建立了一种新型的冷冻熔炼液-液萃取法直接提取啤酒中的 N-二甲基亚硝胺( N-nitrosodimethylamine, NDMA),萃取液经 GC-FID 分析,双柱法定性,外标法定量。优化的前处理条件为:以二氯甲烷为萃取溶剂,啤酒样品和萃取溶剂的体积比为9:1,-19℃下冷冻16 h。结果表明:NDMA 在5~200 mg / L 范围内具有良好的线性关系(r2=0.9996);在5、10和20 mg / L 3个加标水平下的回收率分别为84.94%、83.24%、85.14%,平行7次测定的相对标准偏差(RSD)分别为3.06%、3.19%、2.63%。与常规液-液萃取方法(需要经过蒸馏、萃取、旋蒸、氮吹4个步骤)相比,本方法稳定、可靠,且操作简单,有机溶剂消耗量少。
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 dichlo-romethane. 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 evalu-ated. The results showed that the calibration curve of NDMA was linear in the range of 5-200 mg / L with a good correlation coefficient(r 2 )of 0. 999 6. 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-nitrosodimethyl-amine 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 sol-vent used,the proposed extraction method proved to be easy and simple,and adequate for high-throughput analysis at low cost.
参考文献
[1] | 陈婷;温裕云;欧延.[J].色谱,201432(01):89. |
[2] | 李丕;白桦;李海玉.[J].色谱,201432(01):81. |
[3] | 赵华;王秀元;王萍亚.[J].色谱,201331(03):223. |
[4] | 陈晶;张超杰;李飞.[J].净水技术,200928(04):10. |
[5] | Crews C.[J].Qual Assur Saf Crop Foods |
[6] | 赵宇翔;王翔;胡耀明.[J].分析试验室,201130(05):84. |
[7] | GB/T 5009. 26-2003.[S]. |
[8] | 于品华;常志东;金声超.[J].化工进展,200928(09):1507. |
[9] | 马冰峰;马雅倩;万益群.[J].南昌大学学报(理科版),201337(05):452. |
[10] | Reche F;Garrigos M C;Marin M L.[J].Journal of Chromatography A,2002976:301. |
[11] | 陈军辉;杨柏娟;李文龙.[J].色谱,200725(05):628. |
[12] | Snyder L R;Kirkland J J;Glajch J L;张玉奎,王杰,张维冰,.实用高效液相色谱法的建立[M].北京:华文出版社,2001 |
[13] | 张维冰 .[P].CN 202006038 U,2011-10-12. |
[14] | Sobhanzadeh E;Abu Bakar N K;Abas M R B.[J].J Haz-ard Mater,2011186:1308. |
[15] | 贺小雨;陈树兵;俞雪钧.[J].分析测试学报,200928(03):306. |
[16] | de Pinho G P;Neves A A;de Queiroz M E L R.[J].FOOD CONTROL,201021:1307. |
[17] | 张维冰;王智聪;万昊.[J].中国科学:化学,201343(02):209. |
[18] | Goulart S M;Alves R D;Neves A A.[J].Anal Chim Ac-ta,2010671:41. |
[19] | Rübensam G;Barreto F;Hoff R B.[J].Analytica Chimica Acta,2011705:24. |
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