GB 5009.293-2023 PDF English
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National food safety standard - Determination of monocaprylin in foods
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GB 5009.293-2023: National food safety standard - Determination of monocaprylin 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/GB5009.293-2023
GB
NATIONAL STANDARD OF THE
PEOPLE'S REPUBLIC OF CHINA
National food safety standard - Determination of capryl
monoglyceride in food
ISSUED ON: SEPTEMBER 6, 2023
IMPLEMENTED ON: MARCH 6, 2024
Issued by: National Health Commission of the People's Republic of China;
State Administration for Market Regulation.
Table of Contents
1 Scope ... 3
Method A - Gas chromatography ... 3
2 Principles ... 3
3 Reagents and materials ... 3
4 Instruments and equipment ... 4
5 Analysis steps ... 5
6 Result calculation ... 7
7 Precision ... 7
8 Others ... 8
Method B - Gas chromatography-mass spectrometry ... 8
9 Principles ... 8
10 Reagents and materials ... 8
11 Instruments and equipment ... 9
12 Analysis steps ... 9
13 Result calculation ... 11
14 Precision ... 11
15 Others ... 11
Appendix A Gel permeation chromatography reference analysis conditions ... 12
Appendix B Gas chromatogram and gas chromatography-mass spectrometry selected
ion monitoring (SIM) chromatogram of capryl monoglyceride standard solution ... 13
Appendix C Monitoring ions and relative abundance of capryl monoglyceride ... 15
National food safety standard - Determination of capryl
monoglyceride in food
1 Scope
This standard specifies the gas chromatography and gas chromatography-mass
spectrometry methods for the determination of capryl monoglyceride in food.
This standard is applicable to the determination of capryl monoglyceride in wet flour
products, pastries, baked food fillings and surface paste (only bean paste), meat
sausages, and spicy strips.
Method A - Gas chromatography
2 Principles
Capryl monoglyceride in wet flour products is extracted with n-hexane saturated
acetonitrile, degreased with acetonitrile-saturated n-hexane, measured by gas
chromatography, qualitatively analyzed according to retention time, and quantitatively
analyzed with the external standard method.
Capryl monoglyceride in bean paste, pastries, meat sausages and spicy strips is
extracted with n-hexane saturated acetonitrile, purified by gel permeation
chromatography, and measured by gas chromatography, qualitatively analyzed
according to retention time, and quantitatively analyzed with external standard method.
3 Reagents and materials
Unless otherwise stated, the reagents used in this method are all chromatographically
pure, and the water is first-grade water specified in GB/T 6682.
3.1 Reagents
3.1.1 Absolute ethanol (C2H6O), chromatographically pure.
3.1.2 Acetonitrile (CH3CN), chromatographically pure.
3.1.3 n-Hexane (C6H14), chromatographically pure.
3.1.4 Ethyl acetate (CH3COOC2H5), chromatographically pure.
3.1.5 Cyclohexane (C6H12), chromatographically pure.
3.2 Reagent preparation
3.2.1 n-hexane saturated acetonitrile, acetonitrile-saturated n-hexane: Measure 100 mL
of acetonitrile (3.1.2) into a 250 mL separatory funnel, add 100 mL of n-hexane, shake
vigorously for several minutes, and let it stand; after it separates into layers, take the
lower layer, then the n-hexane saturated acetonitrile solution is obtained; take the upper
layer, then the acetonitrile-saturated n-hexane solution is obtained.
3.2.2 Ethyl acetate-cyclohexane (1+1): Mix ethyl acetate and cyclohexane in a volume
ratio of 1:1.
3.3 Standards
Capryl monoglyceride standard (capryl monoglyceride, C11H22O4, CAS number:
26402-26-6) with a purity of ≥98%, or a standard with national authentication and a
Reference Material Certificate.
3.4 Preparation of standard solution
3.4.1 Capryl monoglyceride standard stock solution (10.0 mg/mL): Accurately weigh
0.1 g (accurate to 0.0001 g) of standard capryl monoglyceride in a 10 mL volumetric
flask, dissolve it in absolute ethanol, dilute to the mark, and mix well. Transfer the
solution to a brown glass bottle and store it at -20 °C. It will be valid for 6 months.
3.4.2 Capryl monoglyceride standard intermediate solution (1.0 mg/mL): Take 1 mL of
capryl monoglyceride standard stock solution (10.0 mg/mL) into a 10 mL volumetric
flask, dilute to volume with absolute ethanol, and mix well. Prepare it fresh just before
use.
3.4.3 Capryl monoglyceride standard series working solution: Take 20 μL, 50 μL of
capryl monoglyceride standard intermediate solution (1.0 mg/mL), and 10 μL, 20 μL,
50 μL and 100 μL of capryl monoglyceride standard stock solution (10.0 mg/mL)
respectively; use absolute ethanol to prepare capryl monoglyceride standard series
working solutions with concentrations of 0.0200 mg/mL, 0.0500 mg/mL, 0.100 mg/mL,
0.200 mg/mL, 0.500 mg/mL, and 1.00 mg/mL, respectively. Prepare the solutions fresh
just before use.
4 Instruments and equipment
4.1 Gas chromatograph (GC): with flame ionization detector (FID).
at 30 °C to 40 °C until nearly dry; dilute to 2 mL with absolute ethanol, and pass through
a 0.22 μm organic filter membrane, for gas chromatography determination later.
