NF EN ISO 17678

NF EN ISO 17678

April 2010
Standard Cancelled

Milk and milk products - Determination of milk fat purity by gas chromatographic analysis of triglycerides (Reference method)

ISO 17678|IDF 202:2010 specifies a reference method for the determination of milk fat purity using gas chromatographic analysis of triglycerides. Both vegetable fats and animal fats such as beef tallow and lard can be detected. By using defined triglyceride equations, the integrity of milk fat is determined. Basically, the method applies to bulk milk, or products made thereof, irrespective of feeding, breed or lactation conditions. In particular, the method is applicable to fat extracted from milk products purporting to contain pure milk fat with unchanged composition, such as butter, cream, milk, and milk powder. However, under the circumstances listed hereafter, a false positive result can be obtained. Hence, the method is not applicable to milk fat: a) obtained from bovine milk other than cow's milk; b) obtained from single cows; c) obtained from cows which received an exceptionally high feeding of pure vegetable oils such as rapeseed oil; d) obtained from colostrum; e) subjected to technological treatment such as removal of cholesterol or fractionation; f) obtained from skim milk or buttermilk; g) extracted by using the Gerber, Weibull–Berntrop or Schmid–Bondzynski–Ratzlaff methods, or that has been isolated using detergents (e.g. the Bureau of Dairy Industries method). With the extraction methods specified in g), substantial quantities of partial glycerides or phospholipids can pass into the fat phase. Consequently, the scope of ISO 17678|IDF 202:2010 excludes certain products and particularly cheese, whose ripening process can also affect the fat composition to such a degree that a false positive result is obtained.

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Main informations

Collections

National standards and national normative documents

Publication date

April 2010

Number of pages

4 p.

Reference

NF EN ISO 17678

ICS Codes

67.100.10   Milk and processed milk products

Classification index

V04-026

Print number

1 - 12/04/2010

International kinship

European kinship

EN ISO 17678:2010
Sumary
Milk and milk products - Determination of milk fat purity by gas chromatographic analysis of triglycerides (Reference method)

ISO 17678|IDF 202:2010 specifies a reference method for the determination of milk fat purity using gas chromatographic analysis of triglycerides. Both vegetable fats and animal fats such as beef tallow and lard can be detected. By using defined triglyceride equations, the integrity of milk fat is determined.

Basically, the method applies to bulk milk, or products made thereof, irrespective of feeding, breed or lactation conditions. In particular, the method is applicable to fat extracted from milk products purporting to contain pure milk fat with unchanged composition, such as butter, cream, milk, and milk powder.

However, under the circumstances listed hereafter, a false positive result can be obtained. Hence, the method is not applicable to milk fat: a) obtained from bovine milk other than cow's milk; b) obtained from single cows; c) obtained from cows which received an exceptionally high feeding of pure vegetable oils such as rapeseed oil; d) obtained from colostrum; e) subjected to technological treatment such as removal of cholesterol or fractionation; f) obtained from skim milk or buttermilk; g) extracted by using the Gerber, Weibull–Berntrop or Schmid–Bondzynski–Ratzlaff methods, or that has been isolated using detergents (e.g. the Bureau of Dairy Industries method).

With the extraction methods specified in g), substantial quantities of partial glycerides or phospholipids can pass into the fat phase. Consequently, the scope of ISO 17678|IDF 202:2010 excludes certain products and particularly cheese, whose ripening process can also affect the fat composition to such a degree that a false positive result is obtained.

Standard replaced by (1)
NF EN ISO 17678
June 2019
Standard Current
Milk and milk products - Determination of milk fat purity by gas chromatographic analysis of triglycerides (Reference method)

