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Simplified assay of diethylene glycol and ethylene glycol in various raw materials by capillary gas chromatography

The FDA has recently taken steps to reduce risks due to raw materials affected by economically motivated adulteration (EMA). One area of great interest is diethylene glycol (DEG) or ethylene glycol (EG) adulteration of glycerin, propylene glycol, and solutions of sorbitol, for which the USP monographs have recently been, revised (1). Such adulterations have occurred many times and in many countries, including a tragic episode between November 2008 and January 2009 in which 84 children in Nigeria died after ingesting teething syrup contaminated with DEG (9, 10). To eliminate this problem, the FDA has required manufacturers of finished products to assay and confirm that incoming glycerin, propylene glycol, and sorbitol solutions meet the USP limits, and the FDA/USP has incorporated such testing into the identity requirements of its updated monographs.

Unfortunately, even though USP test procedures detail a simultaneous DEG and EG assay for these materials, different standard solutions are specified depending upon whether the incoming sample is glycerin, propylene glycol, or a sorbitol solution; in addition, a certain gas chromatography (GC) capillary phase is detailed for sorbitol solutions, while the assays for glycerin and propylene glycol use a different capillary phase, requiring column changeovers, separate GC systems, or front/rear column configuration. In addition, NF monographs for polyethylene glycols (PEG) and polyethylene glycol monomethyl ethers (MPEG) used in pharmaceutical products also require DEG and EG testing (detailing their own specific tests); three separate test procedures for these types of raw materials (the larger PEG‐type polymers are assayed differently than their smaller counterparts), making assay at QC unwieldy.

This paper describes a single, simple test procedure that is applicable to the simultaneous assay of DEG and EG in all types of the described raw materials, using one standard solution. The assay procedure involves straightforward isolation, trimethylsilylation, and simultaneous capillary gas chromatographic quantitation using capillary GC with flame ionization detection. Although the USP‐NF limits are 0.10% DEG and 0.10% EG (and 0.25% total DEG plus EG for the PEG and MPEG products), in reality any EMA would be at levels significantly higher than that, as low‐level illegal EMA would not be economically advantageous. The scope of this project was not to fully validate this technique for inclusion in USP‐NF, but just to demonstrate its applicability for those wishing to utilize it or take it further.

Authors:   Molever, K.
Journal:   International Journal of Cosmetic Science
Volume:   32
edition:   6
Year:   2010
Pages:   471
DOI:   10.1111/j.1468-2494.2010.00619_2.x
Publication date:   01-Dec-2010
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