Scope of application
This standard specifies the gas chromatography-mass spectrometry method for the determination of urethane content in beer, wine, rice wine, liquor and other alcohol and soy sauce.
This standard is applicable to the determination of urethane content in beer, wine, rice wine, liquor and other alcoholic beverages and soy sauce.
Reference standard: “GB 5009·223-2014 Determination of urethane in food”.
Sample preparation
Shake the sample well, weigh 2g (accurate to 0.001g) liquor sample, add 100.0μL 1.0μg/mL urethane working solution, 0.3g sodium chloride, ultrasonically dissolve and mix.
SPE purification steps
SPE column: Welchrom® Celite AZO, size: 2g/12mL
Loading: all the sample solution is loaded, and let stand for 10min
Rinse: 10mL n-hexane, discard
Elution: 15 mL of 5% ethyl acetate-diethyl ether solution, pressed to dryness, received
The eluate was dehydrated by a glass funnel filled with 2g of anhydrous sodium sulfate, collected in a 15mL scale test tube, blown slowly with nitrogen at room temperature to about 0.5mL, and made up to 1.0mL with methanol to make a measurement solution for use. GC/Ms analysis.
Chromatographic conditions
Gas chromatography conditions
Chromatographic column: WM-InoWAX, 30m×0.25mm×0.25μm.
Inlet temperature: 250℃
Heating program: 50°C, hold for 1min, heat up to 180°C at 8°C/min, then run for 5min at 240°C/min
Carrier gas: high purity helium (purity >99.999%)
Injection method: splitless injection
Constant flow mode: 1.0mL/min
Injection volume: 1 μL
MS conditions
Ionization method: Electron bombardment ionization source (EI)
Ionization energy: 70eV
Transfer line temperature: 250℃
Ion source temperature: 230℃
Quadrupole temperature: 150℃
Monitoring method: urethane selected monitoring ions: 44, 62, 74, 89, quantitative ion 62
Solvent delay: 8min
Chromatogram or Spike Recovery Results
Sample spiked 0.05mg/kg recovery table
| Ssubstance | The average recovery rate% | Rsd(N=2)% | |
| Ethyl carbamate | 88.23 | 1.43 |
Related product information
| P/N | Name | Specification |
| 00567-20008 | SPE cartridge | Welchrom®Celite AZO，2g/12mL，20pk |
| 00837-05003 | Centrifuge tube | Welchrom® Disposable Centrifuge Tubes, Conical Bottom, RCF12000xg, Bag, Sterilized, 15mL, 25/pk |
| 00837-05002 | 15mL screw top centrifuge tube | Welchrom® Disposable Centrifuge Tubes, Flat Cap, Conical Bottom, RCF12000xg, Bag, Non-sterile, 15mL, 50/pk |
| 00824-31001 | Solid phase extraction device | Welch Solid Phase Extraction Unit, 12-Position Square Cylinder |
| 00821-32291 | Cover + gasket | Welchrom® pre-slit red Teflon/white silicone septa, 9mm blue short thread, open cap 6mm center hole 100pk |
| 00821-40927 | Vial | Welchrom® 2mL Clear Short Thread Wide Mouth Vial w/Writing 11.6*32mm, 1st Grade Hydrolyzed Glass 100pk |
| 03909-22001 | Analytical column | WM-InoWAX, 30m×0.25mm×0.25μm |
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