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The Japan Food Chemical Research Foundation
Approval of New High-Intensity Sweetner : Sucralose
Last updateF11/30/2006

Revision of the Enforcement Regulations under the Food Sanitation Law and of the Standards and Specifications for Food and Food Additives, etc.*
(published in Official Gazette, No. 2678, July 30, 1999)

July 30, 1999

The Ministry of Health and Welfare has revised the Enforcement Regulations(Ministry of Health and Welfare Ordinance No.23, 1948), based on Article 6 and Article 11, Paragraph 1 of the Food Sanitation Law (Law No. 233, 1947), and the Standards and Specifications for Food and Food Additives, etc. (Ministry of Health and Welfare Announcement No. 370, December 1959), based on Article7-1 of the Food Sanitation Law. These revisions have been based on Ministry of Health and Welfare Ordinance No. 75(Ministerial Ordinance to revise part of the Enforcement Regulations under the Food Sanitation Law) and Ministry of Health and Welfare Announcement No. 167, which were published in Official Gazette, No. 2678, July 30, 1999.

Revision of the Enforcement Regulations

The substance given below has been added in a list of the additives designated as approved by Minister of Health and Welfare,( Table 2 under Article 3 of the Ministerial Ordinance.)
Supplementary provision
This revision has come into effect on the date of publication.

Revision of the Standards and Specifications for Food and Food Additives, etc.

The specifications and standards for components and standards for use, given below, have been added in the specifications and standards for food and food additives based on Paragraph 7-1 and Paragraph 10.



Sucralose
Trichlorogalactosucrose

C12H19Cl3O8 Mol. Wt. 397.64
1,6-dichloro-1,6-dideoxy-beta-D-fructofuranosyl-4-chloro-4-deoxy-alpha-D-galactopyranoside
[56038-13-2]

Content Sucralose, when calculated on the anhydrous basis, contains 98.0 - 102.0 % of Sucralose (C12H19Cl3O8).

Description Sucralose occurs as a white to off-white crystalline powder. It is odorless and has a sweet taste. It is freely soluble in water, in methanol, and in ethanol and slightly soluble in ethyl acetate.

Identification Tests (1) Determine the infrated absorption spectrum of Sucralose as directed in the Potassium Bromide Disk Method under the Infrated Spectrophotometry and compare the obtained spectrum with the Reference Spectrum of Sucralose. Both spectra exhibit similar intensities of absorption at the same wave numbers.
(2) Dissolve 1.0g of Sucralose in 10ml of methanol, and used this solution as the test solution. Perform Thin-Layer Chromatography on 5” l of the test solution, using a sodium chloride solution (dissolve 1g in a solvent to make 20ml)-acetnitrile mixture (7:3) as the developing solvent. The Rf value of the spot is from 0.4 to 0.6. For the thin layer plate, use octadecylsilanized silica gel for thin-layer chromatography. Stop the development when the development solvent rises 15 cm, air-dry, remove the solvent, spray with the 15 % Sulfuric acid-methanol TS, and heat at 125 °C for 10 minutes to develop the color.

Purity Tests (1) Clarity of solution Clear (1.0g, water 10ml)
(2) Specific rotation
(3) pH 3.0 - 6.0 (2.0 g, water 20 ml)
(4) Heavy metals Not more than 10 m g/g as Pb. (1.0 g, Method 2, Control solution Lead Standard Solution 1.0ml)
(5) Arsenic Not more than 4.0 mg/g as As2O3.(0.50g, Method 2, Apparatus B)
(6) Other chlorinated disaccharides Not more than 0.5%
Test solution Dissolve 1.0 g of Sucralose in 10 ml of methanol.
Control solution Measure 0.5 ml of Test solution, add methanol to make 100 ml.
Procedure Perform Thin-Layer Chromatography on 5ml each of Test solution and Control solution, conduct TLC assay of Identification Test (2). The spot in the Test Solution has no other spot which is more intense than the spot in Control solution.
(7) Chlorinated monosaccharide Not more than 0.16 % as fructose
Test solution Weigh 2.5 g of Sucralose, add methanol to make exactly 10 ml.
Control solution A Weigh exactly 10.0 g of mannitol, add water to make exactly 100 ml.
Control solution B Weigh exactly 10.0 g of mannitol and 40 mg of fructose, add water to make exactly 100 ml.
Procedure Apply 1 ml of each of Test solutions, Control solution A and B onto the thin-layer chromatography plate coated with a 0.25 mm thickness of silica gel, air-dry, and repeat this procedure four times. Splay the p-anisidine-phthalic acid TS, and heat at 98 - 102 °C for about 10 minutes to develop the color. The spot from the Test Solution is not more colored than the spot from Control solution B. When the mannitol spot from Control Solution A represent, a second plate should be prepared, and repeat these procedure.
(8) Triphenylphosphine oxide Not more than 150 mg/g
Test solution Weigh accurately about 100 mg of Sucralose, dissolve a mixture of acetnitril-water(67:33) to make exactly 10 ml.
Standard solution Weigh exactly 100 mg of triphenylphosphine oxide, dissolve a mixture of acetnitril-water(67:33) to make exactly 10 ml. Measure exactly 1 ml of the resulting solution and add a mixture of acetnitril-water(67:33) to make exactly 100 ml. Measure exactly 1 ml of the resulting solution and add a mixture of acetnitril-water(67:33) to make exactly 100 ml.
Procedure Perform Liquid Chromatography on 25 ml each of the Test solution and Standard solution under the conditions given below. Record the mean peak areas for the Standard and Test Solutions as As and At respectively. Calculate the concentration of triphenylphosphine oxide (TPPO) in Sucralose from the following formula.

