This standard specifies the determination method of eicosapentaenoic acid and docosahexaenoic acid in food. This standard is applicable to the determination of eicosapentaenoic acid and docosahexaenoic acid in marine fish food, fish oil products and food added with EPA and DHA. The detection limit of this method is 0.1mg/kg. GB/T 5009.168-2003 Determination of eicosapentaenoic acid and docosahexaenoic acid in food GB/T5009.168-2003 Standard download decompression password: www.bzxz.net

ICS 67. 040
National Standard of the People's Republic of China
CB/T 5009.168—2003
Determination of eicosapentaenoic acid anddocosahexaenoic acid in foods
Determination of eicosapentaenoic acid anddocosahexaenoic acid in foods2003-08-11Promulgated
Ministry of Health of the People's Republic of China
Standardization Administration of the People's Republic of China
2004-01-01Implementation
GB/T5009.168—2003
This standard is proposed and drafted by the Ministry of Health of the People's Republic of China. The responsible drafting units of this standard are Guangdong Rong Food Health Supervision and Inspection Institute, Guangdong Pharmaceutical College, and Zhoushan Health and Epidemic Prevention Station.
The main drafters of this standard are: Lei Jianzhuang, Maowei Pu, Qiu Banjian, Zai Fuyu, and Huang Lian. 1
GB/T 5009.168—2003
Fatty acids in food are very important in nutrition, and EPA and DHA, which are high in deep-sea fish oil, have the effects of improving immunity, lowering blood lipids and improving intelligence, which have been confirmed by medical experiments at home and abroad. In order to effectively monitor the popular deep-sea fish oil products and protect the interests of consumers, it is necessary to formulate national standard test methods for EPA and DHA. 2
1 Scope
GB/T5009.168—2003
The content of eicosapentaenoic acid and dicosahexaenoic acid in food
The standard stipulates the content of eicosapentaenoic acid (hereinafter referred to as EPA) and 2-hexaenoic acid (hereinafter referred to as EPA) in food.
This standard specifies the content of EPA and HC in food. Determination of the production of 1,2-pentaenoic acid and 2-dodecanoic acid in foods
The detection limit of this method is .1ug/kg
2 Principle
The oil is treated with autogenous acid to separate the fatty acids, and the long-chain fatty acids (PA and DIA) are aldehyde-treated to increase their volatility. It is proposed to use a chromatograph to effectively separate the fatty acids, and then use a chemical detector to detect the fatty acids. The external standard method is used as the basis, 3 Reagents
3.1 Hexane, pure weight:
3.2 Use: grade 1 pure:
3.32t/L To make sodium hydroxide, take 8 sodium hydroxide solution in 100g methanol, 3.420l/L hydrochloric acid methanol solution, carefully drop the concentrated solution on about 100g of sodium hydroxide, pass the generated oxidizing gas through the light, take about 470ml of methanol, convert the mass increment, adjust to 2m/. Fill the box with methanol, and keep it in the air. 3.5 C12P4, C12P6, C14S04, each 50.0, short hexane is dissolved and the volume is adjusted to 100mT. This solution is 50mgLPA and 2.50mgDHA per liter. Apparatus
4.1 The gas is equipped with a hydrogen flame ionization detector (FIT). 4.2 4.3 Oxidation system (start the end), 4.4 Scale (scale: 2m, 5mL.10l.4.5 Tissue crusher:
