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GB 5009.24-2016 English PDF (GB5009.24-2016)

GB 5009.24-2016 English PDF (GB5009.24-2016)

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GB 5009.24-2016: National Food Safety Standard -- Determination of M Aflatoxins in Foods
GB 5009.24-2016
National Food Safety Standard -- Determination of M Aflatoxins in Foods
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard -
Determination of M Aflatoxins in Foods
Issued on. December 23, 2016 Implemented on. June 23, 2017
Issued by. National Health and Family Planning Commission of the PRC;
China Food and Drug Administration.
Table of Contents
Foreword ...4 
1 Scope ...5 
Method I -- Isotope Dilution Liquid Chromatography - Tandem Mass
Spectrometry ...5 
2 Principle ...5 
3 Reagents and Materials ...5 
4 Instruments and Apparatuses ...7 
5 Analytical Procedure ...8 
6 Expression of Analytical Result ...13 
7 Precision ...13 
8 Others ...13 
Method II -- High-performance Liquid Chromatography ...14 
9 Principle ...14 
10 Reagents and Materials ...14 
11 Instruments and Apparatuses ...15 
12 Analytical Procedure ...16 
13 Expression of Analytical Result ...17 
14 Precision ...18 
15 Others ...18 
Method III -- Enzyme-linked Immunosorbent Assay ...18 
16 Principle ...18 
17 Reagents and Materials ...19 
18 Instruments and Apparatuses ...19 
19 Analytical Procedure ...19 
20 Expression of Analytical Result ...20 
21 Precision ...21 
22 Others ...21 
Appendix A Standard Concentration Calibration Method for AFT M1 and AFT M2
...22 
Appendix B Column Capacity Verification Method for Immunoaffinity Column
...23 
Appendix C Liquid Chromatography - Mass Spectrogram and Sub-ion Scan 24 
Appendix D Liquid Chromatogram ...27 
Appendix E Mass Determination Method of Enzyme-linked Immunosorbent
Assay Kit ...28 
National Food Safety Standard -
Determination of M Aflatoxins in Foods
1 Scope
This Standard specifies the methods for the determination of aflatoxins M1 and
aflatoxins M2 (hereinafter referred to as AFT M1 and AFT M2) in foods.
Method I is isotope dilution liquid chromatography - tandem mass spectrometry, which
is applicable to the determination of AFT M1 and AFT M2 in milk, milk products and milk-
containing special dietary food.
Method II is high-performance liquid chromatography; its scope of application is the
same as Method I.
Method III is enzyme-linked immunosorbent screening assay, which is applicable to
the screening determination of AFT M1 in milk, milk products and milk-containing
special dietary food.
Method I -- Isotope Dilution Liquid Chromatography -
Tandem Mass Spectrometry
2 Principle
Use methanol - water solution to extract aflatoxins M1 and aflatoxins M2 in sample.Use
water or phosphate buffer solution to dilute the supernatant, then, purify and enrich it
through immunoaffinity column.After concentration, constant-volume and filtering of
the purified liquid, separate it through liquid chromatography.Detect it through tandem
mass spectrometry, then, quantify it through isotope internal standard method.
3 Reagents and Materials
Unless it is otherwise stipulated, all reagents adopted in this Method shall be analytical
pure; water shall be Grade-1 water stipulated in GB/T 6682.
3.1 Reagents
3.1.1 Acetonitrile (CH3CN). chromatographic purity.
calibrate the concentration (please refer to Appendix A for the calibration method).
3.4.2 Mixed standard stock solution (1.0 μg/mL). respectively and accurately absorb
1.00 mL of 10 μg/mL AFT M1 and AFT M2 standard stock solution, then, place them in
the same 10 mL volumetric flask.Add acetonitrile to dilute to the constant volume, then,
obtain 1.0 μg/mL mixed standard solution.This solution can be preserved in an airtight
container in the dark at 4 °C; it shall remain valid for 3 months.
3.4.3 Mixed standard working solution (100 ng/mL). accurately absorb 1.0 mL of mixed
standard stock solution (1.0 μg/mL), then, place it in a 10 mL volumetric flask.Use
acetonitrile to dilute to the constant volume.This solution can be preserved in an
airtight container in the dark at 4 °C; it shall remain valid for 3 months.
