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The adulteration of food, lessons from the past, with reference to butter, margarine and fraud

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Abstract

The history of food adulteration and fraud and attempts at their control from the Middle Ages to date is traced for Belgium and for the UK with special reference to butter and margarine. The development of analytical procedures for the authentication of milk fat is outlined, from those based on the characterisation of fatty acids derived from milk fat in the nineteenth century to chromatographic methods in the next century and the recent rapid spectroscopic approaches. The importance of adequate surveillance programmes to reduce the incidence of food fraud is stressed.

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Notes

  1. The full title of this specialised journal is Bulletin du service de surveillance de la fabrication and du commerce des Denrées Alimentaires, Compte rendu mensuel des mesures prises par le Gouvernement en exécution de la Loi du 4 août 1890. Published by Administration du Service Santé et de l'Hygiène publique du Ministère de l'Agiculture et des Travaux Publics, Bruxelles.

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Authors and Affiliations

  1. University of Antwerp, Campus Drie Eiken, Universiteitsplein, 2610, Wilrijk, Belgium

    H. Deelstra

  2. School of Chemistry and Chemical Engineering, The Queen’s University of Belfast, Belfast, BT9 5AG, Northern Ireland, UK

    D. Thorburn Burns

  3. Laboratory of the Government Chemist, Queens Road, Teddington, London, TW11 0LY, UK

    M. J. Walker

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  1. H. Deelstra
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Correspondence to D. Thorburn Burns.

Appendices

Appendix 1: Overview of physical and chemical methods characterising edible lipids (fats and oils) mentioned in this paper

Physical methods:

  1. 1.

    Determination of the melting point.

This is the temperature at which fat/butter when heated very slowly becomes completely clear and liquid.

  1. 2.

    Determination of the specific gravity of fat/butter at 100 °C (Method of C. König (37)).

If the butterfat is pure, its specific gravity lies between 0.865 and 0.868.

  1. 3.

    Determination of refractive index with a butter refractometer

This can be done by Abbé refractometer, Zeiss butyrofractometer or refractometer of E.-H., Amagat and F. Jean.

  1. 4.

    Study by microscope of melted fat and the insoluble residue in ether and in alkali

  2. 5.

    Crismer number or critical temperature of dissolution of from butter or margarine fat (turbidity method)

L. Crismer discovered a completely new method for the examination of lipids when he developed the critical temperature of dissolution method. The temperature of fat in alcohol in a tube is increased until transparency of the mixture. After this transparency, the temperature should be dropped till the first discernible turbidity. This temperature is the critical temperature of dissolution. Because the boiling point of alcohol is 78 °C, it was necessary to work with closed tubes. Crismer proved that it was also possible to work with open tubes; however, in that case it was necessary to use nearly absolute alcohol [47, 50]. The values of the critical temperature of dissolution were for butter between 54 and 55 °C and for margarine between 74 and 78 °C.

Chemical methods:

  1. 1.

    The saponification or Köttstorfer number.

Saponification is the process of breaking down a neutral fat into glycerol and fatty acids (as soap) by treatment of the fat with alkali. The saponification or Köttstorfer number is the number of milligrams of KOH required to saponify 1 g of fat under specified conditions. This number is a measure to the average molecular weight of all fatty acids present. The smaller the number, the larger the fatty acid chain length [33].

  1. 2.

    The Hehner number

The Hehner number is the amount of insoluble fatty acids which is obtained from 100 g of fat after saponification and treatment with an acid. For pure butter, the Hehner number varies between 85.4 and 91.3 %, and the average may be taken as 87.5 % [27].

3. The Reichert–Meissl number

The Reichert–Meissl number is the volume of 0.1 N alkali, expressed in ml, which is required to neutralise the volatile and water-soluble fatty acids from 5 g of saponified fat. The Reichert–Meissl number for pure butter is high, because the volatile fats represent the acids soluble in water: butyric and caproic acid, and may vary between 19 and 34, but only in rare instances does fall below 24 [30, 31].

  1. 3.

