Analysis of Preservatives in Accordance with “Analysis Method of Food Additives in Foods” in Japan (C18M 4E)

Analysis of food additives in foods notified by the Japanese Ministry of Health, Labor and Welfare has a section for “benzoic acid, sorbic acid and their salts, and sodium dehydroacetate'” analysis. It uses an analytical column packed with octadecylsilylated silica gel (ODS column) packed in a 4.6-mm inner diameter and 50- to 250-mm length column. In this application, we analyzed nine preservatives using an ODS column, Silica C18M 4E. All preservatives analyzed were separated well. The detection was performed at two wavelengths: 230 nm and 260 nm.

Reference: Revision of the "Analysis Law for Food Additives in Foods" (Pharmaceuticals and Foods and Foods Regulations No. 0624 No. 1 dated June 24, 2021, and Pharmaceuticals and Foods and Drug Administration No. 0624 No. 1 dated June 24, 2021)" (Attachment 3)

Sample: 20 μL, 5 μg/mL each (in CH3OH/H2O=60/40)

  1. 1.Benzoic acid
  2. 2.Sorbic acid
  3. 3.Dehydroacetic acid
  4. 4.Methyl p-hydroxybenzoate
  5. 5.Ethyl p-hydroxybenzoate
  6. 6.Isopropyl p-hydroxybenzoate
  7. 7.Propyl p-hydroxybenzoate
  8. 8.Isobutyl p-hydroxybenzoate
  9. 9.Butyl p-hydroxybenzoate
chromatogram of preservatives
Column
Shodex Silica C18M 4E (4.6 mm I.D. x 250 mm)
Eluent
A); 5 mM Citrate buffer (pH4.0)/CH3CN/CH3OH=7/2/1
B); 5 mM Citrate buffer (pH4.0)/CH3CN/CH3OH=4/2/4
Linear gradient (High pressure);
(B%) 0 % (0 to 12 min), 0 % to 72 % (12 to 18 min), 72 % to 100 % (18 to 25 min), 100 % (25 to 31 min), 100 % to 0 % (31 to 32 min), 0 % (32 to 42 min)
Flow rate
1.0 mL/min
Detector
UV (230 nm, 260 nm)
Column temp.
40 ℃

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