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TITLE: Method for the detection of zeranol and taleranol in meat and liver
S.O.P. Page
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  • 1.
  • INTRODUCTION

  • Summary
  • 1.1

This SOP describes a screening and confirmation method for the determination of resorcyclic acid lactones (RAL’s) in meat and liver samples of bovine origin. A procedure is described for the detection of a -zearalanol (zeranol) and b-zearalanol

(taleranol) by a combination of solid phase extraction (SPE) and GC-MS. The method consist of, digestion of the meat sample using the enzyme protease and hydrolysis of the liver sample using suc d’Helix Pomatia, extraction of the RAL’s with tert-butylmethylether (TBME), purification using reversed-phase C18 cartridges. This method can also be used for the metabolites a -zearalenol, b-zearalenol, zearalanone and zearalenone. When doing so

validation for these compounds is necessary.

1.2

1.3
Field of application The method is used to perform routine screening in meat and liver samples and has proven to be suitable for the analysis of a -zearalanol and b-zearalanol. The limit of detection is 0.5 mg/g based on the detection of the most abundant diagnostic ions namely m/z 433 and m/z 437 for the internal standard, with a response at the correct retention time exceeding the signal to noise ratio of 3. The method is validated according to SOP ARO/425 (1.3.3).

References
1.3.1. H.J. van Rossum et al, Multi residue analysis anabolic agents, SOP ARO/113, revision 4, 21 January 1997, RIVM.
1.3.2. H.A. Herbold, S.S. Sterk, R.W. Stephany, L.A. van Ginkel. Multi residue method using coupled-column HPLC and GC-MS for the determination of anabolic agents in samples of urine. RIVM report n.389002 - 035, September 1997.
1.3.3. A.A.M. Stolker, Procedure for the validation of analytical methods, SOP ARO/425, revision 1, 28 April 1997, RIVM.
1.3.4. Report: European Commission Decision laying down requirements for analytical methods to be used for detecting certain substances and residue thereof in live animals and animal products according to Council Directive 93/256/EC.
1.3.5 S.M. Gort and R. Hoogerbrugge, Linear regression program Calwer. Report RIVM no.
502501025. A spreadsheet program for calibration. March 1995.

  • 2.
  • MATERIALS

Reference to a company and/or product is for purposes of identification and information only and does not imply approval or recommendation of the company and/or the product by the National Institute of Public Health and Environment (RIVM) to the exclusion of others which might also be suitable.
TITLE: Method for the detection of zeranol and taleranol in meat and liver
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  • 2.1
  • Chemicals

2.1.1 SPE extraction columns, 6 ml, 1 g, disposable octadecyl (C18) (Alltech, 205430). 2.1.2 SPE extraction columns, 6 ml, 1 g, disposable amino (NH2) (Alltech, 211153). 2.1.3 Methanol (Baker, 8045). 2.1.4 Ethanol (Baker, 8006). 2.1.5 Acetone (Baker, 8001). 2.1.6 Iso-octane (Baker, 8715). 2.1.7 Derivatization reagent: N,O-bis(trimethylsilyl)trifkuoracetamide (BSTFA) with 1% TMCS
(Pierce, 38832).
2.1.8 Acetic acid (Merck, 63). 2.1.9 Sodium acetate (Merck, 6268). 2.1.10 Hydrochloric acid, 37% solution (Merck, 317). 2.1.11 Beta-glucuronidase/sulfatase (suc d'Helix Pomatia containing 100.000 units ß-glucuronidase and 100.000 units sulfatase per ml, France, code IBR 213473.
2.1.12 Acetate buffer, 2 mol/l, pH 5.2 Dissolve 25.2 g acetic acid and 129.5 g sodium acetate in
800 ml water. Adjust the pH to 5.2 ± 0.1, add water to a final volume of 1000 ml.
2.1.13 Tris buffer, 0.1 mol/l, pH 9.5. Dissolve 12.1 g of Tris(hydroxymethyl)-amino-methane
(2.1.16) in 800 ml of water. Adjust the pH (5.5.18.) at 9.5 ± 0.1 and add water to a final volume of 1000 ml.
2.1.14 Tert-butylmethylether (TBME) (Merck, 1845). 2.1.15 Subtilisin (Protease) (Sigma, P-5380). 2.1.16 Tris(hydroxymethyl)-amino-methane (Merck, 8382)

