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GB 5009.9-2016

Chinese Standard: 'GB 5009.9-2016'
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BASIC DATA
Standard ID GB 5009.9-2016 (GB5009.9-2016)
Description (Translated English) Determination of starch in foods
Sector / Industry National Standard
Classification of Chinese Standard X09
Date of Issue 2016-12-23
Date of Implementation 2017-06-23
Older Standard (superseded by this standard) GB/T 5009.9-2008; GB/T 5514-2008; GB/T 9695.14-2008
Regulation (derived from) National Health and Family Planning Commission Notice No.17 of 2016

GB 5009.9-2016
GB
NATIONAL STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
National food safety standard -
Determination of starch in foods
食品安全国家标准
食品中淀粉的测定
ISSUED ON. DECEMBER 23, 2016
IMPLEMENTED ON. JUNE 23, 2017
Issued by. National Health and Family Planning Commission of the PRC;
State Food and Drug Administration
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Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Principles ... 4 
3 Reagents and materials ... 4 
4 Instruments and equipment ... 6 
5 Analytical procedures ... 6 
6 Expression of analytical results ... 9 
7 Precision... 11 
8 Principles ... 11 
9 Reagents and materials ... 12 
10 Instruments and equipment ... 13 
11 Analytical procedures ... 13 
12 Expression of analytical results ... 14 
13 Precision ... 15 
14 Principles ... 15 
15 Reagents and materials... 15 
16 Instruments and equipment ... 17 
17 Analytical procedures ... 17 
18 Expression of analytical results ... 19 
19 Precision ... 21 
Foreword
The standard replaces GB/T 5009.9-2008 “Determination of starch in food”,
GB/T 5514-2008 “Inspection of grain and oils – Determination of starch content
in grain and oilseeds”, and GB/T 9695.14-2008 “Meat products –
Determination of starch content”.
As compared with GB/T 5009.9-2008, the main changes of this standard are
as follows.
- ADD the determination operation of low content sample;
- ADD the determination of reagent blank;
- MODIFY the calculation formula in the method 1;
- ADD the method 3. Determination of starch content in meat products.
National food safety standard
Determination of starch in foods
1 Scope
This standard specifies the determination of starch in food.
The method 1 and the method 2 of this standard apply to the determination of
starch in food (except for meat products); the method 3 is applicable to the
determination of starch in meat products, BUT it does not apply to the
determination of starch in other additions which contains both the hydrolyzed
and the reducing sugar.
Method 1. Enzymatic hydrolysis
2 Principles
After removing the fat and soluble sugar from the sample, the starch is
hydrolyzed by amylase into small molecules, which is further hydrolyzed by
hydrochloric acid into monosaccharides AND determined as reducing sugar,
AND the result is converted into the starch content.
3 Reagents and materials
Unless otherwise stated, the reagents used in this method are of analytical
pure AND water is the level 3 water as specified in GB/T 6682.
3.1 Reagents
3.1.1 Iodine (I2).
3.1.2 Potassium iodide (KI).
3.1.3 Taka-diastase amylase. enzyme activity ≥ 1.6 U/mg.
3.1.4 Anhydrous ethanol (C2H5OH) or 95% ethanol.
3.1.5 Petroleum ether. boiling range of 60 °C ~ 90 °C.
3.1.6 Ether (C4H10O).
3.1.7 Toluene (C7H8).
3.1.8 Trichloromethane (CHCl3).
3.1.9 Hydrochloric acid (HCl).
3.1.10 Sodium hydroxide (NaOH).
3.1.11 Copper sulfate (CuSO4 • 5H2O).
3.1.12 Potassium tartrate (C4H4O6KNa • 4H2O).
3.1.13 Potassium ferrocyanide [K4Fe(CN)6 • 3H2O].
3.1.14 Methylene blue (C16H18ClN3S • 3H2O). indicator.
3.1.15 Methyl red (C15H15N3O2). indicator.
3.1.16 Glucose (C6H12O6).
3.2 Reagent preparation
3.2.1 Methyl red indicator solution (2 g/L). WEIGH 0.20 g of methyl red; USE a
small amount of ethanol to dissolve it; ADD water to make its volume reach to
100 mL.
