GB 5009.284-2021 PDF English
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National food safety standard - Determination of vanillin, methyl vanillin, ethyl vanillin and coumarin in foods
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GB 5009.284-2021: National food safety standard - Determination of vanillin, methyl vanillin, ethyl vanillin and coumarin 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/GB5009.284-2021
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Determination of
vanillin, methyl vanillin, ethyl vanillin and coumarin in
foods
Issued on. SEPTEMBER 07, 2021
Implemented on. MARCH 07, 2022
Issued by. National Health Commission of the People's Republic of China;
State Administration for Market Regulation.
Table of Contents
1 Scope... 3
2 Principle... 3
3 Reagents and materials... 3
4 Instruments and apparatuses... 5
5 Analysis steps... 5
6 Expression of the analysis results... 7
7 Precision... 8
8 Others... 8
9 Principle... 8
10 Reagents and materials... 8
11 Instruments and apparatuses... 10
12 Analysis steps... 11
13 Expression of the analysis results... 14
14 Precision... 15
15 Others... 15
16 Principle... 15
17 Reagents and materials... 15
18 Instruments and apparatuses... 16
19 Analysis steps... 16
20 Expression of the analysis results... 19
21 Precision... 19
22 Others... 19
Appendix A Liquid chromatograms of vanillin, methyl vanillin, ethyl vanillin and
coumarin... 20
Appendix B Four compounds and corresponding deuterated isotope internal
standard liquid chromatography-mass spectrometry/mass spectrometry
characteristic ion chromatograms... 21
Appendix C Four compounds and their corresponding deuterated isotope
internal standard gas chromatography-mass spectrometry characteristic ion
scanning chromatograms and mass spectrograms... 25
National Food Safety Standard - Determination of
vanillin, methyl vanillin, ethyl vanillin and coumarin in
foods
1 Scope
This Standard specifies the determination methods of vanillin, methyl vanillin,
ethyl vanillin and coumarin in foods.
This Standard applies to the determination of vanillin, methyl vanillin, ethyl
vanillin and coumarin in infant formula, complementary foods for infants and
young children, cakes, candies, milk and dairy products, beverages, and wheat
flour.
Method I – Liquid chromatography
2 Principle
Add water to mix the sample; then, add acetonitrile for ultrasonic extraction; use
liquid chromatography for separation, ultraviolet detector or diode array
detector for detection, and external standard method for quantitation.
3 Reagents and materials
Unless otherwise specified, all the reagents in this method are analytical
reagents, the water is grade-1 water as specified in GB/T 6682.
3.1 Reagents and materials
3.2 Preparation of reagents
3.2.1 0.1% formic acid methanol solution. draw 1 mL of formic acid and dissolve
it in methanol and dilute to 1 000 mL; prepare it for immediate use.
3.2.2 Hydrochloric acid solution (1 mol/L). draw 8.33 mL of concentrated
hydrochloric acid; dissolve it in water and dilute to 100 mL; prepare it for
immediate use.
3.3 Standard substances
3.3.1 Vanillin standard substance (C8H8O3, CAS number. 121-33-5). purity
≥98%, or a standard substance that is certified by the nation and granted a
standard substance certificate.
3.4 Preparation of standard solutions
3.4.1 Standard stock solution (1 000 mg/L). accurately weigh 10 mg (accurate
to 0.1 mg) of vanillin, methyl vanillin, ethyl vanillin and coumarin; place them in
the 10 mL volumetric flasks respectively; use 0.1% formic acid methanol
solution to dissolve and dilute to the mark; mix well.
3.4.2 Standard mixed intermediate solution (10 mg/L). respectively draw 1.00
mL of standard stock solutions (1 000 mg/L) of vanillin, methyl vanillin, ethyl
vanillin and coumarin; place them in the 100 mL volumetric flasks; add 0.1%
methanol formic acid to fix volume to the mark; mix well. Transfer the solution
to a brown glass container; store at -18 °C in the dark for 3 months.
4 Instruments and apparatuses
4.1 Liquid chromatograph. equipped with diode array or UV detector.
4.2 Balance. the sensitivity is 0.1 mg and 0.01 g.
4.3 Vortex mixer.
4.6 Ultrasonic generator.
5 Analysis steps
5.1 Sample pretreatment
5.1.1 Sample preparation
Shake liquid samples well; semi-solid samples and powder samples with
uniform base materials shall be directly used for the sample extraction in 5.1.2;
other samples need to be homogenized or pulverized uniformly.