  • 2.2.
  • Relevant Internal Standards

2.2.1 a-Zearalanol-d4 and b-zearalanol-d4

The analytes are a mixture of ± 50% of each compound. RIVM/ARO sample no. 87M1553. From these a standard stock solution containing 1 mg/ml is prepared. The stock solutions is prepared by dissolving the appropriate amount of the analytes in ethanol. Quality control includes the registration of a mass spectrum (identity). These solutions are stored in the dark at -20°C for a maximum period of 5 years. Working solutions are prepared by 10-fold dilution of the stock solutions with methanol. These solutions are stored in the dark at 4°C (range 1-10°C) for a maximum period of 6 months.

2.2.2 a-Zearalanol and b-zearalanol

Relevant data of the analytes are listed in table 1. Stock solutions containing 1 mg/ml are prepared by dissolving the appropriate amount of the analytes in ethanol. Quality control includes the registration of a mass spectrum (identity). These solutions are stored in the dark at -20°C for a maximum period of 5 years. Working solutions are prepared by 10-fold dilution of the stock solutions with methanol. These solutions are stored in the dark at 4°C (range 1-10°C) for a maximum period of 6 months.

Table 1. Data of analytes.

  • Analytes
  • CAS #
  • Formula
  • Mol. weight

322.4 a -zearalanol b-zearalanol
26538-44-3 42422-68-4

C18H26O5 C18H26O5

322.4
TITLE: Method for the detection of zeranol and taleranol in meat and liver
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  • 2.3
  • Equipment

2.3.1 ASPEC® (Automated Sample Preparation with Disposable Extraction Columns) XL Gilson.
The ASPEC® consists of three components: a model 401C dilutor, a sample processor and a set of racks and accessories to handle 6 ml SPE columns. The ASPEC® is programmed using the Gilson Sample Manager 721 software.
2.3.2 Collecting tubes for the ASPEC® system, Gilson type B54728-4. 2.3.3 Derivatization vials, Screw Top Vial /PTFE Septa (Omnilabo, 154920). 2.3.4 Automatic pipettes (Gilson P20, P100, P200, P1000 and P5000). 2.3.5 Injection vials, Wide Mouth Crimp (Alltech, 98213), with micro inserts (200 ml) (Alltech,
EK-1022.395) and aluminium caps (Chrompack, 10210).
2.3.6 GC-MS equipment. Hewlett Packard 5890 series 11 gaschromatograph, equipped with a
Hewlett Packard 7673 automatic sampler, a Hewlett Packard Vectra computer 486/66U with HPchem data acquisition software and a 5989A Mass Spectrometer (type Engine).
2.3.7 Fused silica capillary column CP SIL-5, Low bleeding/non polar, length 60 m, i.d. 0.25 mm,
0.1 micron film thickness, (Chrompack, 7818).
2.3.8 Vortex (Vortex-Genie). 2.3.9 pH-meter, (Applikon). 2.3.10 Moulinette S (Moulinex). 2.3.11 Electric water bath, thermostat adjustable ± 5°C, with nitrogen facility (TurboVap, Zymark). 2.3.12 Varifuge 3.0R, centrifuge with swing-out rotor 5315 (Heraeus). 2.3.13 Centrifuge tubes (50 ml), plastic (Omnilabo) 2.3.14 Incubator TH15, (Edmund Bühler).

  • 3.
  • GC-MS CONDITIONS

Table 2: Parameters GC-MS Carrier gas helium Column
0.6 ml/min (EPC system for constant flow) 60 meter CP-SIL-5 Low Bleeding/non polar fused silica capillary (0.25 mm i.d. 0.1 mm film)

250oC MS-source, 120 o C quadruple. 80oC for 1 min, increased at 30oC/min. to 300oC and held at this temperature for 5 min.
Detector temperature Oven temperature

  • Ionisation
  • EI - positive, SIM mode

Injection volume Pressure
3 ml Electronic Pressure Control syst. Pressure is held at 50 psi for 1 minute, decreased at 99 psi/minute to 28.4 psi, constant during the oven-temperature program

  • 433, 437 (internal standard)
  • Mass monitored

  • Tune
  • High mass/sensitivity tune.

