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GB 5009.228-2016 (GB5009.228-2016)

GB 5009.228-2016_English: PDF (GB5009.228-2016)
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BASIC DATA
Standard ID GB 5009.228-2016 (GB5009.228-2016)
Description (Translated English) Method for analysis of hygienic standard of fish and other aquatic products
Sector / Industry National Standard
Classification of Chinese Standard C53
Word Count Estimation 10,146
Date of Issue 2016-08-31
Date of Implementation 2017-03-01
Older Standard (superseded by this standard) GB/T 5009.45-2000; SC/T 3032-2007; GB/T 5009.47-2003; GB/T 5009.45-2003; GB/T 5009.44-2003
Regulation (derived from) Announcement of the State Administration of Public Health and Family Planning 2016 No.11

Standards related to: GB 5009.228-2016

GB 5009.228-2016
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Determination of
Volatile Basic Nitrogen in Food
ISSUED ON: AUGUST 31, 2016
IMPLEMENTED ON: MARCH 01, 2017
Issued by: National Health and Family Planning Commission of the
People's Republic of China
Table of Contents
Foreword ... 4 
1 Scope ... 5 
Method One -- Semi-micro nitrogen method ... 5 
2 Principle ... 5 
3 Reagents and materials ... 5 
4 Instruments and equipment ... 6 
5 Analysis steps ... 7 
6 Expression of analysis results ... 8 
7 Precision ... 9 
Method Two -- Automatic Kjeldahl method ... 9 
8 Reagents and materials ... 9 
9 Instruments and equipment ... 10 
10 Analysis steps ... 10 
11 Expression of analysis results ... 11 
12 Precision ... 12 
Method Three -- Micro-diffusion method ... 12 
13 Principle ... 12 
14 Reagents and materials ... 12 
15 Instruments and equipment ... 13 
16 Analysis steps ... 14 
17 Expression of analysis results ... 15 
18 Precision ... 15 
19 Detection limits ... 16 
Annex A Drawing of semi-micro nitrogen distillation unit ... 17 
National Food Safety Standard - Determination of
Volatile Basic Nitrogen in Food
1 Scope
This Standard specifies determination methods for volatile basic nitrogen in
food.
This Standard is applicable to determination for volatile basic nitrogen in food
that meats are main raw materials, fresh (frozen) animal meats, meat products
and processed meat products, animal aquatic products and seafood as well as
their conditioning products, pickled egg products such as preserved egg
(century egg) and salted egg.
Method One -- Semi-micro nitrogen method
2 Principle
Volatile basic nitrogen refers to that animal food, due to action of enzymes and
bacteria, during corruption process, makes protein decompose so as to
generate basic nitrogenous substances such as ammonia and amines. Volatile
basic nitrogen is volatile. It is distilled in alkaline solution. Use boric acid solution
to absorb. Use standard acid solution to titrate and calculate content of volatile
basic nitrogen.
3 Reagents and materials
Unless otherwise stated, reagents used in this method are analytically-pure and
water is grade-three water specified in GB/T 6682.
3.1 Reagents
3.1.1 Magnesium oxide (MgO).
3.1.2 Boric acid (H3BO3).
3.1.3 Trichloroacetic acid (C2HCl3O2).
3.1.4 Hydrochloric acid (HCl) or sulfuric acid (H2SO4).
4.3 Stopper conical flask: 300 mL.
4.4 Semi-micro nitrogen determination device: as shown in Figure A.1.
4.5 Pipettes: 10.0 mL, 25.0 mL, 50.0 mL.
4.6 Microburette: 10 mL, minimum division is 0.01 mL.
5 Analysis steps
5.1 Semi-micro nitrogen determination device
According to Figure A.1, install semi-micro nitrogen determination device.
Before using, clean and check sealing of device.
5.2 Sample processing
For fresh (frozen) meat: remove skin, fat, bones, tendons; take lean portion. For
fresh (frozen) seafood and aquatic products: remove shell, skin, head, internal
organs, bone spurs; take edible portion; grind and mix well. For finished
products, directly grind and mix well. Minced meat, meat powder, dried meat
floss, fish meal, dried fish floss, liquid sample can be used directly. For pickled
eggs such as preserved egg (century egg) and salted egg, remove eggshell,
remove egg membrane; according to a ratio of egg: water = 2:1, add water; use
mixer to grind and mix well into homogenate. For fresh (frozen) sample, weigh
20 g of sample. For dried products such as meat powder, dried meat floss, fish
meal, dried fish floss, weigh 10 g of sample, to the nearest of 0.001 g. For liquid
sample, pipette 10.0 mL or 25.0 mL; place in stopper conical flask; accurately
add 100.0 mL of water; shake from time to time; sample is evenly dispersed in
sample solution; after 30 min of immersion, filter. For preserved egg sample,
salted egg sample, weigh 15 g of egg homogenate (when calculating content,
multiply egg homogenate mass by 2/3 and it shall be sample mass), to the
nearest of 0.001 g; place in stopper conical flask; accurately add 100.0 mL of
trichloroacetic acid solution; shake vigorously for 1 min; place for 15 min; after
protein is precipitated, filter. Filtrate shall be used in time. When filtrate cannot
be used in time, store in a refrigerator at 0°C~4°C for use. For special sample
that is rich in protein gelatin, that is sticky, that is not easy to filter, it may use
trichloroacetic acid solution to replace water for experiment. For sample that
there are many foams during distillation process, it may add 1~2 drops of de-
foaming silicone oil.
5.3 Determination
Add 10 mL of boric acid solution, 5 drops of mixed indicators into receiving
bottle. Insert the lower end of condenser tube into liquid surface. Accurately
pipette 10.0 mL of filtrate. Inject into reaction chamber from small glass. Use 10
V0 - total volume of sample solution, in milliliters (mL); V0 = 100 in this Method;
