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BS EN ISO 17678:2019 – TC:2020 Edition

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Tracked Changes. Milk and milk products. Determination of milk fat purity by gas chromatographic analysis of triglycerides

Published By Publication Date Number of Pages
BSI 2020 68
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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[6][7]. 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[12]. Both vegetable fats and animal fats such as beef tallow and lard can be detected. 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. Because a false-positive result can occur, the method does not apply to milk fat related to these circumstances: a) obtained from bovine milk other than cow’s milk; b) obtained from single cows; c) obtained from cows whose diet contained a particularly high proportion of vegetable oils such as rapeseed, cotton or palm oil, etc.; d) obtained from cows suffering from serious underfeeding (strong energy deficit); e) obtained from colostrum; f) subjected to technological treatment such as removal of cholesterol or fractionation; g) obtained from skim milk, buttermilk or whey; h) obtained from cheeses showing increased lipolysis; 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). With the extraction methods specified in i), substantial quantities of partial glycerides or phospholipids can pass into the fat phase. NOTE 1 In nature, butyric (n-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[11]. 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. 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[15]. 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[16][17]. 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). NOTE 4 In cases where a positive resu

PDF Catalog

PDF Pages PDF Title
1 compares BS EN ISO 17678:2019
2 TRACKED CHANGES
Text example 1 — indicates added text (in green)
36 undefined
38 European foreword
Endorsement notice
40 Foreword
43 1 Scope
44 2 Normative references
3 Terms and definitions
4 Principle
45 5 Reagents
6 Apparatus
46 7 Sampling
47 8 Procedure
8.1 Preparation of test samples
8.1.1 General
8.1.2 Isolation from butter or butteroil
8.1.3 Extraction according to the Röse–Gottlieb gravimetric method
8.1.4 Extraction from milk using silica gel columns
48 8.1.5 Extraction from cheese
8.2 Preparation of fat sample solution
8.3 Chromatographic triglyceride determination
8.3.1 Baseline drift
8.3.2 Injection technique
8.3.3 Calibration
49 8.3.4 Chromatographic conditions
50 9 Integration, evaluation and control of the analytical performance
52 10 Calculation and expression of results
10.1 Triglyceride composition
10.1.1 Calculation
10.1.2 Expression of test results
53 10.2 S-values
10.2.1 Calculation
10.2.2 Expression of test results
10.3 Detection of foreign fat
54 11 Precision
11.1 Interlaboratory test
11.2 Repeatability
11.3 Reproducibility
55 12 Test report
56 Annex A (normative) Preparation of the packed column
60 Annex B (informative) Quantification of the foreign fat content
62 Annex C (informative) Uncertainty of measurement
63 Annex D (informative) Interlaboratory test
65 Bibliography
BS EN ISO 17678:2019 - TC
$217.84