3.2.2 Hydrochloric acid solution (1 + 1). MEASURE 50 mL of hydrochloric acid;
MIX it with 50 mL of water.
3.2.3 Sodium hydroxide solution (200 g/L). WEIGH 20 g of sodium hydroxide;
ADD water to dissolve and make its volume reach to 100 mL.
3.2.4 Alkaline tartrate solution A. WEIGH 15 g of copper sulfate and 0.050 g of
methylene blue; DISSOLVE it into water; MAKE its volume reach to 1000 mL.
3.2.5 Alkaline copper tartrate solution B. WEIGH 50 g of sodium potassium
tartrate and 75 g of sodium hydroxide; DISSOLVE it in water; ADD 4 g of
potassium ferrocyanide; after it is completely dissolved; USE water to make its
volume reach to 1000 mL; STORE it in a glass bottle with rubber stopper.
3.2.6 Amylase solution (5 g/L). WEIGH 0.5 g of Taka-diastase amylase; ADD
100 mL of water to dissolve it; PREPARE it before use; AND it may also add
several drops of toluene or chloroform to prevent mildew; PRESERVE it in
refrigerator at 4 °C.
Note. It may also use the aforementioned method to calibrate 4 mL ~ 20 mL of
alkaline copper tartrate solution (50% of solution A and 50% of solution B) to
adapt to the change of concentration of the reducing sugar in the sample.
5.2.2 Sample solution prediction
PIPETTE 5.00 mL of alkaline copper tartrate solution A and 5.00 mL of alkaline
copper tartrate solution B; PLACE it in a 150 mL conical flask; ADD 10 mL of
water; ADD two glass beads; HEAT to boil it within 2 min; MAINTAIN boiling; at
the speed from fast to slow, USE the burette to add the sample solution;
MAINTAIN the solution at boiling state; when the solution color becomes light,
TITRATE it at the rate of one drop every two seconds, until the blue color of the
solution disappears; RECORD the volume of the sample solution consumed.
When the glucose concentration in the sample solution is to high, it shall make
formal determination after appropriate dilution, so as to ensure that the volume
of the sample solution consumed for each titration is controlled close to the
volume of the glucose standard solution as consumed in calibrating the
alkaline copper tartrate solution, which is about 10 mL.
5.2.3 Determination of sample solution
PIPETTE 5.00 mL of alkaline copper tartrate solution A and 5.00 mL of alkaline
copper tartrate solution B; PLACE it in a 150 mL conical flask; ADD 10 mL of
water; ADD two glass beads; USE the burette to add the sample solution which
is 1 mL less than the predicted volume into the conical flask; HEAT to boil it
within 2 min; MAINTAIN the solution at boiling state; CONTINUE adding
glucose at the rate of one drop per two seconds, until the blue color of the
solution just disappears; RECORD the total volume of the sample solution as
consumed; and meanwhile MAKE three parallels; TAKE the average value;
MAKE calculation in accordance with the formula (1).
When the concentration is too low, then directly ADD 10.00 mL of sample
solution; DO not add 10 mL of water; USE the glucose standard solution to
make titration to the end; RECORD the glucose content (mg) in 10 mL of
sample solution which is equivalent to the difference of volume as consumed
and the volume of the glucose standard solution as consumed during
calibration. MAKE calculation in accordance with the formula (2) and (3).
5.2.4 Determination of reagent blank
Meanwhile, MEASURE 20.00 mL of water and the amylase solution having an
amount same as that used for sample solution treatment; USE the reverse
dropping method to make reagent blank test. That is, USE the glucose
standard solution to titrate the reagent blank solution to the end. RECORD the
glucose content (mg) in 10 mL of sample solution which is equivalent to the
100 - Constant volume of the sample to be measured (mL);
V0 - The volume of glucose standard solution consumed after the addition of
the blank sample, in milliliters (mL);
Vs - The volume o......
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