Determination of Low Levels of Methanol and Ethanol in Licorice Extract by Large Volume Injection Head-space GC.

Abstract

A large volume injection head-space GC method was established for measuring low levels of residual methanol and ethanol in licorice extract used as a food additive. A vial was kept at 50ῌ in the oven of the head-space sampler. Injection of the head-space gas for 0.75 min into a Poraplot Q GC column with a initial oven temperature of 35ῌ, enabled the determination of low levels (5 mg/g) of methanol and ethanol. The standard deviations for five rounds of analysis of methanol and ethanol in licorice extracts were between 0.82 and 2.97. Methanol was found in 6 samples out of 9 collected in 1999, at concentrations exceeding 50 mg/g, the limit set by the Japanese Government, established in 1999 and coming into force on April 1, 2000. The highest concentration reached 10,000 mg/g. Methanol at a concentration exceeding 50 mg/g was found in 2 out of 9 samples collected in 2000. The highest concentration was 270 mg/g.

Survey of Residue Levels of Organic Solvents in "Existing Food Additives" and Health Food Materials by Head-space GC

“…In addition, it should mix well with water which is used to disperse powder samples. In simultaneous determination of methanol and ethanol in licorice extract 5) , water was used as a carrier solvent for standard solutions. However, water did not mix well with the analytes.…”

Identification of Pharmaceutical Impurities in Formulated Dosage Forms

“…Furthermore, any volatile compounds present in solid materials can be readily detected with head space GC/MS. [125][126][127][128] The presence of small and volatile molecules in excipients (e.g., formaldehyde in povidone) can be studied with this approach. 128 Figure 20 shows the headspace GC/MS studies of multiple batches of povidone excipient manufactured by different vendors.…”