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Basic data
| Standard ID | SN/T 5218-2019 (SN/T5218-2019) |
| Description (Translated English) | (Determination of acetylricinoleate in exported food) |
| Sector / Industry | Commodity Inspection Standard (Recommended) |
| Classification of Chinese Standard | C53 |
| Classification of International Standard | 67.050 |
| Word Count Estimation | 12,126 |
| Date of Issue | 2019 |
| Date of Implementation | 2020-07-01 |
| Issuing agency(ies) | General Administration of Customs |
SN/T 5218-2019: (Determination of acetylricinoleate in exported food)
---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Determination of methyl acetyl ricinoleate in food for export
The People's Republic of China Entry-Exit Inspection and Quarantine Industry Standards
2019-12-27 release
2020-07-01 Implementation
Issued by the General Administration of Customs of the People's Republic of China
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.
The main drafters of this standard. Qian Zhenjie, Cai Deling, Chen Jing, Feng Jiawang, Cai Qinren, Zhao Naiman.
Determination of acetyl ricinoleate in export food
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 ℃ 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 ℃ 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℃~4℃.
To be weighed and processed.
6 Measurement procedure
6.1 Extraction
Accurately weigh about 1 g of the mixed sample (accurate to 0.001 g) into a 50 mL ground glass test tube with a stopper, add 10 mL of water to the sample
Disperse the product, add sodium chloride until the water phase is saturated, add 20 mL ethyl acetate (3.1), vortex for 1 min to disperse the sample, and ultrasonically extract for 20 min.
Centrifuge at 4 000 r/min for 2 min, and collect the supernatant. Repeat the extraction once, combine the supernatants, and dilute to 50 mL with ethyl acetate (3.1).
Take an appropriate amount of the extract, place it in a refrigerated centrifuge, centrifuge at 4 000 r/min at 0 ℃ for 10 min, take the supernatant and bottle it for GC analysis.
6.2 Determination
6.2.1 Chromatographic separation conditions
6.2.1.1 Chromatographic column. HP-5 quartz capillary column, 30 m (column length) × 0.25 mm (inner diameter) × 0.25 μm (film thickness), or equivalent.
6.2.1.2 Temperature of the injection port. 250 ℃.
6.2.1.3 The carrier gas is 99.999% nitrogen, in constant flow mode, and the flow rate is 1.0 mL/min.
6.2.1.4 Detector temperature. 300 ℃.
6.2.1.5 Injection volume. 1.0 μL.
6.2.1.6 Sampling mode. splitless sampling.
6.2.1.7 According to the heating program listed in Table 1, the target analyte can be separated well.
6.2.2 Quantitative determination
Inject the standard series of working fluids into the gas chromatograph to determine the chromatographic peak area of acetyl ricinoleate.
The volume concentration is the abscissa, and the corresponding peak area is the ordinate to draw a standard curve. Inject the sample solution into the instrument to obtain acetyl castor
According to the peak area of the acid ester, the concentration of acetyl ricinoleate in the test solution is obtained according to the standard curve. If the content of the analyte in the sample exceeds the linearity
Range, use ethyl acetate (3.1) to dilute to a suitable concentration and analyze. Reference retention of methyl acetylricinoleate under the above chromatographic conditions
The time is 19.5 minutes, and the gas chromatogram of the standard working solution is shown in Figure A.1 of Appendix A.
6.2.3 Blank test
Except that no sample is added, all are carried out according to the above-mentioned measurement steps.
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
8.1 Lower limit of determination
The lower limit of gas chromatography is 250 mg/kg.
8.2 Recovery rate
For the experimental data of the concentration and recovery rate of this method, please refer to Table C.1 in Appendix C.
The second method gas chromatography-mass spectrometry
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 ℃, 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
12.1 Sample preparation
12.1.1 Liquid and semi-solid samples
Take at least the 3 smallest complete package samples of the same batch (100 mL~500 mL of mixed liquid samples, total amount of semi-solid samples
100 g~500 g), put it in a hard full glassware, mix well, and wait for the sample to be weighed.
12.1.2 Solid or powder samples
Take 500 g of a representative sample, pulverize it with a grinder, then grind it into a fine powder, mix it thoroughly, and put it into a clean glass container.
Inside the sample container, seal and mark it.
12.2 Sample storage
The powdered samples should be stored at 0 ℃~4 ℃; other samples should be frozen and stored below -18 ℃. During the sample preparation operation, avoid connecting
Contact with plastics should prevent the sample from being contaminated or the content of the test substance changed.
13 Measurement procedure
13.1 Sample handling
13.1.1 Liquid samples
Accurately weigh 5 g (accurate to 0.01 g) of a well-mixed liquid sample (if carbon dioxide is contained, remove the carbon dioxide first).
In a 25 mL ground glass test tube with a stopper, add sodium chloride until the water phase is saturated, add 5.0 mL of n-hexane, vortex for 1 min, and centrifuge at 4 000 r/min for 2
Min, collect the supernatant for GC-MS analysis.
13.1.2 Oil-free solid samples
Accurately weigh 5 g (accurate to 0.01 g) of a solid sample without grease into a 50 mL ground glass test tube with a stopper, and add 10 mL of water (depending on
Adjust the amount of water added to the sample condition), add sodium chloride until the water phase is saturated, then add 10 mL of acetonitrile, vortex for 1 min, ultrasonically extract for 20 min, separate
Heart 2 min, collect the supernatant. Repeat the extraction once and combine the supernatants. Blow the extract with nitrogen at (40±2)℃ to near dryness, and use normal hexane
Dissolve the residue with alkane, dilute to 5.00 mL, pass through an organic filter membrane for GC-MS analysis.
13.1.3...
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