Abstract:

A simple and effective sample enrichment method of frozen zone melting liquid-liquid extraction was optimized and validated for the analysis of trace N-nitrosodimethylamine (NDMA) in beer samples. The method was based on high pressure liquid-liquid extraction with a low temperature frozen step. The 90 mL beer was placed in a container with 10 mL dichloromethane. After agitation, the sample was kept in a freezer for 16 h at -19 ℃. The organic extract was analyzed by gas chromatography with a flame ionization detector (GC-FID). The accuracy, precision, detection and quantification limits and linearity of the method were evaluated. The results showed that the calibration curve of NDMA was linear in the range of 5-200 mg/L with a good correlation coefficient (r²) of 0.9996. The recoveries at the spiked levels of 5, 10 and 20 mg/L were 84.94%, 83.24%, 85.14% with the relative standard deviations (n=7)of 3.06%, 3.19%, 2.63%, respectively. The ordinary extraction method of N-nitrosodimethylamine in beer includes the four steps of low-temperature distillation, liquid-liquid extraction, rotary evaporation and nitrogen blowing concentration. With the extremely low volume of solvent used, the proposed extraction method proved to be easy and simple, and adequate for high-throughput analysis at low cost.

Key words: N-nitrosodimethylamine, beer, frozen zone melting liquid-liquid extraction, gas chromatography (GC)