3.4.4 50 ng/mL isotope internal standard working solution 1(13C17-AFT M1). take 1 mL
of AFT M1 isotope internal standard (0.5 μg/mL), then, use acetonitrile to dilute to 10
mL.Preserve it at -20 °C; it shall be used for the determination of liquid sample.It shall
remain valid for 3 months.
3.4.5 5 ng/mL isotope internal standard working solution 2(13C17-AFT M1). take 100 μL
of AFT M1 isotope internal standard (0.5 μg/mL), then, use acetonitrile to dilute to 10
mL.Preserve it at -20 °C; it shall be used for the determination of solid sample.It shall
remain valid for 3 months.
3.4.6 Standard series of working solution. respectively and accurately absorb 5 μL, 10
μL, 50 μL, 100 μL, 200 μL and 500 μL of standard working solution, then, place them
in 10 mL volumetric flask.Add 100 μL of 50 ng/mL isotope internal standard working
solution.Use initial mobile phase to dilute to the constant volume.Thus, prepare AFT
M1 and AFT M2 series of standard solution at the concentration of 0.05 ng/mL, 0.1
ng/mL, 0.5 ng/mL, 1.0 ng/mL, 2.0 ng/mL and 5.0 ng/mL.
4 Instruments and Apparatuses
4.1 Balance. division value. 0.01 g, 0.001 g and 0.00001 g.
4.2 Water bath kettle. temperature controlled at 50 °C ± 2 °C.
4.3 Vortex mixer.
4.4 Ultrasonic cleaner.
4.5 Centrifuge. ≥ 6,000 r/min.
4.6 Rotary evaporator.
4.7 Solid phase extraction device (equipped with vacuum pump).
4.8 Nitrogen blowing instrument.
vortex mixing.If milk powder cannot completely dissolve, place the centrifuge tube in
50 °C water bath; after the milk powder completely dissolves, take it out.Wait till the
sample solution cools down to 20 °C, then, add 10 mL of methanol; start vortex for 3
min.Place it at 4 °C; start centrifugation at 6,000 r/min for 10 min, or, filter it through
glass fiber filter paper.Transfer an appropriate amount of the supernatant or filtrate to
a beaker, then, add 40 mL of water or PBS to dilute it; reserve it for later use.
5.1.3 Cream
Weigh-take 1 g (accurate to 0.001 g) of sample, then, place it in a 50 mL centrifuge
tube.Add 100 μL of 13C17-AFT M1 internal standard solution (5 ng/mL); start oscillation
blending, then, evenly place it for 30 min.Add 8 mL of petroleum ether; wait till cream
dissolves, then, add 9 mL of water and 11 mL of methanol.Start oscillation for 30 min.
Transfer all the liquid to separating funnel.Add 0.3 g of sodium chloride, then,
thoroughly shake and dissolve it.Evenly place it and wait for layering, then, transfer
the lower layer to a round-bottomed flask.Start rotary evaporation, till it is below 10
mL, then, use PBS to dilute it to 30 mL.
5.1.4 Cheese
Weigh-take 1 g (accurate to 0.001 g) of already shredded and evenly mixed sample
(through aperture 1 mm ~ 2 mm round sieve), then, place it in a 50 mL centrifuge tube.
Add 100 μL of 13C17-AFT M1 internal standard solution (5 ng/mL); start oscillation
blending, then, evenly place it for 30 min.Add 1 mL of water and 18 mL of methanol.
Start oscillation for 30 min.Place it at 4 °C; start centrifugation at 6,000 r/min for 10
min, or, filter it through glass fiber filter paper.Transfer an appropriate amount of the
supernatant or filtrate to a round-bottomed flask.Start rotary evaporation, till it is below
2 mL, then, use PBS to dilute it to 30 mL.
5.2 Purification
5.2.1 Preparation of immunoaffinity column
Restore immunoaffinity column, which is preserved at low temperature, to room
temperature.
5.2.2 Purification
After abandoning the liquid in the i...
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