TITLE: Method for the detection of zeranol and taleranol in meat and liver
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4.

ANALYTICAL PROCEDURES

  • Sample pre-treatment
  • 4.1

Meat and liver (1 kg) is crushed and homogenised in a Moulinette S (Moulinex). A test portion of 5.0 g is weighted into a 50 ml centrifuge tube, spiked with a mixture of internal standards (a -zearalanol-d4 and b-zearalanol-d4) at the level of 10 ng

(corresponding to 2 ng/g).

4.1.1 Meat samples

For digestion, 10 ml volume of Trisbuffer (2.1.13) and 5 mg subtilisin (2.1.15) is added. The mixture is vortexed for 30 seconds and shaken thoroughly for two hours at 50o C.

4.1.2 Liver samples

For hydolysis, 40 ml of Suc Helix Pomatia (2.1.11), diluted with 10 ml 2 M acetate buffer (pH 5.2) (2.1.12) is added. The mixture is vortexed for 30 sec., check pH 5.2 (when necessary adjust the pH with acetic acid to 5.2) and hydrolyse overnight at 37oC, with constant shaking by means of an incubator equipped with a shaker.

  • 4.2
  • Liquid/liquid extraction

To the mixture (4.1) 2 ml conc. HCl and 10 ml TBME is added, shake for 10 minutes and centrifuge for 3 minutes at 3600 rpm. The organic layer is collected in a glass tube. This operation is repeated with 5 ml TBME. The extract in the glass tube is evaporated at 50oC under a gentle stream of nitrogen. The dry residue is dissolved in 5 ml of MeOH/milli-Q water (40-60) and washed twice with 1 ml hexane (each time centrifuged for 3 minutes at 3600 rpm). The hexane layer is separated from the MeOH-water fraction and discarded. The MeOH- water layer in the tube is cleaned over C18 disposable column (SPE).

  • 4.3
  • SPE Chromatography

4.3.1 Meat

The C18 column (6 ml) is preconditioned with 5 ml of MeOH and 5 ml milli-Q water at a flow rate of 6 ml/min. The sample (4.2) is passed through the column. The C18 column is washed with 5 ml of milli-Q water and a mixture of 4 ml of MeOH/milli-Q water (40-60). The analytes for meat are eluted with 3 ml of acetone (for liver see 4.3.2). This eluate is collected and evaporated at 50oC under a gently stream of nitrogen, until dryness and dissolved in 0.5 ml MeOH.

4.3.2 Liver

An extra cleanup step with NH2 amino disposable column (SPE) is necessary. The NH2- column is preconditioned with 3 ml acetone and the collected eluate (3 ml of acetone) is passed through the amino column. This eluate is collected and evaporated at 50oC under a gently stream of nitrogen, until dryness and dissolved in 0.5 ml MeOH.

  • 4.4
  • Detection

The extract (4.3) is transferred into a derivatization-vial and evaporated at 50oC under a gently stream of nitrogen until dryness. The dry residue is derivatized with 20 ml BSTFA. The

derivatization-vials are placed in a heater at 60o C for about 30 minutes. Evaporate at 50oC under a stream of nitrogen until dry and dissolve in 20 ml iso-octane and transfer into an injection-vial with micro insert. The 7673 automatic sampler injects 3 ml of these extracts into the GC-MS and measures the diagnostic ions 433 and 437 in the SIM-mode.
TITLE: Method for the detection of zeranol and taleranol in meat and liver
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  • 5
  • INTERPRETATION AND CALCULATION

  • 5.1
  • Checks

The first step in interpreting the results is to check for: - Adequate performance characteristics of the GC-MS system (MS-tuning). - Adequate sensitivity for external derivatized standards (S/N a -zearalanol-d4

[3.0 ng absolute] > 6).
- Adequate signals for internal standard in sample (S/N a -zearalanol-d4 [2 ppb] > 3).

  • 5.2
  • Calculation of quantitative results

Quantitative results are obtained by constructing calibration curves of the response variable versus the concentration. Quantification is only valid if: - The maximum of the signal originating from the analyte has a S/N ratio > 3. - The coefficient of correlation of the constructed calibration curve is better than 0.99. - The numerical value of the intercept does not deviate more than ± 3 SD from zero.

Calibration curves are calculated using calibration software Calwer, option linear regression (1.3.5).

