AOAC Official Method 2000.01 Determination of 3-Chloro-1,2-Propanediol in Foods and Food Ingredients Gas Chromatography/Mass Spectrometric Detection First Action 2000

[The method is applicable to the determination of 3-chloro-1,2-propanediol (3-monochloropropane-1,2-diol; 3-MCPD) in hydrolyzed vegetable protein (HVP), soups and stocks, stock cubes, soy sauce, malt extract, salami, fish, cheese, flour, starch, cereals, and bread.]
Caution:    This work should be performed under a fume hood. Wear laboratory coat, gloves, and eye/face protection. Use double-containment systems for handling concentrated solutions of 3-MCPD-d₅. Take care to avoid ignition of flammable reagents by sparks or static discharge.
See Table 2000.01 for the results of the interlaboratory study supporting acceptance of the method.

A. Principle

Internal standard 3-chloro-1,2-propanediol-d₅ (3-MCPD-d₅) is added to the test portion, followed by salt solution, and the mixture is blended to a homogeneous consistency. After sonication, the contents of an Extrelut^TM refill pack are added and mixed thoroughly. The mixture is transferred to a glass chromatographic tube, and the nonpolar components are eluted with a mixture of hexane and diethyl ether. The 3-MCPD is eluted with diethyl ether, and the extract is concentrated to a small volume. A portion of the concentrated extract is derivatized and analyzed by gas chromatography with mass spectrometric detection (GC/MS). The concentration of 3-MCPD is expressed in mg/kg.