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GB 5413.23-2010: National food safety standard -- Determination of iodine in foods for infants and young children, milk and milk products
Status: Obsolete GB 5413.23: Evolution and historical versions
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| GB 5413.23-2010 | English | 239 |
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National food safety standard -- Determination of iodine in foods for infants and young children, milk and milk products
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GB 5413.23-2010
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| GB/T 5413.23-1997 | English | 199 |
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Milk powder and formula foods for infant and young children--Determination of iodine content
| Obsolete |
GB/T 5413.23-1997
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PDF similar to GB 5413.23-2010
Basic data | Standard ID | GB 5413.23-2010 (GB5413.23-2010) | | Description (Translated English) | National food safety standard -- Determination of iodine in foods for infants and young children, milk and milk products | | Sector / Industry | National Standard | | Classification of Chinese Standard | C53;X82 | | Classification of International Standard | 67.100.10 | | Word Count Estimation | 6,648 | | Date of Issue | 2010-03-26 | | Date of Implementation | 2010-06-01 | | Older Standard (superseded by this standard) | GB/T 5413.23-1997 | | Regulation (derived from) | Circular of the Ministry of Health (2010)7 | | Issuing agency(ies) | Ministry of Health of the People's Republic of China | | Summary | This Chinese standard specifies the infant foods and milk products Determination of iodine. This standard applies to infant foods and milk products Determination of iodine. | GB 5413.23-2010: National food safety standard -- Determination of iodine in foods for infants and young children, milk and milk products
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National food safety standard.Determination of iodine in foods for infants and young children, milk and milk products
National Standards of People's Republic of China
People's Republic of China Ministry of Health issued
Issued on. 2010-03-26
2010-06-01 implementation
National Food Safety Standard
Determination of infant foods and dairy iodine
National food safety standard
Determination of iodine in foods for infants and young children,
milk and milk products
Foreword
This standard replaces GB/T 5413.23-1997 "infant formula and milk powder Determination of Iodine"
This standard compared with GB/T 5413.23-1997, main changes are as follows.
- To fill the column quartz capillary column;
- Increase the detection limit.
Appendix A of this standard is an informative annex.
This standard replaces the standards previously issued as follows.
--GB 5413-1985, GB/T 5413.23-1997.
National Food Safety Standard
Determination of infant foods and dairy iodine
1 Scope
This standard specifies the method for determination of infant foods and dairy iodine.
This standard applies to the determination of infant foods and dairy iodine.
2 Normative references
The standard file referenced in the application of this standard is essential. For dated references, only the edition date of the note
Apply to this standard. For undated references, the latest edition (including any amendments) applies to this standard.
Principle 3
Iodine in the sample under conditions of sulfuric acid and iodine derivatives generate butanone and butanone reacted by gas chromatography with electron capture detector inspection
Testing, external standard.
4 Reagents and materials
Unless otherwise specified, the reagents used in this method are analytically pure water GB/T 6682 provided a water.
4.1 Peak's (Taka-Diastase) amylase. enzyme activity ≥1.5 U/mg.
4.2 potassium iodide (KI) or potassium iodate (KIO3). pure class distinctions.
4.3 butanone (C4H8O). chromatography.
4.4 sulfuric acid (H2SO4). pure class distinctions.
4.5 n-hexane (C6H14).
4.6 anhydrous sodium sulfate (Na2SO4).
4.7 Hydrogen peroxide (3.5%). lessons 11.7 mL volume fraction of 30% hydrogen peroxide diluted to 100 mL.
4.8 potassium ferrocyanide solution (109 g/L). Weigh 109 g of potassium ferrocyanide, water volume to 1000 mL volumetric flask.
4.9 zinc acetate solution (219 g/L). Weigh 219 g of zinc acetate, water volume to 1000 mL volumetric flask.
4.10 iodine standard solution.
4.10.1 iodine standard stock solution (1.0 mg/mL). Weigh 131 mg of potassium iodide (4.2) (accurate to 0.1 mg) or 168.5 mg potassium iodate
(4.2) (accurate to 0.1 mg), dissolved in water and dilute to 100 mL, 5 ℃ ± 1 ℃ refrigerated within a week effective.