5.3

5.4
Calculation in case of deuterated internal standard When for the analyte concerned the corresponding deuterated internal standard was added to the test portion, quantification is straight forward. The area of the selected ion of the standard and internal standard are calculated and the ratio is the response variable. A calibration curve is constructed by analysing different concentrations of standard in range of the inspected concentration in the sample. A linear curve is fitted using least squares linear regression calculation. Unknown concentrations are calculated by interpolation.

Identification For identification according to the EC-criteria it is mandatory that the GC retention time corresponds with the retention time of the internal standard and that at least 4 ions are monitored. Each ion monitored (response) should fulfil the criterion that the S/N ratio of the maximum exceeds a value of 3. The ratio of the analyte’s retention time to that of the internal standard (relative retention time), should correspond to that of the calibration standard at a tolerance of ± 0.5%. The relative intensities of the detected ions, expressed as a percentage of the intensity of the most intense ion (base peak) must correspond to those of the standard analyte, either from calibration standards or from spiked samples, at comparable concentrations, within the following tolerances (table 3).

Table 3: Maximum permitted tolerances for relative ion intensities. Relative intensity compared to base peak. Relative error compared to calibration (Ratio in % of base peak) > 50% > 20% - 50% > 10% - 20% £ 10% standard. ± 10% ± 15% ± 20% ± 50%
TITLE: Method for the detection of zeranol and taleranol in meat and liver
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  • 6.
  • VALIDATION OF METHOD

  • Reproducibility
  • 6.1

The reproducibility, definitions and criteria according to European Commission decision 93/256/EC, determined at the level of 1 ppb, on 5 different days in triplate. Internal standard at 2 ppb level.

Table 4: Results reproducibility. Matrix

  • a -Zearalanol
  • b-Zearalanol

  • Average (%) STD
  • VC(%) Average (%) STD
  • VC(%)

30 17
Liver Meat

  • 94
  • 19

18
21 17
102 112
31

  • 20
  • 108

6.2

6.3
Limit of detection The limit of detection is the amount of the analyte which is necessary for a signal/noise of 6 (S/N). Samples of 5.0 g liver (or meat) are spiked with a mixture of internal standards (a - zearalanol-d4 and b-zearalanol-d4) at the level of 2 ppb and spiked with a mixture of a - zearalanol and b-zearalanol at the level of 0.2, 0.5, 1.0, 2.0 ppb. In this case, the limit of detection for liver and meat is given at 0.5 ppb and the signal/noise is 6.

Accuracy A sample of 5.0 g is spiked with a mixture of internal standards (a -zearalanol-d4 and bzearalanol-d4) at the level of 2 ppb and spiked with a mixture of a -zearalanol and bzearalanol at the levels 0.2, 0.5 and 1 ppb, in triplo.(The yield must be > 80%). (Results see table 5)

Table 5: Results accuracy.

  • a -Zearalanol
  • b-Zearalanol

Matrix

Average (%) 85.8 116.9
STD 15.6 24.9

  • VC(%) Average (%)
  • STD

22.2 24.1
VC (%) 22.1 24.5
Liver Meat
18.1 21.3
100.7 98.6

  • 6.4
  • Repeatability

The repeatability is determined at the level of 1 ppb by spiking a blank sample and measuring it 10 times. Samples of 5.0 g liver (or meat) are spiked with a mixture of internal standards (a -zearalanol-d4 and b-zearalanol-d4) at the level of 2 ppb and spiked with a mixture of a - zearalanol and b-zearalanol at the level of 1.0 ppb (10 times). Results see table 6.

Table 6: Results repeatability. Matrix a -Zearalanol Average (%) 93.8 b-Zearalanol

  • VC(%) Average (%) STD
  • STD

13.8 24.5
VC(%) 22.8 13.6
Liver Meat
14.8 22.8
96.7 117.4
22.0

  • 15.9
  • 107.4

TITLE: Method for the detection of zeranol and taleranol in meat and liver
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  • 6.5
  • Ruggedness

The ruggedness of a method can be estimated by measuring the effects of changes in external conditions. In this case, 5 different blank liver samples are spiked at the level of 1 ppb and a mixture of internal standards (a -zearalanol-d4 and b-zearalanol-d4) at the level of 2 ppb.