5.1.2 Sample extraction
5.1.2.1 Infant formula, complementary foods for infants and young children
Weigh 1.00 g of sample; add 10 mL of water and 480 μL of hydrochloric acid
solution; vortex for 1 min;
5.1.2.2 Cakes, candies, milk and dairy products, beverages
Weigh 1.00 g of sample; add 5 mL of water (for gum-based candy, add 10 mL
of water, and dissolve in a water bath at 50 °C); vortex for 1 min; add 20 mL of
acetonitrile; vortex for 1 min; after 30 min of ultrasonic extraction, add 5 g of
sodium chloride; vortex for 2 min;
5.2 Apparatus reference conditions
5.2.1 Chromatographic column. C18 column, 250 mm × 4.6 mm (inner diameter),
5 μm (filler particle size) or equivalent.
5.2.2 Column temperature. 30 °C.
5.2.3 Injection volume. 10 μL;
5.2.4 Detection wavelength. 279 nm.
5.2.5 Flow velocity. 1.0 mL/min.
5.3 Preparation of the standard curve
Inject the standard mixed series working solutions into the liquid chromatograph
respectively; measure the corresponding peak areas. Take the concentrations
of vanillin, methyl vanillin, ethyl vanillin and coumarin in the standard series
working solutions as the abscissa, and the peak area as the ordinate, to draw
a standard curve. For the chromatograms of standard solutions of vanillin,
methyl vanillin, ethyl vanillin and coumarin, see Figure A.1 in Appendix A.
6 Expression of the analysis results
Calculate the content of the tested compound in the sample according to
Formula (1).
7 Precision
The absolute difference of two independent test results which are obtained
under repeatability cannot exceed 15% of the arithmetic mean value.
8 Others
The detection-limit of this method is 0.07 mg/kg; the quantitation-limit is 0.20
mg/kg.
9 Principle
Add water to mix the sample well; then, use acetonitrile for ultrasonic extraction;
use the solid-phase extraction column to purify the extracting solution; then, use
liquid chromatograph-mass spectrometer/mass spectrometer for determination,
and internal standard method for quantitation.
10 Reagents and materials
Unless otherwise specified, all the reagents in this method are analytical
reagents, the water is grade-1 water as specified in GB/T 6682.
10.1 Reagents and materials
10.1.4 Sodium chloride (NaCl).
10.1.5 Concentrated hydrochloric acid (HCl). 12 mol/L.
10.1.6 Polar group-containing reverse-phase polymer solid-phase extraction
column.
10.2 Preparation of reagents
10.2.1 0.1% formic acid methanol solution. draw 1 mL of formic acid and
dissolve it in methanol and dilute to 1 000 mL; prepare it for immediate use.
10.2.2 Hydrochloric acid solution (1 mol/L). draw 8.33 mL of concentrated
hydrochloric acid; dissolve it in water and dilute to 100 mL; prepare it for
immediate use.
10.2.3 Methanol-aqueous solution (4+1). mix methanol and water at 4.1
(volume ratio) uniformly.
10.3 Standard substances
10.3.1 Vanillin standard substance (C8H8O3, CAS number. 121-33-5). purity
≥98%, or a standard substance that is certified by the nation and granted a
standard substance certificate.
10.3.6 D3-methyl vanillin standard substance (C9H7D3O3, CAS number.
143318-06-3). purity ≥98%.
10.4.4 Internal standard mixed intermediate solution (10 mg/L). draw 1.00 mL
of the standard stock solutions of D3-vanillin, D3-methyl vanillin, D5-ethyl vanillin
and D4-coumarin (1 000 mg/L) respectively; place them in the 100 mL
volumetric flasks; add 0.1% formic acid methanol solution to fix volume to the
mark; mix well. Transfer the solution to a brown glass container; store at -18 °C
in the dark for 3 months.
10.4.5 Standard and internal standard mixed series working solutions.
respectively draw 0.05 mL, 0.2 mL, 0.5 mL, 1 mL, 2 mL of the standard mixed
intermediate solution (10 mg/L) and 0.1 mL of the internal standard mixed
intermediate solution (10 mg/L); place them to in the 10 mL volumetric flasks;
add methanol-aqueous solution to the mark; mix well.
11 Instruments and apparatuses
11.1 Liquid chromatography tandem quadrupole mass spectrometer. equipped
with electrospray ionization source.
11.2 Balance. the sensitivity is 0.1 mg and 0.01 g.
11.5 High-speed refrigerated centrifuge.
11.6 Nitrogen concentrator.
11.8 Solid-phase extraction device.
12 Analysis steps
12.1 Sample pretreatment
12.1.1 Sample preparation
Shake liquid samples well; semi-solid samples and powder samples with
uniform base materials shall be directly used for sample extraction in 12.1.2;
gum-based candies shall be crushed and stirred well; other samples need to
be homogenized or crushed uniformly.
12.1.2 Sample extraction
12.2 Apparatus reference conditions
12.2.1 Liquid chromatography reference conditions
12.2.2 MS/MS reference conditions
12.2.2.1 Ionization mode. electrospray ionization, positive ion mode.
12.2.2.2 Scanning method. multiple reaction monitoring (MRM).
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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