5.1.3.2 Bean paste, pastries, meat sausages and spicy strips
Transfer bean paste, pastry, meat sausage, and spicy strip concentrate processed in 5.1.2
to a 10 mL volumetric flask, wash the eggplant-shaped evaporation flask twice with 6
mL of ethyl acetate-cyclohexane (3 mL each time), and combine the washing liquid into
the same 10 mL volumetric flask; dilute to the mark with ethyl acetate-cyclohexane
(1+1), and filter with a 0.22 μm organic filter membrane. After the filtrate is purified
by gel permeation chromatography, collect the eluate (for gel permeation
chromatography conditions, please refer to Appendix A), rotary evaporate at
30 °C~40 °C until almost dry, dilute to 1 mL with absolute ethanol, and pass through a
0.22 μm organic filter membrane, for gas chromatography determination later.
5.2 Instrument reference conditions
The reference conditions for gas chromatography are as follows:
a) Chromatographic column: (35%-phenyl)-methylpolysiloxane capillary
column, 30 m×0.25 mm (inner diameter) ×0.25 μm (film thickness), or
equivalent.
b) Temperature programming: The initial temperature is 60 °C, and hold for 1
minute; increase temperature to 340 °C at 20 °C/min, and hold for 5 minutes.
c) Inlet temperature: 340 °C.
d) Detector temperature: 340 ℃, with a hydrogen flow of 30 mL/min, an air flow
of 400 mL/min, and a makeup flow of 30 mL/min.
e) Carrier gas: nitrogen with a purity of ≥99.999%, constant flow mode, and flow
rate of 1.0 mL/min.
f) Injection method: Splitless injection; open the valve after 0.5 minutes.
g) Injection volume: 1.0 μL.
5.3 Preparation of standard curve
Inject the capryl monoglyceride standard series working solutions into the gas
chromatograph respectively, and measure the corresponding peak area of capryl
monoglyceride. Take the concentration of capryl monoglyceride in the standard
working solution as the abscissa, the peak area of capryl monoglyceride as ordinate,
and draw the standard curve. For the chromatogram of the capryl monoglyceride
standard solution, see Figure B.1 in Appendix B.
8 Others
The detection limit of this method is 0.050 g/kg, and the quantitation limit is 0.10 g/kg.
Method B - Gas chromatography-mass spectrometry
9 Principles
Capryl monoglyceride in wet flour products is extracted with n-hexane saturated
acetonitrile, degreased with acetonitrile-saturated n-hexane, and measured with gas
chromatography-mass spectrometry; the selected ion monitoring mode (SIM) is used,
the qualitative analysis is carried out according to the retention time and the abundance
ratio of qualitative ion fragments, and external standard method is used for quantitative
analysis.
Capryl monoglyceride in bean paste, pastries, meat sausages and spicy strips is
extracted with n-hexane saturated acetonitrile, purified with gel permeation
chromatography, and measured with gas chromatography-mass spectrometry; the
selected ion monitoring mode (SIM) is used, the qualitative analysis is carried out
according to the retention time and the abundance ratio of qualitative ion fragments,
and external standard method is used for quantitative analysis.
10 Reagents and materials
10.1 Reagents
Same as 3.1.
10.2 Reagent preparation
Same as 3.2.
10.3 Standards
Same as 3.3.
10.4 Preparation of standard solution
10.4.1 Capryl monoglyceride standard stock solution (10.0 mg/mL): Same as 3.4.1.
10.4.2 Capryl monoglyceride standard intermediate solution (1.0 mg/mL): Same as
3.4.2.
10.4.3 Capryl monoglyceride standard series working solution: Take 20 μL, 50 μL of
capryl monoglyceride standard intermediate solution (1.0 mg/mL) and 10 μL, 20 μL,
50 μL and 100 μL of capryl monoglyceride standard stock solution (10.0 mg/mL)
respectively, and prepare capryl monoglyceride matrix standard solutions with the
concentrations of 0.0200 mg/mL, 0.0500 mg/mL, 0.100 mg/mL, 0.200 mg/mL, 0.500
mg/mL, and 1.00 mg/mL, respectively. Prepare the solutions fresh just before use.
11 Instruments and equipment
11.1 Gas chromatography-mass spectrometer (GC-MS): equipped with electron impact
ion source (EI).
11.2 Gel permeation chromatograph (GPC): See Appendix A for relevant parameters.
11.3 Electronic balance: The sensitivity is 0.1 mg and 0.01 g, respectively.
11.4 Vortex mixer.
11.5 Centrifuge.
11.6 Rotary evaporator.
11.7 Nitrogen blower.
11.8 Microporous filter membrane (organic phase): 0.22 μm.
11.9 Ultrasonic generator: The power is 185 W.
12 Analysis steps
12.1 Sample pretreatment
It is the same as 5.1, for gas chromatography-mass spectrometry measurement.
12.2 Gas chromatography reference conditions
12.2.1 Chromatographic column: (35%-phenyl)-methylpolysiloxane capillary column,
30 m×0.25 mm (inner diameter) ×0.25 μm (film thickness), or equivalent.
12.2.2 Temperature programming: The initial temperature is 60 °C, and hold for 1
minute; increase temperature to 340 °C at 20 °C/min, and hold for 5 minutes.
12.2.3 Inlet temperature: 340 ℃.
12.2.4 Carrier gas: helium with a purity of ≥99.999%, constant flow mode, and flow
rate of 1.0 mL/min.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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