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EN 14177:2003

Current

Current

The latest, up-to-date edition.

Foodstuffs - Determination of patulin in clear and cloudy apple juice and puree - HPLC method with liquid/liquid partition clean-up

Published date

17-12-2003

Foreword
1 Scope
2 Normative references
3 Principle
4 Reagents
   4.1 General
   4.2 Sodium carbonate solution, mass concentration
        rho(Na[2]CO[3]) approx. 15 g/l
   4.3 Acetic acid, volume concentration varphi(CH[3]COOH)
        approx. 98%.
   4.4 Sodium sulfate anhydrous
   4.5 pH 4 water
   4.6 Absolute ethanol, varphi(CH[3]CH[2]OH) >= 99,7%
   4.7 Ethyl acetate
   4.8 Perchloric acid, varphi(HclO[4]) = 60%
   4.9 Acetonitrile
   4.10 Endogalacturonase enzyme solution, typical activity
        1 400 U/g
   4.11 HPLC mobile phase
   4.12 Patulin stock solution
   4.13 Patulin standard solution
   4.14 Patulin standard solution for calibration
5 Apparatus
   5.1 General
   5.2 Displacement pipettes of 5 ml, 1 ml, 200 micro l and
        50 micro l capacity with appropriate pipette tips
   5.3 Analytical balance
   5.4 UV spectrophotometer, double beam and recording suitable
        for measurement at 250 nm to 350 nm
   5.5 Quartz cells, of optical path length 1 cm
   5.6 Centrifuge, capable of operating at 4 500 g
   5.7 Centrifuge tubes of 50 ml capacity with screw cap lids
   5.8 Rotary evaporator, with water bath set at 40 degree C
   5.9 Filter paper, with pore size 20 micro m to 25 micro m
   5.10 Disposable syringe filters, of 0,2 micro m pore size
        (optional)
   5.11 HPLC apparatus, comprising the following
   5.12 Round bottom flasks, of 250 ml capacity with ground
        glass joint
6 Procedure
   6.1 Preparation of test samples
   6.2 Extraction of patulin
   6.3 Removal of interfering acidic compounds
   6.4 Preparation of the sample test solution
7 Spiking procedure
   7.1 Clear apple juice
   7.2 Cloudy apple juice
   7.3 Apple puree
8 HPLC determination
   8.1 Calibration graph
   8.2 HPLC operating conditions
9 Calculation
10 Precision
   10.1 Interlaboratory test
   10.2 Repeatability
   10.3 Reproducibility
   10.4 Test report
Annex A (informative) Precision data
Bibliography

This European Standard specifies a method for the determination of patulin in apple juices and apple puree up to 128 ug/kg using high performance liquid chromatography (HPLC).

Committee
CEN/TC 275
DocumentType
Standard
PublisherName
Comite Europeen de Normalisation
Status
Current

Standards Relationship
DIN EN 14177:2004-03 Identical
NBN EN 14177 : 2004 Identical
NEN EN 14177 : 2004 Identical
NS EN 14177 : 1ED 2004 Identical
I.S. EN 14177:2004 Identical
PN EN 14177 : 2005 Identical
SN EN 14177 : 2004 Identical
UNI EN 14177 : 2004 Identical
UNE-EN 14177:2004 Identical
BS EN 14177:2003 Identical
NF EN 14177 : 2004 Identical

ISO 3696:1987 Water for analytical laboratory use — Specification and test methods
EN ISO 3696:1995 Water for analytical laboratory use - Specification and test methods (ISO 3696:1987)

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