the
chromatograph, and record the chromatogram. Measure the areas under
the major peaks occurring at relative retention times of approximately 0.51
(alpha-tocopherol) and 1.00 (hexadecyl hexadecanoate), and record the
values as au and a1, respectively.

Calculate the weight, in mg, of dl-alpha-tocopherol in the sample by the


formula (10C1/F) x (au/a1).

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