SN/T 5218-2019Determination of acetylricinoleate in exported food (English PDF)

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009.

This standard was proposed and managed by the General Administration of Customs of the People's Republic of China.

Drafting organization of this standard. Gongbei Customs of the People's Republic of China.

1 Scope

This standard specifies the method for the determination of acetyl ricinoleate in food. The first method is gas chromatography, and the second method is gas chromatography-quality Spectrum joint usage.

The first method of this standard is suitable for the determination of acetyl ricinoleate content in gum-based candies (chewing gum, bubble gum), and the second method is suitable for fruit Determination of acetyl ricinoleate content in foods such as juice, solid beverages (malted milk extract), biscuits and edible fats and oils.

Method 1 Gas Chromatography

2 Method summary

After extraction and purification, the gum-based confectionery food is separated by gas chromatograph, and detected by a hydrogen flame ionization detector.

The retention time is qualitative, and the external standard method is quantified.

3 Reagents and materials

Unless otherwise specified, all reagents are of analytical grade (stored in glass bottles, avoid contact with plastics), and water is deionized water.

3.1 Ethyl acetate. chromatographically pure.

3.2 Anhydrous sodium sulfate (Na2SO4). Burn at 650 °C for 4 h, cool to room temperature in a desiccator, and store in a sealed bottle for later use.

3.3 Methyl acetylricinoleate. molecular formula C21H38O4, CAS number 140-03-4, purity greater than or equal to 99%.

3.4 Standard stock solution of methyl acetyl ricinoleate (1 g/L). accurately weigh 0.1 g (accurate to 0.1 mg) of methyl acetyl ricinoleate standard substance (3.3), transfer to a 100 mL volumetric flask, dilute with ethyl acetate (3.1), constant volume, and store in a refrigerator at 4 °C in the dark.

3.5 Standard working solution of methyl acetyl ricinoleate. pipette 0.50 mL, 1.00 mL, 2.00 mL, 5.00 mL, 10.00 mL and 20.00 mL standard stock solution (3.4) is placed in a 100 mL volumetric flask, diluted with ethyl acetate, and the volume is constant, and the concentration is 5 mg/L, 10 mg/L, Standard series solutions of 20 mg/L, 50 mg/L, 100 mg/L and.200 mg/L should be prepared immediately before use.

4 Apparatus and equipment

4.1 Gas chromatograph (GC) with hydrogen flame ionization detector (FID).

4.2 Analytical balance. Sensitivity 0.1 mg, 0.01 g and 0.001 g.

4.3 Nitrogen blowing instrument.

4.4 Oscillator.

4.5 Vortex mixer.

4.6 Ultrasonic extractor.

4.7 Organize the masher.

4.8 Refrigerated centrifuge. the maximum speed is not less than 4 000 r/min.

5 Preparation and storage of samples

Take at least the 3 smallest complete package samples of the same batch (the total amount of samples is about 100 g), and freeze them in liquid nitrogen for about 5 minutes.

Take it out and place it in a pulverizer immediately, take it out quickly and mix it evenly, place it in a hard all-glassware, and store it in an airtight manner at 0°C~4°C.

To be weighed and processed.

6 Measurement procedure

7 Calculation and expression of results

The content of acetyl ricinoleate in the sample is calculated according to formula (1).

Where.

X - The content of acetyl ricinoleate in the sample, in milligrams per kilogram (mg/kg);

c - The solution concentration of acetyl ricinoleate obtained from the standard curve, in milligrams per liter (mg/L);

c0-the concentration of acetyl ricinoleate in the blank sample, in milligrams per liter (mg/L);

V - The final constant volume of the sample solution, in milliliters (mL);

m-the mass of the sample, in grams (g);

K - the dilution factor.

It is expressed as the arithmetic mean of two independent determination results obtained under repeatability conditions, and the test results retain three significant digits.

8 Low limit of determination, recovery rate

9 Method summary

After solvent extraction and purification, all kinds of foods are determined by gas chromatography-mass spectrometry. Use selected ion monitoring scan mode (SIM), qualitative by retention time and abundance ratio of qualifier ions, and quantified by external standard method.

10 Reagents and materials

Unless otherwise specified, all reagents are of analytical grade (stored in glass bottles, avoid contact with plastics), and water is deionized water.

10.1 n-hexane. chromatographically pure.

10.2 Acetonitrile. chromatographically pure.

10.3 Ethanol. chromatographically pure.

10.4 Sodium chloride.

10.5 Anhydrous sodium sulfate. same as 3.2.

10.6 Methyl acetylricinoleate. molecular formula C21H38O4, CAS number 140-03-4, purity greater than or equal to 99%.

10.7 Standard stock solution of methyl acetyl ricinoleate (1 g/L). accurately weigh 0.1 g (accurate to 0.1 mg) of methyl acetyl ricinoleate standard the quality (10.6) is transferred to a 100 mL volumetric flask, diluted with n-hexane (10.1), constant volume, and stored in a refrigerator at 4 °C, protected from light.

10.8 Methyl acetyl ricinoleate standard intermediate solution (100 mg/L). Pipette 10 mL standard stock solution (10.7) into a 100 mL volumetric flask, Dilute to volume with n-hexane (10.1).

10.9 Methyl acetyl ricinoleate standard working solution. pipette 0.10 mL, 0.50 mL, 1.00 mL, 2.00 mL, 5.00 mL and 10.00 mL standard working solution (10.8) is placed in a 100 mL volumetric flask, dilute with n-hexane (10.6) to release the constant volume, that is, the concentration is 0.1 mg/L, Standard series solutions of 0.5 mg/L, 1.0 mg/L, 5.0 mg/L and 10.0 mg/L should be prepared immediately before use.

11 Apparatus and equipment

Except for gas chromatography-mass spectrometry (GC-MS), equipped with electron impact ion source (EI), the other equipment used is the same as 4.2~4.8.

12 Preparation and storage of samples

13 Measurement procedure