Djurfoder

Ämnesområden: Djurfoder
Kommittébeteckning: SIS/TK 435 (Livsmedel och foder)
Källa: CEN
Svarsdatum: den 15 okt 2018
Se merSe mindre
 

This document specifies a gas chromatographic mass spectrometric (GC-MS) method for the determination of organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) in animal feeding stuffs and oil.

The method is applicable to animal feeding stuffs consisting of less than 20 % by mass and oil/fatty samples containing residues of one or more of the following OCPs and PCBs and some of their isomers and degradation products:

— aldrin;

— dieldrin;

— chlordane, as the sum of chlordane isomers and oxychlordane;

— dichlorodiphenyltrichloroethane (DDT), as the sum of isomers op'-DDT, pp'-DDT, pp'-TDE (pp'-DDD), and pp'-DDE;

— endosulfan, as the sum of α-/β-isomers and endosulfan-sulphate;

— endrin, as the sum of endrin and delta-keto-endrin;

— heptachlor, as the sum of heptachlor and heptachlor epoxide;

— hexachlorobenzene (HCB);

— hexachlorocyclohexane isomers α-HCH (α-BHC), β-HCH (β-BHC), γ-HCH (γ-BHC or lindane);

— photo heptachlor;

cis- and trans-nonachlor;

— non dioxin-like PCBs (ndl-PCBs), as the sum of PCB 28, 52, 101, 138, 153 and 180.

The method has been fully validated by a collaborative trial for the substances and corresponding ranges (ng/g) noted in Table 1.

The method has not been fully validated for oxychlordane, endrin ketone, cis- and trans-nonachlor and photo heptachlor in all matrices.

The method is not applicable to chlorocamphene (toxaphene), a complex mixture of polychlorinated camphenes. Chlorocamphene has a very distinctive chromatographic profile and is easily recognizable by GC/ECD. Positive identification of the toxaphene isomers can be performed by negative chemical ionization mass spectrometry (NCI-MS), electron impact tandem mass spectrometry (EI MS × MS) or electron impact high resolution mass spectrometry (EI-HRMS), which is not within the scope of this method.

A limit of quantification (LOQ) for the mentioned organochlorine pesticides of 5 ng/g should normally be obtained. However, 10 ng/g applies for heptachlor aldrin, endrin, dieldrin, and endosulfan (α-, β- and sulphate). For the ndl-PCBs an LOQ of 0,5 to 1,0 ng/g should be obtained. The LOQs mentioned apply to the individual compounds (i.e. not the sum of two or more compounds). Individual laboratories are responsible for ensuring that the equipment that they used will achieve these LOQs. On customers' demand the standard may be applied to solely the analysis of PCBs or OCPs.

 

Ämnesområden: Djurfoder
Kommittébeteckning: SIS/TK 435 (Livsmedel och foder)
Källa: CEN
Svarsdatum: den 15 okt 2018
Se merSe mindre
 

This document specifies a gas chromatographic method with electron capture detection (ECD) for the determination of organochlorine pesticides (OCP’s) in animal feeding stuffs.

The method is applicable to animal feeding stuffs with a water content up to about 20 % by weight and oil/fatty samples containing residues of one or more of the following OCP’s, toxaphene and some of their isomers and degradation products:

— aldrin;

— dieldrin;

— chlordane (as the sum of chlordane isomers and oxychlordane);

— dichlorodiphenyltrichloroethane (DDT) (as the sum of isomers op'-DDT, pp'-DDT, pp'-TDE (pp'-DDD), and pp'-DDE);

— endosulfan (as the sum of α-/β-isomers and endosulfan-sulphate);

— endrin (sum of endrin and delta-keto-endrin);

— heptachlor (as the sum of heptachlor and heptachlor epoxide);

— hexachlorobenzene (HCB);

— hexachlorocyclohexane isomers α-HCH (α-BHC), β-HCH (β-BHC), γ-HCH (γ-BHC or lindane);

— photo heptachlor;

— cis- and trans-nonachlor;

A limit of quantification (LOQ) for the mentioned OCPs of 5 ng/g is intended to be obtained. However, 10 ng/g applies for heptachlor, aldrin, endrin, dieldrin, and endosulfan (α-/β– and sulphate). Individual laboratories are responsible for ensuring that the equipment that they use, achieves these limits of quantifications. The LOQs apply to the individual OCPs.

