EN 17362:2020

SLOVENSKI STANDARD
01-julij-2020
Krma: metode vzorčenja in analize - Določevanje pentaklorofenola (PCP) v
sestavinah krme in krmni mešanici z LC-MS/MS
Animal feeding stuffs: Methods of sampling and analysis - Determination of
pentachlorophenol (PCP) in feed materials and compound feed by LC-MS/MS
Futtermittel: Probenahme- und Untersuchungsverfahren - Bestimmung von
Pentachlorphenol (PCP) in Futtermittel und Mischfuttermittel mittels LC-MS/MS
Aliments pour animaux : Méthodes d’échantillonnage et d’analyse - Détermination de la
teneur en pentachlorophénol (PCP) dans les matières premières pour aliments des
animaux et les aliments composés pour animaux par CL-SM/SM
Ta slovenski standard je istoveten z: EN 17362:2020
ICS:
65.120 Krmila Animal feeding stuffs
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN 17362
EUROPEAN STANDARD
NORME EUROPÉENNE
April 2020
EUROPÄISCHE NORM
ICS 65.120
English Version
Animal feeding stuffs: Methods of sampling and analysis -
Determination of pentachlorophenol (PCP) in feed
materials and compound feed by LC-MS/MS
Aliments pour animaux : Méthodes d'échantillonnage Futtermittel: Probenahme- und
et d'analyse - Détermination de la teneur en Untersuchungsverfahren - Bestimmung von
pentachlorophénol (PCP) dans les matières premières Pentachlorphenol (PCP) in Futtermittel und
pour aliments des animaux et les aliments composés Mischfuttermittel mittels LC-MS/MS
pour animaux par CL-SM/SM
This European Standard was approved by CEN on 7 March 2020.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17362:2020 E
worldwide for CEN national Members.

Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 7
5 Reagents and materials . 7
5.1 General . 7
5.2 Chemicals . 7
6 Apparatus . 10
6.1 Analytical balance, accuracy to 0,1 mg . 10
6.2 Centrifuge . 10
6.3 Water bath . 10
6.4 Liquid chromatograph connected to a triple-quadrupole mass spectrometer . 10
7 Sampling . 11
8 Preparation of the test sample . 12
9 Procedure. 12
9.1 General . 12
9.2 Test portions and extraction . 12
9.3 LC-MS/MS . 13
10 Calculation and expression of results . 13
10.1 General . 13
10.2 Calibration criteria . 14
10.3 Identification and confirmation. 14
10.4 Calculation . 14
10.5 Recovery . 15
11 Precision . 15
11.1 Collaborative test . 15
11.2 Repeatability limit . 15
11.3 Reproducibility limit . 15
12 Test report . 16
Annex A (informative) Collaborative trial. 17
Bibliography . 19

European foreword
This document (EN 17362:2020) has been prepared by Technical Committee CEN/TC 327 “Animal
feeding stuffs: Methods of sampling and analysis”, the secretariat of which is held by NEN.
This document shall be given the status of a national standard, either by publication of an identical text
or by endorsement, at the latest by October 2020, and conflicting national standards shall be withdrawn
at the latest by October 2020.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document has been prepared under a standardization request given to CEN by the European
Commission and the European Free Trade Association.
According to the CEN-CENELEC Internal Regulations, the national standards organisations of the
following countries are bound to implement this document: Austria, Belgium, Bulgaria, Croatia, Cyprus,
Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy,
Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of North
Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United
Kingdom.
1 Scope
This document specifies a liquid chromatographic method with triple-quadrupole mass spectrometry
(MS/MS) detection for the determination of pentachlorophenol (PCP) in feed materials and compound
feed.
The limit of quantitation (LOQ) for the PCP determination in guar gum, fatty acid distillates (FAD) and
compound feed is 10 µg/kg. Individual laboratories are responsible for ensuring that the equipment that
they use will achieve this limit of quantification.
The method is validated in an international collaborative trial for pentachlorophenol in compound feed,
guar gum and fatty acid distillate in the range between 9 µg/kg and 22 µg/kg.
The results of the collaborative trial, in which 16 laboratories participated, have shown that the method
is applicable for the determination of PCP in compound feed, guar gum and FAD at the desired limit of
10 µg/kg. Satisfactory results were obtained for one compound feed sample, guar gum and the two FAD
samples (HorRat < 2), while for the second compound feed sample a HorRat value of 2,2 was obtained.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
EN ISO 6498, Animal feeding stuffs — Guidelines for sample preparation (ISO 6498)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— IEC Electropedia: available at http://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp
3.1
calibration
complete set of operations which estimates under specified conditions the calibration function from
observations of the response variable obtained on reference states
[SOURCE: ISO 3534-2:2006, 3.5.13 [1]]
3.2
collaborative trial
interlaboratory comparisons
organization, performance and evaluation of measurements or tests on the same or similar items by two
or more laboratories in accordance with predetermined conditions
[SOURCE: EN ISO/IEC 17043:2010, 3.4 [2]]
3.3
feed material
products of vegetable or animal origin, whose principal purpose is to meet animals’ nutritional needs, in
their natural state, fresh or preserved, and products derived from the industrial processing thereof, and
organic or inorganic substances, whether or not containing feed additives, which are intended for use in
oral animal-feeding either directly as such, or after processing, or in the preparation of compound feed,
or as carrier of premixtures
[SOURCE: Regulation (EC) No 767/2009 (Article 3(2)(g)) [3]]
3.4
HorRat
ratio of the reproducibility relative standard deviation to that calculated from the Horwitz equation
–0,15
Note 1 to entry: Predicted relative standard deviation PRSD = 2 C
R
HorRatR = RSDR / PRSDR (1)
HorRatr = RSDr / PRSDr (2)
Note 2 to entry: If applied to within-laboratory studies, the normal range of HorRat(r) is 0,30 to 1,30.
−6
Note 3 to entry: To check proper calculation of PRSDR, a C of 10 should give a PRSDR of 16 %. C is concentration
expressed as a mass fraction (both numerator and denominator expressed in the same units). The HorRat is
indicative of method performance for a large majority of methods in chemistry. Normal values lie between 0,50 and
2,00.
[SOURCE: ISO 16577:2016, 3.75 [4]]
3.5
limit of quantitation
measured quantity value, obtained by a given measurement procedure, which is the lowest concentration
of a measurand that can be determined with an acceptable level of repeatability precision and trueness
Note 1 to entry: The “limit of quantitation” is not a concept defined in ISO/IEC Guide 99:2007 [5] but has been
defined as described above.
Note 2 to entry: The abbreviation LOQ is sometimes used.
3.6
precision
closeness of agreement between indications or measured quantity values obtained by replicate
measurements on the same or similar objects under specified conditions
Note 1 to entry: Measurement precision is usually expressed numerically by measures of imprecision, such as
standard deviation, variance, or coefficient of variation under the specified conditions of measurement.
Note 2 to entry: The ‘specified conditions’ can be, for example, repeatability conditions of measurement,
intermediate precision conditions of measurement, or reproducibility conditions of measurement (see ISO 5725-1
[6]).
Note 3 to entry: Measurement precision is used to define measurement repeatability, intermediate measurement
precision, and measurement reproducibility.
Note 4 to entry: Sometimes 'measurement precision'
...