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GB 5009.25-2016 English PDF (GB5009.25-2016)
GB 5009.25-2016 English PDF (GB5009.25-2016)
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GB 5009.25-2016: Determination of sterigmatocystin in vegetable foods
GB 5009.25-2016
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard -
Determination of Sterigmatocystin in Food
ISSUED ON: DECEMBER 23, 2016
IMPLEMENTED ON: JUNE 23, 2017
Issued by: National Health and Family Planning Commission of the
People’s Republic of China;
China Food and Drug Administration.
Table of Contents
Foreword ... 3
1 Scope ... 4
Method I -- Liquid Chromatography - Tandem Mass Spectrometry ... 4
2 Principle ... 4
3 Reagents and Materials ... 4
4 Instruments and Equipment ... 6
5 Analytical Procedures ... 6
6 Expression of Analytical Result ... 9
7 Precision ... 10
8 Others ... 10
Method II -- Liquid Chromatography ... 10
9 Principle ... 10
10 Reagents and Solutions ... 10
11 Instruments and Equipment ... 12
12 Analytical Procedures ... 12
13 Expression of Analytical Result ... 14
14 Precision ... 14
15 Others ... 14
Method III -- Thin-layer Chromatography ... 15
16 Principle ... 15
17 Reagents and Solutions ... 15
18 Instruments and Equipment ... 16
19 Analytical Procedures ... 16
Appendix A Mass Spectrometry Conditions and Ion Source Control Conditions
... 20
Appendix B Liquid Chromatogram ... 23
National Food Safety Standard -
Determination of Sterigmatocystin in Food
1 Scope
This Standard specifies the methods for the determination of sterigmatocystin: liquid
chromatography - tandem mass spectrometry and high-performance liquid
chromatography.
This Standard is applicable to the determination of sterigmatocystin in rice, corn, wheat,
soy and peanut.
Method I -- Liquid Chromatography - Tandem Mass
Spectrometry
2 Principle
Use acetonitrile - aqueous solution to extract sterigmatocystin in the sample. Through
vortex, ultrasound and centrifugation, take the supernatant for dilution. Through solid
phase extraction column or immunoaffinity column, purify and concentrate it. Use
methanol - aqueous solution to reach a constant volume. Use microporous membrane
to filter it. Use liquid chromatography for separation. Use electrospray ion source for
ionization. Use multiple reactive ion monitoring for detection. Use isotope internal
standard method to quantify it.
3 Reagents and Materials
Unless it is otherwise stipulated, all reagents used in this Method shall be analytically
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.
3.1.3 Sodium chloride (NaCl).
3.4.3 Isotope internal standard working solution (1.0 μg/mL): accurately transfer-take
0.40 mL of sterigmatocystin isotope internal standard (25 μg/mL), then, place it into a
10 mL volumetric flask. Use methanol to dilute to a constant volume. Store it at -20 °C.
The storage life is 3 months.
3.4.4 Standard series working solution: accurately transfer-take a proper amount of
the standard working solution, then, place it into a 5 mL volumetric flask. Add 50 μL of
1.0 μg/mL isotope internal standard working solution. Use methanol - aqueous solution
(70 + 30) to reach to a constant scale (series standard solutions, in which,
sterigmatocystin concentration is: 1 ng/mL, 2 ng/mL, 5 ng/mL, 10 ng/mL, 20 ng/mL, 30
ng/mL, 40 ng/mL and 50 ng/mL). Prepare it right before usage.
3.5 Materials
3.5.1 Immunoaffinity column: column capacity 600 ng (please refer to B.2 for the
method of validating column capacity).
3.5.2 Solid phase extraction column: N-vinyl pyrrolidone and divinylbenzene
copolymer packed column (200 mg/6 mL), or equivalent. Before usage, respectively
use 5 mL of methanol and 5 mL of water to activate it.
3.5.3 Microporous membrane: 0.22 μm.
4 Instruments and Equipment
4.1 Liquid chromatograph - tandem mass spectrometer: equipped with electrospray
ion source.
4.2 High-speed pulverizer.
4.3 Vortex mixer.
4.4 Ultrasonic generator.
4.5 Balance: division value: 0.01 g and 0.00001 g.
4.6 Centrifuge: rotating speed 6,000 r/min.
4.7 Solid phase extraction device (equipped with vacuum pump).
4.8 Nitrogen blower.
4.9 Test sieve: aperture 1 mm ~ 2 mm.
5 Analytical Procedures
5.1 Sample Preparation
eluent into the scale test tube. Use vacuum pump to drain the affinity column. At 60 °C,
use nitrogen to slowly blow the eluent, till it becomes dry. Use methanol - aqueous
solution (70 + 30) to dilute to a constant volume of 1.0 mL. Conduct vortex for 30 s to
dissolve the residue. Use 0.22 μm membrane to filter it. Gather the filtrate in an
injection bottle to prepare for sample injection. In accordance with the same method of
operation, conduct blank test.
NOTE: in accordance with the practical situation in the laboratory, one of the above-
mentioned purification methods may be selected.