Results see table 7.

Table 7: Results ruggedness. Matrix a -Zearalanol Average (%) 67.8 b-Zearalanol

  • VC(%) Average (%) STD
  • STD

14.8 8.3
VC(%) 22.0 17.4
Liver Meat
21.8 7.8
102.4 110.0
22.5

  • 19.1
  • 106.6

  • 6.6
  • Recovery

For the absolute recovery of the method, samples of 5.0 g (liver or meat) is spiked with a mixture of a -zearalanol and b-zearalanol at the level of 1.0 ppb (3 times) and after clean-up with a mixture of internal standards (a -zearalanol-d4 and b-zearalanol-d4) at the level of 2 ppb. Results see table 8.

Table 8: Results recovery. Matrix a -Zearalanol Average (%) 47.0 b-Zearalanol

  • VC(%) Average (%) STD
  • STD

8.0 1.0
VC(%) 25.0 2.6
Liver Meat
17.0 6.0
54.7 22
13.7

  • 0.6
  • 16

TITLE: Method for the detection of zeranol and taleranol in meat and liver
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  • 7.
  • CHROMATOGRAM LIVER SAMPLE

Figure 1: Blank liver sample. Internal standard m/z 437 (2 ppb).

Ion 433.00 (432.70 to 433.70): 99020294.D
Abundance

1000

950 900
Time-->

  • 11.00
  • 11.05
  • 11.10
  • 11.15
  • 11.20
  • 11.25
  • 11.30
  • 11.35
  • 11.40
  • 11.45

Ion 437.00 (436.70 to 437.70): 99020294.D
Abundance

1500

  • 11.17
  • 11.25

1000
Time-->

  • 11.00
  • 11.05
  • 11.10
  • 11.15
  • 11.20
  • 11.25
  • 11.30
  • 11.35
  • 11.40
  • 11.45

Figure 2: Spiked liver sample, level 1 ppb. Diagn. ions m/z 433, 437
(internal st. 2 ppb)

Ion 433.00 (432.70 to 433.70): 99020295.D
Abundance

  • 11.19
  • 11.26

1800

1600 1400 1200 1000 Time-->

  • 11.05
  • 11.10
  • 11.15
  • 11.20
  • 11.25
  • 11.30
  • 11.35
  • 11.40
  • 11.45

Ion 437.00 (436.70 to 437.70): 99020295.D
Abundance

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    Acta Veterinaria (Beograd), Vol. 56, No. 2-3, 121-136, 2006. DOI: 10.2298/AVB0603121S UDK 619:636.4.087.7 HAEMATOLOGICAL AND BIOCHEMICAL PARAMETERS OF WEANED PIGLETS FED ON FODDER MIXTURE CONTAMINATED BY ZEARALENONE WITH ADDITION OF CLINOPTILOLITE [PERANDA MARCELA*, LIKER B**, [PERANDA T*, [ERI] V***, ANTUNOVI] Z*, GRABAREVI] @****, SEN^I] \*, GRGURI] D***** and STEINER Z* *Faculty of Agriculture, Osijek, Croatia; **Faculty of Agriculture, Zagreb, Croatia; ***Clinical Hospital Osijek, Croatia; ****Faculty of Veterinary Medicine, Zagreb, Croatia; *****Centar for Livestock Improvement, Osijek (Received 20. October 2005) The effect of zeolite clinoptilolite (CLIN) on some metabolic parameters in blood serum and haematological values in weaned piglets fed with increased levels of zearalenone (ZEN) was investigated over a 14-day period. The research involved four groups of weaned piglets aged 40 to 54 days. All groups were fed on fodder mixture for growing pigs containing 20% crude protein and 12.57 MJ ME/kg. The first control group (C1) received a concentrate mixture without added ZEN or mycotoxin adsorbent Min-a-Zel Plus®. The second control group (C2) was fed on fodder mixture containing 0.2% of modified clinoptilolite (Min-a-Zel Plus®; levels of zearalenone <5.1 ng/g). Piglets in the experimental group (E1) were fed on fodder mixture containing added zeralenone (3 mg/kg) (Sigma-Aldrich Co) and 0.2% of Min-a-Zel Plus® preparation. The second experimental group (E2) was fed on fodder mixture to which 3 mg/kg of zearalenone was added, but with no addition of Min-a-Zel Plus®. Oestrogenic effect of ZEN was evident in the sinergistic action with insulin which was manifested in an increased total protein level, lower level of glucose, triacylglycerols, serum iron, a higer level of cholesterol and higher aminotransaminase activity.
  • Pharmaceutical Appendix to the Tariff Schedule 2

