This standard specifies the analysis method of the hygienic indicators of seafood and aquatic products. This standard is applicable to the analysis of various hygienic indicators of seafood and aquatic products. GB/T 5009.45-2003 Analysis method of hygienic standard of aquatic products GB/T5009.45-2003 Standard download decompression password: www.bzxz.net

ICS 67.040
National Standard of the People's Republic of China
GB/T5009.45—2003
Replaces GB/T5009.45—1996
Method for analysis of hygienic standard of fishand other aquatic products
Promulgated on August 11, 2003
Ministry of Health of the People's Republic of China
Standardization Administration of China
Implementation on January 1, 2004
GB/T5009.45—2003
This standard replaces GB/T5009.45—1996 "Method for analysis of hygienic standard of aquatic products". Compared with GB/T5009.45-1996, this standard has been modified as follows: The structure of the original standard has been modified in accordance with GB/T20001.4-2001 "Standard Writing Rules Part 4: Chemical Analysis Methods".
This standard is proposed and managed by the Ministry of Health of the People's Republic of China. This standard was drafted by Shanghai Food Hygiene Supervision and Inspection Institute, Jiangsu Provincial Health and Epidemic Prevention Station, Hangzhou Municipal Health and Epidemic Prevention Station, Food Hygiene Supervision and Inspection Institute of the Ministry of Health, Qinghai Provincial Health and Epidemic Prevention Station, and Fujian Provincial Health School. This standard was first issued in 1985, revised for the first time in 1996, and this is the second revision. 360
Analysis methods for sanitary standards of aquatic products
This standard specifies the analysis methods for sanitary indicators of marine products and aquatic products. This standard is applicable to the analysis of various sanitary indicators of marine products and aquatic products. The detection limit of histamine in this method is 50mg/kg.
2 Normative references
GB/T 5009.45—2003
The clauses in the following documents become the clauses of this standard through reference in this standard. For all referenced documents with dates, all subsequent amendments (excluding errata) or revisions are not applicable to this standard. However, parties that reach an agreement based on this standard are encouraged to study whether the latest versions of these documents can be used. For all referenced documents without dates, the latest versions are applicable to this standard. GB2733 Hygienic standard for fresh and frozen aquatic products of animal origin GB/T5009.11 Determination of total and inorganic arsenic in food GB/T5009.15 Determination of cadmium in food
GB/T5009.17 Determination of total mercury and organic mercury in food GB/T5009.19 Determination of 666 and DDT residues in food GB/T5009.44—2003 Analytical method for hygienic standard for meat and meat products Fresh fish
Applicable to the determination of various hygienic indicators of yellow croaker, hairtail, fish, fish, cuttlefish (squid), black carp, grass carp, silver carp, carp, scale fish, blue round (pond fish), herring, and huangyu. 3 Sensory inspection
Take the sample quantity that guarantees sensory inspection (after thawing of frozen products) and conduct sensory inspection under natural light. The results should comply with the provisions of GB2733.
Physical and chemical tests
4.1 Volatile basic ammonia nitrogen
According to 4.1 of GB/T5009.44-2003. 4.2 Mercury
According to GB/T5009.17.
4.3 Benzene hexachloride and DDT
According to GB/T5009.19.
4.4 Histamine
4.4.1 Principle
Histamine in fish is extracted with n-pentanol, and turns orange when it meets azo reagent. It is quantitatively compared with the standard series. 4.4.2 Reagents
4.4.2.1 n-pentanol.
Trichloroacetic acid solution (100g/L).
Sodium carbonate solution (50g/L).