5.4 Reference Conditions of Instruments
5.4.1 Chromatographic reference conditions
a) Liquid phase chromatographic column: C18 column, column length: 100 mm;
internal diameter: 2.1 mm; particle size: 1.8 μm, or equivalent chromatographic
column;
b) Mobile phase: Phase-A: water; Phase-B: methanol;
c) Gradient elution conditions: 70% B (0 min ~ 5 min); 100% B (5 min ~ 8 min);
70% B (8 min ~ 12 min);
d) Flow rate: 0.2 mL/min;
e) Chromatographic column temperature: 40 °C;
f) Injection volume: 10 μL.
5.4.2 Mass spectrometry reference conditions
a) Mode of detection: multi-ion reaction monitoring (MRM);
b) Please refer to Table A.1 for mass spectrometry conditions and ion selection
parameters;
c) Please refer to Figure A.1 ~ Figure A.2 for sub-ion scan;
d) Please refer to Figure A.3 for liquid chromatography - mass spectrometry.
5.5 Draw a Standard Curve
In accordance with the sequence from low concentration to high concentration, inject
the standard series working solution into the liquid chromatograph - tandem mass
spectrometer; measure the peak area of corresponding chromatographic peak. Take
the concentration of sterigmatocystin in the standard series working solution as the x-
coordinate. Take the ratio of the peak area of sterigmatocystin chromatographic peak
and the peak area of isotope internal standard chromatographic peak as the y-
X---content of sterigmatocystin in the sample, expressed in (μg/kg);
---concentration of sterigmatocystin in the sample solution, obtained through the
standard curve, expressed in (ng/mL);
V---final constant volume, expressed in (mL);
m---weighing mass of the sample, expressed in (g);
f---dilution factor (f = 10);
The calculation result shall retain 3 significant figures.
7 Precision
The absolute difference of two independent determination results obtained under
repeatability condition shall not exceed 20% of the arithmetic mean value.
8 Others
When 5 g of rice, corn and wheat sample is weighed and taken, the detection limit is
0.6 μg/kg; the quantitation limit is 2 μg/kg. When 2 g of soy and peanut sample is
weighed and taken, the detection limit is 1.5 μg/kg; the quantitation limit is 5 μg/kg.
Method II -- Liquid Chromatography
9 Principle
Use acetonitrile - aqueous solution to extract sterigmatocystin in the sample. Through
homogenization, vortex, ultrasound and centrifugation, take the supernatant; use
phosphate buffer solution to dilute it. Use immunoaffinity column for purification and
elution. Use nitrogen to blow it to dryness and concentrate it. Use the mobile phase to
reach a constant volume. Use ...
Get QUOTATION in 1-minute: Click GB 5009.25-2016
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GB 5009.25-2016: Determination of sterigmatocystin in vegetable foods
GB 5009.25-2016
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard -
Determination of Sterigmatocystin in Food
ISSUED ON: DECEMBER 23, 2016
IMPLEMENTED ON: JUNE 23, 2017
Issued by: National Health and Family Planning Commission of the
People’s Republic of China;
China Food and Drug Administration.
Table of Contents
Foreword ... 3
1 Scope ... 4
Method I -- Liquid Chromatography - Tandem Mass Spectrometry ... 4
2 Principle ... 4
3 Reagents and Materials ... 4
4 Instruments and Equipment ... 6
5 Analytical Procedures ... 6
6 Expression of Analytical Result ... 9
7 Precision ... 10
8 Others ... 10
Method II -- Liquid Chromatography ... 10
9 Principle ... 10
10 Reagents and Solutions ... 10
11 Instruments and Equipment ... 12
12 Analytical Procedures ... 12
13 Expression of Analytical Result ... 14
14 Precision ... 14
15 Others ... 14
Method III -- Thin-layer Chromatography ... 15
16 Principle ... 15
17 Reagents and Solutions ... 15
18 Instruments and Equipment ... 16
19 Analytical Procedures ... 16
Appendix A Mass Spectrometry Conditions and Ion Source Control Conditions
... 20
Appendix B Liquid Chromatogram ... 23
National Food Safety Standard -
Determination of Sterigmatocystin in Food
1 Scope
This Standard specifies the methods for the determination of sterigmatocystin: liquid
chromatography - tandem mass spectrometry and high-performance liquid
chromatography.
This Standard is applicable to the determination of sterigmatocystin in rice, corn, wheat,
soy and peanut.
Method I -- Liquid Chromatography - Tandem Mass
Spectrometry
2 Principle
Use acetonitrile - aqueous solution to extract sterigmatocystin in the sample. Through
vortex, ultrasound and centrifugation, take the supernatant for dilution. Through solid
phase extraction column or immunoaffinity column, purify and concentrate it. Use
methanol - aqueous solution to reach a constant volume. Use microporous membrane
to filter it. Use liquid chromatography for separation. Use electrospray ion source for
ionization. Use multiple reactive ion monitoring for detection. Use isotope internal
standard method to quantify it.
3 Reagents and Materials
Unless it is otherwise stipulated, all reagents used in this Method shall be analytically
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.