    Pharmaceutical Appendix to the Tariff Schedule 2

    Harmonized Tariff Schedule of the United States (2007) (Rev. 2) Annotated for Statistical Reporting Purposes PHARMACEUTICAL APPENDIX TO THE HARMONIZED TARIFF SCHEDULE Harmonized Tariff Schedule of the United States (2007) (Rev. 2) Annotated for Statistical Reporting Purposes PHARMACEUTICAL APPENDIX TO THE TARIFF SCHEDULE 2 Table 1. This table enumerates products described by International Non-proprietary Names (INN) which shall be entered free of duty under general note 13 to the tariff schedule. The Chemical Abstracts Service (CAS) registry numbers also set forth in this table are included to assist in the identification of the products concerned. For purposes of the tariff schedule, any references to a product enumerated in this table includes such product by whatever name known. ABACAVIR 136470-78-5 ACIDUM LIDADRONICUM 63132-38-7 ABAFUNGIN 129639-79-8 ACIDUM SALCAPROZICUM 183990-46-7 ABAMECTIN 65195-55-3 ACIDUM SALCLOBUZICUM 387825-03-8 ABANOQUIL 90402-40-7 ACIFRAN 72420-38-3 ABAPERIDONUM 183849-43-6 ACIPIMOX 51037-30-0 ABARELIX 183552-38-7 ACITAZANOLAST 114607-46-4 ABATACEPTUM 332348-12-6 ACITEMATE 101197-99-3 ABCIXIMAB 143653-53-6 ACITRETIN 55079-83-9 ABECARNIL 111841-85-1 ACIVICIN 42228-92-2 ABETIMUSUM 167362-48-3 ACLANTATE 39633-62-0 ABIRATERONE 154229-19-3 ACLARUBICIN 57576-44-0 ABITESARTAN 137882-98-5 ACLATONIUM NAPADISILATE 55077-30-0 ABLUKAST 96566-25-5 ACODAZOLE 79152-85-5 ABRINEURINUM 178535-93-8 ACOLBIFENUM 182167-02-8 ABUNIDAZOLE 91017-58-2 ACONIAZIDE 13410-86-1 ACADESINE 2627-69-2 ACOTIAMIDUM 185106-16-5 ACAMPROSATE 77337-76-9
  • TGA Review of Hgps

    TGA Review of Hgps

    A REVIEW TO UPDATE AUSTRALIA’S POSITION ON THE HUMAN SAFETY OF RESIDUES OF HORMONE GROWTH PROMOTANTS (HGPs) USED IN CATTLE Prepared by Chemical Review and International Harmonisation Section Office of Chemical Safety Therapeutic Goods Administration of the Department of Health and Ageing Canberra July 2003 A draft of this report was tabled at the 25th Meeting of the Advisory Committee on Pesticides and Health (ACPH), held in Canberra on the 1st May 2003. The report was subsequently endorsed out-of-session by the ACPH. Hormone Growth Promotants TABLE OF CONTENTS ABBREVIATIONS ................................................................................................................................................................4 EXECUTIVE SUMMARY ..................................................................................................................................................7 INTRODUCTION..................................................................................................................................................................9 HEALTH CONCERNS ASSOCIATED WITH HGP S................................................................................................................9 DIFFICULTIES ASSOCIAT ED WITH ASSESSING THE SAFETY OF HGPS.........................................................................10 RISK ASSESSMENTS OF HGP S .........................................................................................................................................10 PURPOSE OF THE CURRENT
  • NORMATIVE INSTRUCTION 5 of APRIL 23, 2019 (Published in the Official Gazette of the Federal Government (DOU) on 25/04/2019)

    NORMATIVE INSTRUCTION 5 of APRIL 23, 2019 (Published in the Official Gazette of the Federal Government (DOU) on 25/04/2019)