    The Polenske number

The Polenske number is the volume of 0.1 N alkali in ml, which is required to neutralise the water-insoluble fatty volatile acids distilled from 5 g of saponified fat. The Polenske number in the case of pure butter is low, because the volatile acids insoluble in water include caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid and oleic acid. For pure butter, the Polenske number varies between 1.5 and 3.5 [67].

Hence, the UK standard method referred to as the Reichert, Polenske and Kirschner, RPK, approach depends on the following definitions.

If M is the number of millilitres of 0.1 M aqueous alkali required to neutralise the fatty acids released on saponification and distillation from 5 g fat under the precise conditions specified in the method:

  • The Reichert value, R, is M for the water-soluble volatile fatty acids,

  • The Polenske value, P, is M for the water-insoluble volatile fatty acids, and

  • The Kirschner value, K, is M for water-soluble volatile fatty acids that form water-soluble silver salts.

There are macro (5 g fat) and semi-micro (1 g fat) versions of the RPK procedure, the latter with a scaled down apparatus specified and 0.02 M NaOH or 0.01 M BaOH as titrant [191].

As with all biological products, there is a natural (including species) variation in R, P and K values which are also influenced by season, feeding and the nutritional and health status of the producing animals. Genuine milk fat seldom yields an R of less than 24, known relationships exist between R, P and K and their relative values can give clues as to the nature of any non-milk fat present. Equations have been established from which the percentage of milk fat in a fat sample can be estimated. If the RPK values are in the correct ratio, it is not safe to assume adulteration if they are somewhat low; positive proof of an adulterant should be sought [191].

4. Iodine Number

The iodine number is a measure of degree of unsaturation, which is the number of carbon–carbon double bonds in relation to the amount of fat or oil. The iodine number is defined as the grams of iodine absorbed per 100-g sample [25].

Appendix 2

a. Royal Decree of October 31st 1900 (63) giving details of the Law of May 4th 1900, article 10 (62):

Article 3: Abnormal butter: Prohibition to sell

When in the sample at least two values of the following values are present, the butter should be declared abnormal.

  • A refractive index (Abbe-Zeiss) 40 °C, higher than 1.4565;

  • A critical temperature of dissolution in alcohol (99.1 g/L) higher than 59 °C;

  • A specific gravity at 100 °C lower then 0.864;

  • A value of volatile fatty acids (Meissl) lower than 25;

  • A content of non-volatile fatty acids (Hehner) higher than 89.5 %;

  • A value of saponification (Köttstorfer) lower than 221.

b. Royal Decree of October 20th 1903 (76) giving details of the Law of August 12th 1903, article 11, section C (75):

Article 4: Shall be considered as abnormal butter, if deviating from two of the values of the majority of pure butters, from the following values:

  • A refractive index (Abbe-Zeiss) 40 °C, higher than 1.4565;

  • A critical temperature of dissolution in alcohol (99.1 g/L) higher than 59 °C;

  • A specific gravity at 100 °C lower than 0.864;

  • A value of volatile fatty acids (Meissl) lower than 25;

  • A content of non-volatile fatty acids (Hehner) higher than 9.5 %;

  • A value of saponification (Köttstorfer) lower than 221.

c. Law of November 21st 1904 (78)

Changing article 11, section C of the Royal Decree of October 20th 1903 (76):

Article 2: changing article 4 of the Royal Decree of October 20th 1903 (76): Shall be considered as abnormal butter, when the values which are different for pure butter, an index of fatty volatile and soluble acids (Reichert–Meissl) lower than 28 and one of the other values:

  • A refractive index (Abbe-Zeiss) 40 °C, higher than 1.4552;

  • A critical temperature of dissolution in alcohol (99.1 g/L) higher than 57 °C;

  • A specific gravity at 100 °C lower than 0.865;

  • A content of non-volatile fatty acids (Hehner) higher than 88.5 %;

  • A value of saponification (Köttstorfer) lower than 222.

These abnormal butters are declared illegal to sell.

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Deelstra, H., Burns, D.T. & Walker, M.J. The adulteration of food, lessons from the past, with reference to butter, margarine and fraud. Eur Food Res Technol 239, 725–744 (2014). https://doi.org/10.1007/s00217-014-2274-0

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