Citation: PENG Qiaorong, TANG Tao, YU Shuxin, SUN Yuanshe, LEI Wu, WANG Fengyun, ZHANG Weibing, LI Tong. Determination of N-nitrosodimethylamine in beer by frozen zone melting liquid-liquid extraction/gas chromatography[J]. Chinese Journal of Chromatography, ;2014, 32(4): 433-437. doi: 10.3724/SP.J.1123.2013.12030 shu

Determination of N-nitrosodimethylamine in beer by frozen zone melting liquid-liquid extraction/gas chromatography

PENG Qiaorong ^1,2 ,
TANG Tao ^1,2 ,
YU Shuxin ² ,
SUN Yuanshe ² ,
LEI Wu ¹ ,
WANG Fengyun ¹ ,
ZHANG Weibing ³ ,
LI Tong ^2,,

1.
1. Nanjing University of Science and Technology, Nanjing 210094, China;

Corresponding author: LI Tong,
Received Date: 25 December 2013
Available Online: 24 February 2014
Fund Project: 国家重大科学仪器设备开发专项项目(2012YQ12004401，2012YQ12004403)；国家自然科学基金项目(51242001). (2012YQ12004401，2012YQ12004403)；国家自然科学基金项目(51242001)

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.
- frozen zone melting liquid-liquid extraction,
- gas chromatography (GC),
- N-nitrosodimethylamine,
- beer
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