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

Figure 1. Control profile of urethane 0.1 μg/mL
Figure 2. Spectrum of liquor samples
Figure 3. Spectrum of liquor samples spiked with 0.05mg/kg

Sample spiked 0.05mg/kg recovery table

SsubstanceThe average recovery rate%Rsd(N=2)%
Ethyl carbamate88.231.43

Related product information

00567-20008SPE cartridgeWelchrom®Celite AZO,2g/12mL,20pk
00837-05003Centrifuge tubeWelchrom® Disposable Centrifuge Tubes, Conical Bottom, RCF12000xg, Bag, Sterilized, 15mL, 25/pk
00837-0500215mL screw top centrifuge tubeWelchrom® Disposable Centrifuge Tubes, Flat Cap, Conical Bottom, RCF12000xg, Bag, Non-sterile, 15mL, 50/pk
00824-31001Solid phase extraction deviceWelch Solid Phase Extraction Unit, 12-Position Square Cylinder
00821-32291Cover + gasketWelchrom® pre-slit red Teflon/white silicone septa, 9mm blue short thread, open cap 6mm center hole 100pk
00821-40927VialWelchrom® 2mL Clear Short Thread Wide Mouth Vial w/Writing 11.6*32mm, 1st Grade Hydrolyzed Glass 100pk
03909-22001Analytical columnWM-InoWAX, 30m×0.25mm×0.25μm
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