4.6 Mixer required.
4.7 Heat transfer
5 Sample preparation
5.1 Full fish food: rinse with vegetable water and dry: first arrange on a sieve to remove impurities and bones, then use a group period shaker to crush the mixture, drain the sentence, and crush 50g of the mixture into a 2=0mL layer of glass. Add 10CmL~2%mL petroleum resistant (rising range 50℃~50:) and fully stir, place overnight, filter the oil with oil paper, and reduce the pressure to detect half a month. After the actual fat is weighed (the increase rate can be calculated). 5.2 If the product is weighed, 10*ml of the sample is placed in a dry medium and stored in 60m Take twice (1 μl of extract at once), combine the extracts, add 70% water to 1% for later use: 5.3 Preparation: Continue to perform pre-treatment. 393
GT5009.168-2033
Analysis steps
6.3 Chemical transformation
5.1.1 Blood products and fish food: Take the fish food obtained by the treatment in 5.1 and add 10ml of n-hexane to dissolve the oil in a 10mL volumetric flask, and make up to the mark with n-hexane. Absorb 1.00ml~5.3mL of this liquid in another 10mL colorimetric medium, add 1 μl of sodium methyl ether (M+H)-1, stir thoroughly for 10min, then put it in a water container and heat for 1min-2min. After the saponification is completed, cool it down and get the methyl ester. 6.1.2 Add 2mL of hexane to the food. Divide the concentrated sample obtained by the treatment in 5.2 into 0.0 mL of hexane in two portions. Add 32.0 mL of sodium hydroxide-formaldehyde solution to the food according to 6.1.1. 6.2 Formic acidification 6.2.1 Standard solution, accurately pipette 1.0, 2.0, and 5.0 mL into 3 mL of 3.5 mL of standard solution respectively, then add 2mL of 2mL of hexane to a 50% water bath, perform formic acidization, and then discard the solution. Add 2I of boiling water to wash and remove the ice layer, drip through the liquid layer, dehydrate in another bucket without water, superheat the concentrated end with 70°C water, make up to 1ml... Wait for test on the machine. The concentration of FPA or HA in this series is 5.1.t, 2.5mg/mL, 6.2.2 Product density: 6, add 201/hydrochloric acid-ethanol solution less than 2m2 in a single product box with a thickness of less than 1ml, and operate according to the "full drug" in 5.2.1 for 10min... 6.3 Gas chromatography determination 6.3.1 Chromatographic column 1mX4nm (id), filled with 10% DECS:Chrama or DMCS 0-10 days of solvent. 6.3.2 Gas and gas flow rate: Hydrogen 50mT/min, Hydrogen 70ml/min, Air 100mL/min. 5.3.3 System temperature: Chromatographic column 18℃, Sample injection 21℃, Detector 210.5.4 Determination: 5.4.1 Preparation of standard solution: Take 3.0L of the standard solution after the treatment of 6.2.1 and inject it into the gas chromatograph to obtain the peak height of EPA and 13HA enzymes. Take the degree as the horizontal axis and the corresponding peak height response value as the axis. Plot the results. 6.4.2 1.5.0±1.0L of the sample solution after the treatment of 6.2 and inject it into the gas chromatograph to determine the qualitative analysis and quantitative analysis by comparing the measured peak height response value with the standard solution. G.5 Calculation of results 6.5.1 Marine fish (based on fat) is calculated according to formula (1): X-AXVXV 6.5.2 Intestines are calculated according to formula (2). 6.5.3 Food is calculated according to formula (3): --- the content of 22-hydroxy-2-dodecaned acid in the sample, expressed in milligrams per gram (mg/mL); --- the content of 2,000 carbon pentanoic acid or 1,2-hydroxy-2-dodecaned alcohol in the microbalanced sample solution, expressed in milligrams per liter (mg/mL): the total volume of the saponification test sample of fish and marine fish, expressed in liters (m3); 1. Sample volume of blood lake and fish samples, in liters (mL); sample set volume, in whole liters [n! 2. Sample mass, in grams ().
Calculation results are guaranteed to be two significant digits:
6.6 Precision
GB/T5009.168—2003
The difference between two independent determination results obtained under heavy conditions shall not exceed 1% of the arithmetic mean
The gaseous chromatogram of EPA private HA is shown in Figure T. bZxz.net
FPA
Di-1-dHA)
Tip: This standard content only shows part of the intercepted content of the complete standard. If you need the complete standard, please go to the top to download the complete standard document for free.