GB 5009.158-2016 PDF English
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| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivery | Name of Chinese Standard | Status |
| GB 5009.158-2016 | English | 115 |
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National food safety standard - Determination of Vitamin K1 in Foods
| Valid |
| GB/T 5009.158-2003 | English | 279 |
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3 days
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Determination of vitamin K1 in vegetables
| Obsolete |
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GB 5009.158-2016: National food safety standard - Determination of Vitamin K1 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/GB5009.158-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard -
Determination of Vitamin K1 in Foods
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;
State Food and Drug Administration of the People’s Republic
of China.
Table of Contents
Foreword... 3
1 Scope... 4
Method I High-performance Liquid Phase Chromatography - Fluorescence
Detection... 4
2 Principle... 4
3 Reagents and Materials... 4
4 Instruments and Equipment... 7
5 Analytical Procedures... 7
6 Expression of Analysis Results... 10
7 Precision... 10
8 Others... 11
Method II Liquid Phase Chromatography - Tandem Mass Spectrometry... 11
9 Principle... 11
10 Reagents and Materials... 11
11 Instruments and Equipment... 13
12 Analytical Procedures... 14
13 Expression of Analysis Results... 18
14 Precision... 18
15 Others... 18
Appendix A Methods of Correcting Vitamin K1 Standard Concentration... 19
Appendix B High-performance Liquid Phase Chromatogram... 20
Appendix C Mass Spectrometry Reference Figure... 21
Foreword
This Standard is drafted as a replacement of GB/T 5009.158-2003 “Determination of
Vitamin K1 in Vegetables” and GB 5413.10-2010 “National Food Safety Standard -
Determination of Vitamin K1 in Foods for Infants and Young Children, Milk and Milk
Products”.
In comparison with GB/T 5009.158-2003, there are several main modifications as
follows.
-- The name of this Standard is modified into “National Food Safety Standard -
Determination of Vitamin K1 in Foods”;
-- The method of high-performance liquid phase chromatography - fluorescence
detection is added;
-- The method of liquid phase chromatography - tandem mass spectrometry is
added;
-- The method of high-performance liquid phase chromatography - UV detection is
deleted.
National Food Safety Standard -
Determination of Vitamin K1 in Foods
1 Scope
This Standard specifies the method of determining vitamin K1 in foods.
In this Standard, Method I is high-performance liquid phase chromatography -
fluorescence detection, Method II is liquid phase chromatography - tandem mass
spectrometry, which are both applicable to the determination of vitamin K1 in all kinds
of formula food, vegetable oil, fruit and vegetable.
Method I -- High-performance Liquid Phase
Chromatography - Fluorescence Detection
2 Principle
Through lipase and amylase enzymolysis of samples like foods for infants and young
children, dairy products and vegetable oil, adopt N-hexane to extract vitamin K1 from
the sample. Adopt C18 liquid phase chromatographic column to separate vitamin K1
from other impurities. Adopt zinc column for reduction, adopt fluorescence detector for
detection; quantify with the external standard method.
3 Reagents and Materials
Unless otherwise indicated, the reagents adopted under this method are of analytical
purity. The water is first-grade water as specified in GB/T 6682.
3.1 Reagents
3.1.9 Glacial acetic acid (CH3COOH). chromatographic purity.
3.1.10 Zinc chloride (ZnCl2). chromatographic purity.
3.1.11 Anhydrous sodium acetate (CH3COONa).
3.1.12 Potassium hydroxide (KOH).
3.1.13 Lipase. enzyme activity≥700 U/mg.
3.2 Preparation of Reagents
3.2.1 40% potassium hydroxide solution. weigh-take 20 g of potassium hydroxide and
place it in 100 mL beaker; add 20 mL of water to dissolve it; cool it down, then, add
water to 50 mL; store in polyethylene bottle.
3.3 Standards
Vitamin K1 (C31H46O2, CAS No..84-80-0). purity≥99%, or standard substance with a
national-level certificate and a certificate of standard substance.
3.4 Preparation of Standard Solutions
3.4.1 Standard stock solution of vitamin K1 (1 mg/mL). accurately weigh-take 50 mg
(accurate to 0.1 mg) of standard vitamin K1 and place it in 50 mL volumetric flask; use
methanol to dissolve and dilute to the constant volume. Transfer the solution to a
brown glass container, store under -20 °C and keep away from light.
3.4.2 Standard intermediate fluid of vitamin K1 (100 μg/mL). accurately absorb 10.00
mL of standard stock solution of vitamin K1 and place it in 100 mL volumetric flask; add
methanol to the constant volume, mix it up. Transfer the solution to a brown glass
container, store under -20 °C and keep away from light. It can remain valid for 2
months.