    NORMATIVE INSTRUCTION 5 OF APRIL 23, 2019 (Published in the Official Gazette of the Federal Government (DOU) on 25/04/2019) THE SECRETARY FOR ANIMAL AND PLANT HEALTH OF THE MINISTRY OF AGRICULTURE, LIVESTOCK AND FOOD SUPPLY, using the power attributed to him by Articles 21 and 63, of Appendix I, of Decree 9,667, of January 2, 2019, taking into consideration what is set forth in Ordinance (Portaria) 51, of February 6, 1986, Ordinance (Portaria) 527 of August 15, 1995, SDA Normative Instruction 42 of December 20, 1999, Decree 9,013 of March 29, 2017; and what is set forth in Case File 21000.022222/2019-71, resolves: Article 1. To approve the publication of the sampling plan and the reference limits for the National Plan for the Control of Residues and Contaminants in Animal Products - PNCRC of 2019, for the chains of beef, pork, goat, mutton, equine, rabbit, poultry, ostrich meat, and milk, fisheries, honey and eggs. Paragraph 1. The sampling plan and limits of reference stated in the heading hereof will be published in the Ministry of Agriculture, Livestock and Food Supply. Article 2. The tests for the Monitoring and Exploratory Subprogram of the PNCRC described in Article 1 herein are be performed in the official and authorized laboratories of the National Network of Agricultural Laboratories of the Unified System for Animal and Plant Health, as established by Normative Instruction 57 of December 11, 2013. Article. 3 This Normative Instruction shall come into force as of the date of its publication. JOSÉ GUILHERME TOLLSTADIUS LEAL TABLE
  • World Mycotoxin Journal, February 2014; 7 (1): 3-33 Publishers

    World Mycotoxin Journal, February 2014; 7 (1): 3-33 Publishers

    Wageningen Academic World Mycotoxin Journal, February 2014; 7 (1): 3-33 Publishers Developments in mycotoxin analysis: an update for 2012-2013 F. Berthiller1, P.A. Burdaspal2, C. Crews3, M.H. Iha4, R. Krska1, V.M.T. Lattanzio5, S. MacDonald3, R.J. Malone6, C. Maragos7, M. Solfrizzo5, J. Stroka8 and T.B. Whitaker9 1University of Natural Resources and Life Sciences, Vienna, Department for Agrobiotechnology (IFA-Tulln), Christian Doppler Laboratory for Mycotoxin Metabolism and Center for Analytical Chemistry, Konrad Lorenz Str. 20, 3430 Tulln, Austria; 2National Centre for Food, Spanish Food Safety and Nutrition Agency, Carretera de Majadahonda a Pozuelo km 5, 228220 Majadahonda, Spain; 3The Food and Environment Research Agency, Sand Hutton, York YO41 1LZ, United Kingdom; 4Instituto Adolfo Lutz, Laboratrio I de Ribeiro Preto, Av Dr Arnaldo 355, CEP 14085-410, Ribeiro Preto SP, Brazil; 5Institute of Sciences of Food Production, National Research Council, Via Amendola 122/o, Bari 700126, Italy; 6Trilogy Analytical Laboratory, 870 Vossbrink Drive, Washington, MO 63090, USA; 7USDA, ARS National Center for Agricultural Utilization Research, 1815 N. University St., Peoria, IL 61604, USA; 8Institute for Reference Materials and Measurements (IRMM), European Commission Joint Research Centre, Retieseweg 111, 2440 Geel, Belgium; 9Biological and Agricultural Engineering Department, N.C. State University, P.O. Box 7625, Raleigh, NC 27695-7625, USA; [email protected] Received: 12 September 2013 / Accepted: 2 December 2013 © 2014 Wageningen Academic Publishers REVIEW ARTICLE Abstract This review highlights developments in mycotoxin analysis and sampling over a period between mid-2012 and mid-2013. It covers the major mycotoxins: aflatoxins, Alternaria toxins, ergot alkaloids, fumonisins, ochratoxins, patulin, trichothecenes and zearalenone.
  • WT/DS320/R Page 141