Operating Conditions
Detector : Ultraviolet range absorption detector (measurement wavelength : 220 nm)
Column packing material :5mm octadecylsilanized silica gel.
Column tube :Stainless steel tube (length : 15 cm, internal diameter : 4.6 mm)
Column temperature :40°C
Mobile phase :acetonitrile - water (67:33)
Flow rate :1.5 ml/min.
(9) Methanol Not more than 0.1%
Test solution Weigh accurately about 2.0 g of Sucralose, add water to make exactly 10 ml, and mix.
Control solution Measure exactly 2 ml of methanol, add water to make exactly 100 ml, and mix. Measure exactly 1 ml of this solution, add water to make exactly 100 ml, and mix.
Procedure Measure each 1ml of Test solution and Control solution, and perform Gas Chromatography under the operating conditions given below. Measure the peak area of each solution, calculate SA and AS, and calculated the content by the following formula:
CS is the concentration of methanol in the Control solution in percent.
Operating conditions
Detector : Hydrogen flame ionization detector.
Column packing material : 150 ~ 180mm porous polymer for gas chromatography
Column tube : Glass tube (length : about 2 m, internal diameter : 2-4 mm)
Column temperature : Constant temperature of 140 - 160 °C
Inlet temperature : 200°C
Detector temperature : 250°C
Carrier gas and flow rate : Use nitrogen or helium. Adjust the flow rate so that the retention time of methanol is about 4 minutes.

Residue in Ignition Not more than 0.7%

Water Not more than 2.0% (1 g, direct titration).

Assay Weigh accurately about 1g of Sucralose, and dissolve in water to make exactly 100 ml. Measure exactly 10 ml of this solution, added 10 ml of sodium hydroxide solution (dissolved 1g in a solvent to make 10ml). Equip with reflex condenser, and gently heat for 30 minutes. Cool and neutralize with dilute nitric acid, and titrate with 0.1mol/l silver nitrate. The end point is usually confirmed by using a potentiometer (Indicator electrode : Silver electrode, expect that for silver-silver chloride electrode as reference electrode is used.) Perform a blank test in the same manner, and make any necessary correction and calculate on the dry basis.





Standards for use of sucralose
Additives
Major use
Standards for use
Foods
Maximum Limit of use
Limitation of use
Sucralose Sweetener Confections
1.8g/kg
The maximum limits do not apply to foods approved to be labeled as "special dietary use."
Chewing gum
2.6g/kg
Jam
1.0g/kg
Lactic acid bacteria drinks
0.40g/kg

(Applied to dilutions to the case of concentrated products)
Milk drinks
Miscellaneous alcoholic beverages
Nonalcoholic beverages
"Sake"(rice wine)
"Sake"(compounded)
Wine
Substitute for Sugar
12g/kg
Other foods
0.58g/kg

Note: This translation is an outline of Ministry of Health and Welfare Ordinance No.75 (Ministerial Ordinance to revise part of the Enforcement Regulations under the Food Sanitation Law) and Ministry of Health and Welfare Announcement No. 167. This is translated by The San-Ei Gen Foundation for Food Chemical Research. If there is any discrepancy in this document, please refer to the Official Gazette in Japanese, No. 2678, July 30, 1999.