GB/T5009.45-—2003
4.4.2.4 Sodium hydroxide solution (250g/L). 4.4.2.5 Hydrochloric acid (1+11).
4.4.2.6 Histamine standard stock solution: Accurately weigh 0.2767g of histamine phosphate dried at 100℃±5℃ for 2h, dissolve it in water, transfer it into a 100mL volumetric flask, and then dilute it to the mark with water. Each milliliter of this solution is equivalent to 1.0mg of histamine. 4.4.2.7 Histamine phosphate standard working solution: Take 1.0mL of histamine standard solution, place it in a 50mL volumetric flask, and dilute it to the mark with water. Each milliliter of this solution is equivalent to 20.0μg of histamine. 4.4.2.8 Azo reagent is as follows:
4.4.2.8.1 Liquid A: Weigh 0.5g of p-nitroaniline, add 5mL of hydrochloric acid solution to dissolve, then dilute with water to 200mL, and place in a refrigerator. 4.4.2.8.2 Liquid B: Sodium nitrite solution (5g/L), prepared before use. Take 5mL of Liquid A and 40mL of Liquid B and mix them and use immediately. 4.4.3 Analysis steps
4.4.3.1 Sample treatment
Weigh 5.00g~10.00g of the minced and mixed sample, place it in a stoppered conical flask, add 15mL~20mL of trichloroacetic acid solution (4.4.2.2), soak for 2h~3h, and filter. Pipette 2.0mL of filtrate into a separatory funnel, add sodium hydroxide solution (4.4.2.4) to make it alkaline, add 3mL of n-pentanol each time, shake for 5 minutes, extract three times, combine the n-pentanol and dilute to 10.0mL. Pipette 2.0mL of n-pentanol extract into a separatory funnel, add 3mL of hydrochloric acid (1+11) each time, shake and extract three times, combine the hydrochloric acid extract and dilute to 10.0mL for use.
4.4.3.2 Determination
Pipette 2.0mL of hydrochloric acid extract into a 10mL colorimetric tube, and separately pipette 0, 0.20, 0.40, 0.60, 0.80, 1.0ml. Histamine standard solution (equivalent to 0, 4.0, 8.0, 12, 16, 20μg histamine), respectively, into 10mL colorimetric tubes, add water to 1mL, and then add 1mL of hydrochloric acid (1+11) to each. Add 3mL sodium carbonate solution (50g/L) and 3mL azo reagent to the sample and standard tube, add water to the scale, mix well, let stand for 10min, adjust the zero point with a 1cm colorimetric cup and a zero tube, measure the absorbance at a wavelength of 480nm, draw a standard curve for comparison, or compare with the standard series by visual inspection.
4.4.4 Calculation of results
The content of histamine in the sample is calculated according to formula (1). X=
%×1000
Where:
X—the content of histamine in the sample, in milligrams per 100g (mg/100g); X100
the volume of trichloroacetic acid solution (100g/L) added, in milliliters (mL); -the mass of histamine in the sample during the determination, in micrograms (μg); mi
—the mass of the sample, in grams (g).
The calculation result is expressed to one decimal place. 4.4.5 Precision
++o+++++***(1)
The absolute difference between two independent determination results obtained under repeatability conditions shall not exceed 10% of the arithmetic mean. 4.5 Inorganic arsenicbZxz.net
According to GB/T5009.11.
4.6 Methyl mercury
According to GB/T5009.17.
According to GB/T5009.15.
Other aquatic products
GB/T 5009.45---2003
Applicable to the determination of various hygienic indicators of river shrimp and prawns, white shrimp, mantis shrimp, hawk claw shrimp and other marine shrimps and oysters (oysters, sea oysters), crabs, clams and razor clams.
5 Sensory examination
Same as Chapter 3.
6 Physical and chemical tests
6.1 Volatile basic nitrogen
Operate according to 4.1 of GB/T5009.44-2003. 6. 2 pH value-acidometer method
Applicable to oysters (oysters, oysters).
6.2.1 Principle
Use an acidometer to directly measure the pH value of the sample aqueous solution. 6.2.2 Instrument
Acidometer (accuracy above 0.050).
6.2.3 Analysis steps
Weigh 10.00g of minced sample, add freshly boiled and cooled water to 100ml, shake the hook, soak for 30min, filter or centrifuge, take about 50mL of filtrate in a 100mL beaker, and measure the pH value with an acidometer. The calculation result retains two significant figures.
6.2.4 Precision
The absolute difference between two independent determination results obtained under repeatability conditions shall not exceed 0.1 pH. 6.3 Mercury
Operate in accordance with GB/T5009.17.
6.4 BHC and DDT
Operate in accordance with GB/T5009.19.
6.5Inorganic arsenic
Operate in accordance with GB/T5009.11.
6. 6Methylmercury
Operate in accordance with GB/T5009.17.
Operate in accordance with GB/T5009.15.
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