Ämnesområden: Djurfoder
Kommittébeteckning: SIS/TK 435 (Livsmedel och foder)
Källa: CEN
Svarsdatum: den 15 okt 2018
Se merSe mindre
 

This document method is applicable for the determination of theobromine in compound feed by liquid chromatography with UV detection in the tested range of 27 mg/kg to 307 mg/kg. This method has been validated using complementary compound feed for adult dogs and complementary compound feedstuff for horses. The actual working range can extend beyond the tested range. Alternative chromatography conditions using liquid chromatography tandem mass spectrometry (LC-MS/MS) are also provided for the validated range of 49 mg/kg to 307 mg/kg. This method has also been shown to be fit for purpose for the determination of theobromine in baking chocolate by both HPLC-UV and LC-MS/MS.

Ämnesområden: Djurfoder; Kemisk analys
Kommittébeteckning: SIS/TK 435 (Livsmedel och foder)
Källa: CEN
Svarsdatum: den 30 okt 2018
Se merSe mindre
 

This document specifies a method for the determination of organic acids in animal feeding stuffs by Ion

Chromatography with conductivity detection (IC-CD).

The method is intended to be used for the determination of formic acid, lactic acid, propionic acid, citric

acid, fumaric acid and malic acid as active substances in feed additives, premixtures, compound feed and

water and for screening of acetic acid in the same matrices. This method determines the total extractable

concentration of the above mentioned organic acids and their salts.

It is advisable that the user of this standar determine the working range of the method for each organic

acid. The lower limit of the working range depends on the matrix and the interferences encountered. A

working range between 10 [mg/l] and 100 [mg/l] should be achievable.

The method was successfully tested in an inter-laboratory study in concentrations between 0,02 % up to

27 % of the above mentioned organic acids.

NOTE Limitation occurs during simultaneous determination of high concentration of lactic acid and low

concentration of acetic acid. If the ratio of concentration of lactic acid to acetic acid exceeds factor 20, the

determination of acetic acid is not guaranteed.

On the basis of the referred working range, sample weight and extraction volume, limits of quantification

(LOQ), as calculated (Table 1) should be achievable.

Table 1 — Limits of quantification (LOQ)

Organic acid LOQ [mg/kg]

Formic acid 200

Lactic acid 200

Propionic acid 200

Citric acid 200

Fumaric acid 200

Acetic acid 200

Malic acid 200

 

Ämnesområden: Djurfoder; Kemisk analys
Kommittébeteckning: SIS/TK 435 (Livsmedel och foder)
Källa: CEN
Svarsdatum: den 30 okt 2018
Se merSe mindre
 

This document specifies a method for the determination of benzoic acid and sorbic acid in animal feeding stuffs by high-performance liquid chromatography method with ultraviolet detection (HPLC-UV).

The method is intended to be used for the determination of benzoic acid and sorbic acid as active substances in feed additives, premixtures and compound feed and for benzoic acid in water. This method determines the total extractable concentration of these organic acids and their salts.

It is advisable that the working range of the method is determined for each organic acid by the user of this standard. The lower limit of the working range depends on the matrix and the interferences encountered. It is advisable that a working range between 5 mg/l and 100 mg/l is accessible.

The method was successfully tested in an inter-laboratory study in concentrations between 0,02 % up to 9,0 %.

On the basis of the referred working range, sample weigh and extraction volume, limits of quantification (LOQ), as calculated (Table 1) on the basis of a wavelength of 230 nm, can be achievable.

Table 1 — Limits of quantification (LOQ) at 230 nm Organic acid

LOQ (mg/kg)

Benzoic acid

200

Sorbic acid

200

Kommittébeteckning: SIS/TK 435 (Livsmedel och foder)
Källa: CEN
Svarsdatum: den 30 okt 2018
Se merSe mindre
 

This document specifies a high performance liquid chromatographic – tandem mass spectrometry (LC-MS/MS) method for the simultaneous screening and/or determination of the eleven authorized coccidiostats (halofuginone, robenidine hydrochloride, nicarbazin, diclazuril, decoquinate, monensin sodium, salinomycin sodium, narasin, lasalocid sodium, semduramicin sodium and maduramicin ammonium alpha) contents in poultry, cattle and pig feed at additive and cross-contamination levels and of five non-registered coccidiostats (ethopabate, clopidol, ronidazole, dimetridazole and amprolium) at sub-additive levels and for the screening of the prohibited furazolidone antibiotic at sub-additive level, in the same matrices.

The range of application of the method is fit for the purpose of the screening and determination of all eleven coccidiostats at the values set by European legislation, of the non-registered coccidiostats and of the screening of the banned antibiotic.