3.5 Materials
3.5.1 Neutral alumina. particle size 50 μm~150μm.
3.5.2 Neutral alumina column. 2 g/6 mL, 10% of water is contained in the filling.
Commodity column can be purchased directly, or it can be replaced by filling.
3.5.3 Zinc column. length 50 mm, internal diameter 4.6 mm; zinc column can be
purchased directly, or it can be replaced by filling.
3.5.4 Microporous filter head. equipped with 0.22 μm organic microporous membrane.
4 Instruments and Equipment
4.1 High-performance liquid phase chromatograph. equipped with fluorescence detector.
4.2 Homogenizer.
4.7 pH meter. accuracy. 0.01.
4.8 Balance. division value. 1 mg and 0.1 mg.
4.9 Centrifuge. rotating speed≥6,000 r/min.
4.12 Ultrasonic oscillator.
5 Analytical Procedures
5.1 Preparation of Samples
After mixing powdered samples like rice flour and flour, directly take the sample; use
sample grinder to grind flaky and granular samples into powder, store it in a sample
bag for later usage;
5.2 Processing of Samples
Note. during the processing, avoid direct UV light irradiation, keep away from light.
5.2.1 Foods for infants and young children, dairy products and vegetable oil
5.2.2 Fruit and vegetable
5.2.2.1 Extraction
Accurately weigh-take 1 g~5 g (accurate to 0.01 g, the content of vitamin K1 shall be
≥0.05 μg) of homogenized sample, place it in 50 mL centrifuge tube. Add 5 mL of
isopropanol, start vortex for 1 min and ultrasonic for 5 min. Add 10 mL of N-hexane,
start vortex or oscillation extraction for 3 min, start centrifugation at 6,000 r/min for 5
min. Remove-take the supernatant in 25 mL brown volumetric flask.
5.2.2.2 Purification and concentration
Use a small amount of N-hexane to transfer 1 mL of the above-mentioned extract to
neutral alumina column that’s previously activated with 5 mL of N-hexane. Wait till the
extract is almost drained, use 5 mL of N-hexane to rinse it; use 6 mL of N-hexane -
ethyl acetate mixed solution to elute to 10 mL tube.
5.3 Chromatography Reference Conditions
5.4 Draw a Standard Curve Line
Adopt the external standard curve line to quantify. Respectively inject the standard
series of working fluid of vitamin K1 into high-performance liquid phase
chromatograph, determine the corresponding peak area.
5.5 Determination of Sample Solution
Under the same chromatographic conditions, respectively inject the prepared blank
solution and sample solution for high-performance liquid phase chromatographic
analysis.
6 Expression of Analysis Results
The content of vitamin K1 in the sample shall be calculated in accordance with
Formula (1).
7 Precision
The absolute difference between the two independent determination results obtained
under repeatability conditions shall not exceed 10% of the arithmetic mean value.
8 Others
Foods for infants and young children, dairy products and vegetable oil. when the
amount of sampling is 1 g and the constant volume is 5 mL, the detection limit is 1.5
μg/100 g and the quantitation limit is 5 μg/100 g;
9 Principle
Through lipase and amylase enzymolysis of samples like foods for infants and young
children, dairy products and vegetable oil, adopt N-hexane to extract vitamin K1 from
the sample. Adopt C18 liquid phase chromatographic column to separate vitamin K1
from other impurities. Adopt tandem mass spectrometry for detection; quantify with
the isotope-labeled internal standard method.
10 Reagents and Materials
Unless otherwise indicated, the reagents adopted under this method are of analytical
purity. The water is first-grade water as specified in GB/T 6682.
10.1 Reagents
10.1.8 Methanol (CH3OH). chromatographic purity.
10.1.9 Ethyl acetate (C4H8O2).
10.2 Preparation of Reagents
10.2.1 40% potassium hydroxide solution. weigh-take 20 g of potassium hydroxide
and place it in 100 mL beaker; add 20 mL of water to dissolve it; cool it down, then,
add water to 50 mL; store in polyethylene bottle.
10.3 Standards
10.3.1 Vitamin K1 (C31H46O2, CAS No..84-80-0). purity≥99.3%.
10.3.2 Vitamin K1-D7 (C31H46O2, CAS No..1233937-39-7). purity≥99.5%.
10.4 Preparation of Standard Solutions
10.4.1 Standard stock solution of vitamin K1 (1 mg/mL). accurately weigh-take 50 mg
(accurate to 0.1 mg) of standard vitamin K1 and place it in 50 mL volumetric flask; use
methanol to dissolve and dilute to the constant volume. Transfer the solution to a
brown glass container, store under -20 °C and keep away from light.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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