100 - conversion factor that is used to convert calculation results to milligrams
per hundred grams (mg/100g) or milligrams per hundred liters (mg/100mL).
The experimental results are expressed as arithmetic mean values of two
independent determination results obtained under repetitive conditions. The
result retains three significant digits.
7 Precision
The absolute difference between two independent determinations obtained
under repeatability conditions shall not exceed 10% of the arithmetic mean.
Method Two -- Automatic Kjeldahl method
8 Reagents and materials
Unless otherwise stated, reagents used in this method are analytically-pure and
water is grade-three water specified in GB/T 6682.
8.1 Reagents
8.1.1 Magnesium oxide (MgO).
8.1.2 Boric acid (H3BO3).
8.1.3 Hydrochloric acid (HCl) or sulfuric acid (H2SO4).
8.1.4 Methyl red indicator (C15H15N3O2).
8.1.5 Bromocresol green indicator (C21H14Br4O5S).
8.1.6 95% ethanol (C2H5OH).
8.2 Reagent preparation
8.2.1 Boric acid solution (20 g/L): same as 3.2.2.
8.2.2 Hydrochloric acid standard titration solution (0.1000 mol/L) or sulfuric acid
standard titration solution (0.1000 mol/L): same as 3.2.4.
8.2.3 Methyl red ethanol solution (1 g/L): same as 3.2.6.
8.2.4 Bromocresol green ethanol solution (1 g/L): same as 3.2.7.
egg, remove eggshell, remove egg membrane; according to a ratio of egg:
water = 2:1, add water; use mixer to grind and mix well into homogenate. For
preserved egg sample, salted egg sample, weigh 15 g of egg homogenate
(when calculating content, multiply egg homogenate mass by 2/3 and it shall
be sample mass). Weigh 10 g of sample for other samples, to the nearest of
0.001 g. Pipette 10.0 mL of liquid sample in distillation tube. Add 75 mL of water.
Shake to make sample evenly dispersed. Immerse 30 min.
10.3 Determination
10.3.1 Operate instrument according to requirements of instrument operating
instructions. Through cleaning, trail operation, make instrument go into normal
test running status. Perform reagent blank determination first to obtain blank
value.
10.3.2 Add 1 g of magnesium oxide into distillation tube that has been loaded
with well-processed sample. Immediately connect to distiller. According to
instrument set conditions and instrument operating instructions, start
determination.
10.3.3 When determination ends, timely clean and dredge liquid-adding line
and distillation system.
11 Expression of analysis results
The content of volatile basic nitrogen in sample is calculated according to
formula (2):
Where,
X - content of volatile basic nitrogen in sample, in milligrams per hundred grams
(mg/100g) or milligrams per hundred liters (mg/100mL);
V1 - volume of hydrochloric acid or sulfuric acid standard titration solution
consumed by testing solution, in milliliters (mL);
V2 - volume of hydrochloric acid or sulfuric acid standard titration solution
consumed by reagent blank, in milliliters (mL);
c - concentration of hydrochloric acid or sulfuric acid standard titration solution,
in Moores per liter (mol/L);
16 Analysis steps
16.1 Sample processing
For fresh (frozen) meat: remove skin, fat, bones, tendons; take lean portion. For
fresh (frozen) seafood and aquatic products: remove shell, skin, head, internal
organs, bone spurs; take edible portion; grind and mix well. For finished
products, directly grind and mix well. Minced meat, meat powder, dried meat
floss, fish meal, dried fish floss, liquid sample can be used directly. For pickled
eggs such as preserved egg (century egg) and salted egg, remove eggshell,
remove egg membrane; according to a ratio of egg: water = 2:1, add water; use
mixer to grind and mix well into homogenate. For fresh (frozen) sample, weigh
20 g of sample. For dried products such as meat powder, dried meat floss, fish
meal, dried fish floss, weigh 10 g of sample. For preserved egg sample, salted
egg sample, weigh 15 g of egg homogenate (when calculating content, multiply
egg homogenate mass by 2/3 and it shall be sample mass), to the nearest of
0.001 g. For liquid sample, pipette 10.0 mL or 25.0 mL; place in stopper conical
flask; accurately add 100.0 mL of water; shake from time to time; sample is
evenly dispersed in sample solution; after 30 min of immersion, filter. Filtrate
shall be used in time. When filtrate cannot be used in time, store in a refrigerator
at 0°C~4°C for use.
16.2 Determination
Apply water soluble glue on edges of diffuser. Add 1 mL of boric acid solution
and 1 drop of mixed indicator into central inner chamber of diffuser. In outer
chamber of diffuser, accurately add 1.0 mL of filtrate. Cover with frosted glass
cover. At notched opening of frosted glass cover and edge of diffuser, only gap
that can be inserted with pipette tip or dropper shall be saved. Through frosted
glass cover, observe whether water-soluble glue seal is tight. If there is loose
seal, it needs re-applying water soluble glue. Then from gap, quickly add 1 mL
of saturated potassium carbonate solution. Immediately flat push frosted glass
cover. Cover diffusion tight. Gently turn it on table in a circular motion way to
make sample solution and saturated potassium carbonate solution completely
mix. Place in 37°C ± 1°C incubator for 2 h. Cool to room temperature. Remove
cover. Use hydrochloric acid or sulfuric acid standard titration solution (0.0100
mol/L) to titrate. Use 1 methyl red ethanol solution and 5 bromocresol green
ethanol solution mixed indicator solutions. End color is till magenta. Use 2
methyl red ethanol solutions and 1 methylene blue ethanol solution mixed
indicator solution. End color is till blue purple. Perform reagent blank at the
same time.
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