4.10.2 iodine standard working solution (1.0 μg/mL). draw 10 mL standard stock solution of iodine, water volume to 100 mL and mix, then draw
1.0 mL, 100 mL water to the mix, prepared before use.
5. Apparatus
5.1 Balance. a sense of the amount of 0.1 mg.
5.2 Gas chromatography with electron capture detector.
Step 6 Analysis
6.1 Sample Processing
6.1.1 Starch-free sample
Weigh mixed solid sample 5 g, liquid sample 20 g (accurate to 0.0001 g) in 150 mL Erlenmeyer flask, with a solid sample
25 mL of hot water about 40 ℃ dissolved.
6.1.2 sample containing starch
Weigh mixed solid sample 5 g, liquid sample 20 g (accurate to 0.0001 g), in 150 mL flask was added 0.2 g
Peak's amylase (4.1), solid sample with 25 mL of hot water about 40 ℃ fully dissolved, placed in 50 ℃ ~ 60 ℃ incubator hydrolysis 30 min,
Remove to cool.
6.2 Preparation of sample measurement solution
6.2.1 precipitate. the processed sample solution transferred to 100 mL volumetric flask, add 5 mL potassium ferrocyanide solution (4.8) and 5
mL zinc acetate solution (4.9), the water volume to the mark still shaken after 10 min. After the filter paper to absorb the filtrate 10 mL
100 mL separating funnel, add 10 mL of water.
6.2.2 Derivatives and extraction. separating funnel was added to 0.7 mL of sulfuric acid (4.4), 0.5 mL butanone (4.3), 2.0 mL of hydrogen peroxide (4.7),
Mix well, kept at room temperature for 20 min was added 20 mL of n-hexane (4.5) oscillation was extracted 2 min. After resting stratification, the aqueous phase shifted
Another separatory funnel, and then a second extraction. The combined organic phase was washed with water two or three times. Dehydrated over anhydrous sodium sulfate and filtered shift
Into 50mL volumetric flask with normal hexane, this is the sample measurement solution.
6.3 Preparation of standard iodine solution Determination
Pipette 1.0 mL, 2.0 mL, 4.0 mL, 8.0 mL, 12.0 mL iodine standard working solution (4.10.2), equivalent to 1.0 μg, 2.0 μg,
4.0 μg, 8.0 μg, 12.0 μg of iodine, other analytical step with 6.2.
6.4 Determination
6.4.1 Reference chromatographic conditions
Column. filler is 5% cyanopropyl - methyl silicone capillary column (column length 30 m, an inner diameter of 0.25 mm, film thickness 0.25 μm)
Or equivalent performance of the column.
Inlet temperature. 260 ℃.
ECD detector temperature. 300 ℃.
Split ratio. 1. 1.
Injection volume. 1.0 μL.
Temperature program shown in Table 1.
Table 1 temperature program
Heating rate (/ min ℃) Temperature (℃) Duration (min)
6.4.2 standard curve
Determination of the iodine standard solution (6.3) were injected into a gas chromatograph (chromatogram see Appendix A) to give a peak area standard assay solution
(Or peak height). In the standard assay solution peak area (or peak height) for the vertical axis, to the quality of (6.3) standard working solution of iodine in iodine as the horizontal
Standard curve.
6.4.3 Determination of sample solution
Determination of the sample solution (6.2) is injected into the gas chromatograph to obtain the peak area (or peak height), to obtain a sample from the standard curve of iodine-containing
The amount (μg).
7 expression analysis
The iodine content of the sample according to equation (1).
100 × =
CX s (1)
Where.
X-- sample iodine content in micrograms per hundred grams (μg/100 g);
Cs-- iodine content in the sample obtained from the standard curve, in micrograms (μg);
m-- sample mass, in grams (g).
The arithmetic mean of two under the same condition of independent determination results indicated that the results of reservations to one decimal place.
8 Precision
Two independent determination results under the absolute difference in repetition condition must not exceed 10% of the arithmetic mean.
9 Other
The standard detection limit of 2.0 μg/100 g.
Appendix A
(Informative)
Iodine standard derivative gas chromatogram
A.1 iodine standard derivative gas chromatogram
Iodine standard derivative gas chromatography is shown in Figure A.1.
Figure A.1 iodine standard derivative gas chromatogram
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