GB 5009.24-2016 PDF English
US$115.00 · In stock · Download in 9 secondsGB 5009.24-2016: National food safety standard - Determination of M Aflatoxins in Foods Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedureStatus: Valid GB 5009.24: Evolution and historical versions
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivery | Name of Chinese Standard | Status |
| GB 5009.24-2016 | English | 115 |
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National food safety standard - Determination of M Aflatoxins in Foods
| Valid |
| GB 5009.24-2010 | English | 239 |
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3 days
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National food safety standard -- Determination of aflatoxins M1 and B1 in foods
| Obsolete |
| GB/T 5009.24-2003 | English | 239 |
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2 days
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Determination of aflatoxins M1 and B1 in foods
| Obsolete |
| GB/T 5009.24-1996 | English | 199 |
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2 days
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Method for determination of aflatoxions M1 and B1 in foods
| Obsolete |
| GB 5009.24-1985 | English | 199 |
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2 days
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Method for determination of aflatoxins M1 and B1 in foods
| Obsolete |
Excerpted PDFs (Download full copy in 9 seconds upon purchase)PDF Preview: GB 5009.24-2016
GB 5009.24-2016: National food safety standard - Determination of M Aflatoxins in Foods---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GB5009.24-2016
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
Foreword
This Standard serves as a replacement of GB 5413.37-2010 National Food Safety
Standard - Determination of Aflatoxin M1 in Milk and Milk Products; GB 5009.24-2010
National Food Safety Standard - Determination of Aflatoxin M1 and B1 in Foods; GB/T
23212-2008 Determination of Aflatoxin B1, B2, G1, G2, M1, M2 Content in Milk and Milk
Powder - HPLC-fluorescence Detection Method; SN/T 1664-2005 Determination of
Aflatoxin M1, B1, B2, G1, G2 Content in Milk and Milk Powder.
In comparison with GB 5413.37-2010, the main changes are as follows.
---The name of the standard is modified into “National Food Safety Standard -
Determination of M Aflatoxins in Foods”;
---The scope of application of the methods is extended;
---The detection of aflatoxins M2 is added;
---Enzyme-linked immunosorbent assay is modified; the name of the third method
is modified into enzyme-linked immunosorbent screening assay;
---Liquid chromatography-mass spectrometry is modified;
---The pretreatment method of liquid chromatography is modified;
---Immunochromatography purification fluorescence spectrophotometry is deleted.
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.
3.1.2 Methanol (CH3OH). chromatographic purity.
3.1.8 Hydrochloric acid (HCl).
3.1.9 Petroleum ether (CnH2n+2). boiling range. 30 °C ~ 60 °C.
3.2 Reagent Preparation
3.2.1 Ammonium acetate solution (5 mmol/L). weigh-take 0.39 g of ammonium acetate;
dilute it in 1,000 mL of water, then, mix it up.
3.2.2 Acetonitrile - water solution (25 + 75). measure-take 250 mL of acetonitrile; add
it to 750 mL of water, then, mix it up.
3.3 Standards
3.3.1 AFT M1 standard (C17H12O7, CAS. 6795-23-9). purity ≥ 98%, or nationally certified
standard substance with the standard substance certificate.
3.3.2 AFT M2 standard (C17H14O7, CAS. 6885-57-0). purity ≥ 98%, or nationally certified
standard substance with the standard substance certificate.
3.3.3 13C17-AFT M1 isotope solution (C17H14O7). 0.5 μg/mL.
3.4 Standard Solution Preparation
3.4.1 Standard stock solution (10 μg/mL). respectively weigh-take 1 mg (accurate to
0.01 mg) of AFT M1 and AFT M2; respectively use acetonitrile to dissolve it, then, dilute
to the constant volume of 100 mL.
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.
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.
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.
4.8 Nitrogen blowing instrument.
4.9 Liquid chromatography - tandem mass spectrometer. equipped with electrospray
ion source.
4.10 Round sieve. 1 mm ~ 2 mm aperture.
4.11 Glass fiber filter paper. rapid, high-load, particle retention in liquid. 1.6 μm.
4.12 Disposable microporous filter head. equipped with 0.22 μm microporous
membrane (before use, selected filter membrane shall adopt standard solution to
confirm that there is no absorption phenomenon).
5 Analytical Procedure
The application of immunoaffinity columns provided by different manufacturers might
be slightly different in sample operation, such as sample loading, leaching and elution.
Thus, operation shall comply with the requirements in the operating instructions
provided by the manufacturers.
5.1 Sample Extraction
5.1.1 Liquid milk and yogurt
Weigh-take 4 g (accurate to 0.001 g) of evenly mixed 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 10 mL of methanol, then, 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.
5.2 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 immunoaffinity column, transfer the above-mentioned
sample solution to a 50 mL syringe;
5.3 Liquid Chromatography Reference Conditions
Liquid chromatography reference conditions are listed below.
5.6 Draw a Standard Curve
Under the liquid chromatography - tandem mass spectrometry analytical conditions in
5.3 and 5.4, inject the standard series of solution for determination from low
concentration to high concentration. Use the peak area ratio - concentration of AFT M1
and AFT M2 chromatographic peak and internal standard chromatographic peak 13C17-
AFT M1 to draw the curve. Obtain standard curve regression equation; its linear
correlation coefficient shall be more than 0.99.
5.8 Blank Test
Do not weigh or take sample; comply with the steps in 5.1 and 5.2 to conduct the blank
test. Make sure that there is no substance that would interfere the component to be
determined.
6 Expression of Analytical Result
The residue of AFT M1 or AFT M2 in the sample shall be calculated in accordance with
Formula (1).
7 Precision
The absolute difference of two independent determination results obtained under
repeatability conditions shall not exceed 20% of the arithmetic mean value.
8 Others
When weighing-taking 4 g of liquid milk and yogurt, this Method’s detection limit of AFT
M1 is 0.005 μg/kg; the detection limit of AFT M2 is 0.005 μg/kg; the quantitation limit of
AFT M1 is 0.015 μg/kg; the quantitation limit of AFT M2 is 0.015 μg/kg.
9 Principle
Use methanol - water solution to extract aflatoxins M1 and aflatoxins M2 in sample.
After diluting the supernatant, purify and enrich through the immunoaffinity column.
After concentration,
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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