3.1.3 Sodium chloride (NaCl).
3.4.3 Isotope internal standard working solution (1.0 μg/mL): accurately transfer-take
0.40 mL of sterigmatocystin isotope internal standard (25 μg/mL), then, place it into a
10 mL volumetric flask. Use methanol to dilute to a constant volume. Store it at -20 °C.
The storage life is 3 months.
3.4.4 Standard series working solution: accurately transfer-take a proper amount of
the standard working solution, then, place it into a 5 mL volumetric flask. Add 50 μL of
1.0 μg/mL isotope internal standard working solution. Use methanol - aqueous solution
(70 + 30) to reach to a constant scale (series standard solutions, in which,
sterigmatocystin concentration is: 1 ng/mL, 2 ng/mL, 5 ng/mL, 10 ng/mL, 20 ng/mL, 30
ng/mL, 40 ng/mL and 50 ng/mL). Prepare it right before usage.
3.5 Materials
3.5.1 Immunoaffinity column: column capacity 600 ng (please refer to B.2 for the
method of validating column capacity).
3.5.2 Solid phase extraction column: N-vinyl pyrrolidone and divinylbenzene
copolymer packed column (200 mg/6 mL), or equivalent. Before usage, respectively
use 5 mL of methanol and 5 mL of water to activate it.
3.5.3 Microporous membrane: 0.22 μm.
4 Instruments and Equipment
4.1 Liquid chromatograph - tandem mass spectrometer: equipped with electrospray
ion source.
4.2 High-speed pulverizer.
4.3 Vortex mixer.
4.4 Ultrasonic generator.
4.5 Balance: division value: 0.01 g and 0.00001 g.
4.6 Centrifuge: rotating speed 6,000 r/min.
4.7 Solid phase extraction device (equipped with vacuum pump).
4.8 Nitrogen blower.
4.9 Test sieve: aperture 1 mm ~ 2 mm.
5 Analytical Procedures
5.1 Sample Preparation
eluent into the scale test tube. Use vacuum pump to drain the affinity column. At 60 °C,
use nitrogen to slowly blow the eluent, till it becomes dry. Use methanol - aqueous
solution (70 + 30) to dilute to a constant volume of 1.0 mL. Conduct vortex for 30 s to
dissolve the residue. Use 0.22 μm membrane to filter it. Gather the filtrate in an
injection bottle to prepare for sample injection. In accordance with the same method of
operation, conduct blank test.
NOTE: in accordance with the practical situation in the laboratory, one of the above-
mentioned purification methods may be selected.
5.4 Reference Conditions of Instruments
5.4.1 Chromatographic reference conditions
a) Liquid phase chromatographic column: C18 column, column length: 100 mm;
internal diameter: 2.1 mm; particle size: 1.8 μm, or equivalent chromatographic
column;
b) Mobile phase: Phase-A: water; Phase-B: methanol;
c) Gradient elution conditions: 70% B (0 min ~ 5 min); 100% B (5 min ~ 8 min);
70% B (8 min ~ 12 min);
d) Flow rate: 0.2 mL/min;
e) Chromatographic column temperature: 40 °C;
f) Injection volume: 10 μL.
5.4.2 Mass spectrometry reference conditions
a) Mode of detection: multi-ion reaction monitoring (MRM);
b) Please refer to Table A.1 for mass spectrometry conditions and ion selection
parameters;
c) Please refer to Figure A.1 ~ Figure A.2 for sub-ion scan;
d) Please refer to Figure A.3 for liquid chromatography - mass spectrometry.
5.5 Draw a Standard Curve
In accordance with the sequence from low concentration to high concentration, inject
the standard series working solution into the liquid chromatograph - tandem mass
spectrometer; measure the peak area of corresponding chromatographic peak. Take
the concentration of sterigmatocystin in the standard series working solution as the x-
coordinate. Take the ratio of the peak area of sterigmatocystin chromatographic peak
and the peak area of isotope internal standard chromatographic peak as the y-
X---content of sterigmatocystin in the sample, expressed in (μg/kg);
---concentration of sterigmatocystin in the sample solution, obtained through the
standard curve, expressed in (ng/mL);
V---final constant volume, expressed in (mL);
m---weighing mass of the sample, expressed in (g);
f---dilution factor (f = 10);
The calculation result shall retain 3 significant figures.
7 Precision
The absolute difference of two independent determination results obtained under
repeatability condition shall not exceed 20% of the arithmetic mean value.
8 Others
When 5 g of rice, corn and wheat sample is weighed and taken, the detection limit is
0.6 μg/kg; the quantitation limit is 2 μg/kg. When 2 g of soy and peanut sample is
weighed and taken, the detection limit is 1.5 μg/kg; the quantitation limit is 5 μg/kg.
Method II -- Liquid Chromatography
9 Principle
Use acetonitrile - aqueous solution to extract sterigmatocystin in the sample. Through
homogenization, vortex, ultrasound and centrifugation, take the supernatant; use
phosphate buffer solution to dilute it. Use immunoaffinity column for purification and
elution. Use nitrogen to blow it to dryness and concentrate it. Use the mobile phase to
reach a constant volume. Use ...
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