<p>This document specifies a reference method for the determination of milk fat purity using gas chromatographic analysis of triglycerides. The method utilizes the differences in triglyceride fingerprint of milk fat from the individual triglyceride fingerprints of other fats and oils to determine samples which are outside the range normally observed for milk fat. This is achieved by using the defined triglyceride formulae based on the normalized weighted sum of individual triglyceride peaks which are sensitive to the integrity of the milk<sup>[6][7]</sup>. The integrity of the milk fat can be determined by comparing the result of these formulae with those previously observed for a range of pure milk fat samples<sup>[12]</sup>. Both vegetable fats and animal fats such as beef tallow and lard can be detected.</p> <p>The method is applicable to bulk milk, or products made thereof, irrespective of the variation in common feeding practices, breed or lactation conditions. In particular, the method is applicable to fat extracted from milk products purporting to contain pure milk fat with unchanged composition, such as butter, cream, milk and milk powder.</p> <p>Because a false-positive result can occur, the method does not apply to milk fat related to these circumstances:</p> <p>a) obtained from bovine milk other than cow's milk;</p> <p>b) obtained from single cows;</p> <p>c) obtained from cows whose diet contained a particularly high proportion of vegetable oils such as rapeseed, cotton or palm oil, etc.;</p> <p>d) obtained from cows suffering from serious underfeeding (strong energy deficit);</p> <p>e) obtained from colostrum;</p> <p>f) subjected to technological treatment such as removal of cholesterol or fractionation;</p> <p>g) obtained from skim milk, buttermilk or whey;</p> <p>h) obtained from cheeses showing increased lipolysis;</p> <p>i) extracted using the Gerber, Weibull?Berntrop or Schmid?Bondzynski?Ratzlaff methods, or that has been isolated using detergents (e.g. the Bureau of Dairy Industries method).</p> <p>With the extraction methods specified in i), substantial quantities of partial glycerides or phospholipids can pass into the fat phase.</p> <p>NOTE 1 In nature, butyric (<i>n</i>-butanoic) acid (C4) occurs exclusively in milk fat and enables quantitative estimations of low to moderate amounts of milk fat in vegetable and animal fats to be made. Due to the large variation of C4, for which the approximate content ranges from 3,1 % fat mass fraction to 3,8 % fat mass fraction, it is difficult to provide qualitative and quantitative information for foreign fat to pure milk fat ratios of up to 20 % mass fraction<sup>[</sup><sup>11</sup><sup>]</sup>.</p> <p>NOTE 2 In practice, quantitative results cannot be derived from the sterol content of vegetable fats, because they depend on production and processing conditions. Furthermore, the qualitative determination of foreign fat using sterols is ambiguous.</p> <p>NOTE 3 Due to special feeding practices such as those related to c) and d), false-positive results have sometimes been reported for milk from certain Asian regions<sup>[</sup><sup>15</sup><sup>]</sup>. Moreover, grass-only diets such as mountain and, in particular, highland pasture feeding sometimes cause false-positive results, which can be substantiated by a content of conjugated linoleic acid (C18:2 c9t11) of ≥ 1,3 % fatty acid mass fraction<sup>[16][17]</sup>. Nevertheless, results conforming to the criteria of milk fat purity specified in this document are accepted, even if samples were undoubtedly produced under conditions reported in this note, including those described in h).</p> <p>NOTE 4 In cases where a positive result is suspected to be caused by circumstances related to c) or d), another analytical method, such as fatty acid or sterol analysis, can be applied to confirm the finding. Due to similar or increased limitations (e.g. as described in NOTE 1 and NOTE 2), a negative result obtained by another method is not appropriate to contrastingly confirm milk fat purity.</p>

Table of contents
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  • Avant-propos
    iv
  • 1 Domaine d'application
    1
  • 2 Références normatives
    2
  • 3 Termes et définitions
    2
  • 4 Principe
    2
  • 5 Réactifs
    2
  • 6 Appareillage
    3
  • 7 Échantillonnage
    4
  • 8 Mode opératoire
    5
  • 8.1 Préparation des échantillons pour essai
    5
  • 8.2 Préparation de la solution échantillon de matière grasse
    6
  • 8.3 Analyse chromatographique des triglycérides
    6
  • 9 Intégration, évaluation et contrôle de la performance analytique
    8
  • 10 Calcul et expression des résultats
    10
  • 10.1 Composition des triglycérides
    10
  • 10.2 Valeurs de S
    11
  • 10.3 Détection des matières grasses étrangères
    11
  • 11 Fidélité
    12
  • 11.1 Essai interlaboratoires
    12
  • 11.2 Répétabilité
    12
  • 11.3 Reproductibilité
    12
  • 12 Rapport d'essai
    13
  • Annexe A (normative) Préparation de la colonne remplie
    14
  • Annexe B (informative) Quantification des matières grasses étrangères
    18
  • Annexe C (informative) Incertitude de mesure
    20
  • Annexe D (informative) Essai interlaboratoires
    21
  • Bibliographie
    23
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