    WT/DS320/R Page 141

    WT/DS320/R Page 141 (b) Summary of the main arguments of the parties315 7.2 With reference to the Panel's question whether panels are permitted to open hearings to public observation under Articles 12 (including Appendix 3), 14.1 and 17.10 of the DSU, the European Communities argues that a panel may adopt working procedures that foresee open hearings, as Article 12.1 of the DSU provides that panels may depart from the working procedures in Appendix 3 after consulting the parties to the dispute. 7.3 The European Communities also argues that this conclusion is not affected by Article 14.1 of the DSU on confidentiality of panel deliberations. The term "deliberations" does not cover the meetings with the parties, for which a different terminology is used in Appendix 3 of the DSU. 7.4 The European Communities considers that in the present case where all the parties have agreed to open hearings, the Panel should accommodate the parties' request. Article 18.2 of the DSU also supports the position that parties are entitled to "waive" the confidentiality of their positions. 7.5 Regarding the legal implications of open hearings on covered persons under the Rules of Conduct, the European Communities considers that no legal issues arise under the Rules of Conduct. In the European Communities view, the Rules of Conduct are and remain fully binding on all covered persons in this dispute, even if the hearings are opened to the public. The Panel's deliberations will in any event not be affected by the opening and remain confidential, as required by Article 14.1 of the DSU.
  • Wo 2008/127291 A2

    Wo 2008/127291 A2

    (12) INTERNATIONAL APPLICATION PUBLISHED UNDER THE PATENT COOPERATION TREATY (PCT) (19) World Intellectual Property Organization International Bureau (43) International Publication Date PCT (10) International Publication Number 23 October 2008 (23.10.2008) WO 2008/127291 A2 (51) International Patent Classification: Jeffrey, J. [US/US]; 106 Glenview Drive, Los Alamos, GOlN 33/53 (2006.01) GOlN 33/68 (2006.01) NM 87544 (US). HARRIS, Michael, N. [US/US]; 295 GOlN 21/76 (2006.01) GOlN 23/223 (2006.01) Kilby Avenue, Los Alamos, NM 87544 (US). BURRELL, Anthony, K. [NZ/US]; 2431 Canyon Glen, Los Alamos, (21) International Application Number: NM 87544 (US). PCT/US2007/021888 (74) Agents: COTTRELL, Bruce, H. et al.; Los Alamos (22) International Filing Date: 10 October 2007 (10.10.2007) National Laboratory, LGTP, MS A187, Los Alamos, NM 87545 (US). (25) Filing Language: English (81) Designated States (unless otherwise indicated, for every (26) Publication Language: English kind of national protection available): AE, AG, AL, AM, AT,AU, AZ, BA, BB, BG, BH, BR, BW, BY,BZ, CA, CH, (30) Priority Data: CN, CO, CR, CU, CZ, DE, DK, DM, DO, DZ, EC, EE, EG, 60/850,594 10 October 2006 (10.10.2006) US ES, FI, GB, GD, GE, GH, GM, GT, HN, HR, HU, ID, IL, IN, IS, JP, KE, KG, KM, KN, KP, KR, KZ, LA, LC, LK, (71) Applicants (for all designated States except US): LOS LR, LS, LT, LU, LY,MA, MD, ME, MG, MK, MN, MW, ALAMOS NATIONAL SECURITY,LLC [US/US]; Los MX, MY, MZ, NA, NG, NI, NO, NZ, OM, PG, PH, PL, Alamos National Laboratory, Lc/ip, Ms A187, Los Alamos, PT, RO, RS, RU, SC, SD, SE, SG, SK, SL, SM, SV, SY, NM 87545 (US).
  • Front Page Food

    Front Page Food

    Food Safety www.chiron.no Chiron AS Stiklestadveien 1 N-7041 Trondheim, Norway Tel: +47 73 87 44 90 Fax: +47 73 87 44 99 Mail: [email protected] www.chiron.no Food Safety Catalogue - 2012 Table of contents General ......................................................................................................................................................... 2 Food safety I: Highly Purified Natural Toxins for Food Analysis ............................................................. 4 Food Safety II: Food Contaminants ............................................................................................................. 9 Food safety III: Food Colour and Aroma .................................................................................................... 15 Isopropylthioxanthone (ITX) ...................................................................................................................... 19 Desphenylchloridazon-15N2........................................................................................................................20 PCBs .......................................................................................................................................................... 21 PBDEs, PBBs, Flame Retardants, Halobenzenes and Phenols ................................................................... 27 PCNs, PBNs and HaloPAHs ....................................................................................................................... 35 SCCP/PCA, Chloroalkanes .......................................................................................................................